Liu Diss

APPLICATIONS OF GEOPOLYMER IN CIVIL ENGINEERING：
FEASIBILITY STUDY OF LOESS STABILIZATION AND WASTE

CONCRETE RECYCLING
A Dissertation
Submitted to the Graduate Faculty of the

Louisiana State University and
Agricultural and Mechanical College
in partial fulfillment of the
requirements for the degree of
Doctor of Philosophy
in
The Department of Civil and Environmental Engineering
by
Zhen Liu
B.S., China University of Geosciences, 2007
M.S., China University of Geosciences, 2009
M.S., New Mexico State University, 2010
August 2015
To my parents and my family
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ACKNOWLEDGEMENTS
I would like to express my sincere appreciation to my advisor Dr. Steve C.S. Cai, whose
expertise, dedication and patience benefited me considerably during my Ph.D. study in
Louisiana State University. Without his continuous support and encouragement, this
dissertation could not have been completed. I cannot thank you enough for your great
help and guidance in the past years. Dr. Guoping Zhang, who was my advisor before his
leaving Louisiana State University, is also acknowledged for his advice on the
investigation of the origin of collapsibility for the loess samples.
I am extremely grateful to the members of my graduate committee, Dr. Guoqiang Li, Dr.
Michele Barbato, Dr. Shengli Chen and Dr. Kevin S. McCarter, for your valuable
comments and suggestions on my research. Technical supports of Dr. V.P. Singh,
CAMD-LSU, Dr. Dongmei Cao, Material Characterization Cementer, Ms. Wanda
LeBlanc, X-Ray Diffraction & Geochemistry Lab, Ying Xiao, Biological Sciences, Dr.
Tyson Rupnow, LTRC, Mr. Greg Tullier, LTRC, Mr. Norris Rosser, LTRC, and Mr. Joe
Bell, Chemical Engineering, for the sample preparing and testing are greatly appreciated.
My special thanks also go to the visiting scholars Dr. Hui Peng, Dr. Yan Han, Dr. Jian
Yang, and Dr. Lianghao Zou for your great encouragement and help. Thank all my
colleagues in Prof. Cai’s research group for your friendship and insightful discussions.
Last but not least, I would like to thank my parents and my family. Your love and support
have encouraged me and provided me strength to pursue my dreams.
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TABLE OF CONTENTS
ACKNOWLEDGEMENTS ............................................................................................... iii
LIST OF TABLES ............................................................................................................ vii
LIST OF FIGURES ......................................................................................................... viii
ABSTRACT…. ................................................................................................................. xii
CHAPTER 1 INTRODUCTION..................................................................................... 1
1.1 Background ............................................................................................................... 1
1.1.1 Loess soil ............................................................................................................ 2
1.1.2 Waste concrete recycling .................................................................................... 3
1.1.3 Fly ash based geopolymer .................................................................................. 4
1.2 Objective and scope .................................................................................................. 5
1.3 Organization of the dissertation ................................................................................ 6
1.4 References ................................................................................................................. 7
CHAPTER 2 LITERATURE REVIEW........................................................................ 11

2.1 Origin of Loess ........................................................................................................ 11
2.2 Distribution of loess around the world .................................................................... 14
2.2.1 North America .................................................................................................. 14
2.2.2 South America .................................................................................................. 15
2.2.3 Europe............................................................................................................... 16
2.2.4 China................................................................................................................. 17
2.2.5 Central Asia ...................................................................................................... 19
2.3 Problems related to loess ......................................................................................... 20
2.4 Recycled aggregate concrete ................................................................................... 21
2.4.1 Recycling of C&D waste .................................................................................. 21
2.4.2 Recycled aggregate concrete ............................................................................ 25
2.4.3 Interfacial transition zone in concrete .............................................................. 29
2.4.4 Application of fly ash in concrete .................................................................... 30
2.5 References ............................................................................................................... 33
CHAPTER 3 ORIGIN OF THE COLLAPSIBILITY OF LOESS ............................... 40

3.1 Introduction ............................................................................................................. 40
3.2 Materials and methods ............................................................................................ 43
3.2.1 Soil samples ...................................................................................................... 43
3.2.2 Collapsibility measurement .............................................................................. 45
3.2.3 Mineralogical analysis ...................................................................................... 46
3.2.4 Microstructural characterization ....................................................................... 47
3.2.5 Image analyses.................................................................................................. 49
3.3 Analyses of results .................................................................................................. 51
3.3.1 Collapsibility coefficient .................................................................................. 51
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3.3.2 Soil mineralogy ................................................................................................ 53
3.3.3 Microstructure .................................................................................................. 56
3.3.4 Particle morphology ......................................................................................... 61
3.3.5 EDXS elemental analysis ................................................................................. 65
3.4 Discussion ............................................................................................................... 69
3.4.1 A conceptual microstructure model.................................................................. 69
3.4.2 Origin of collapsibility ..................................................................................... 71
3.4.3 Engineering implications .................................................................................. 72
3.5 Conclusions ............................................................................................................. 73
3.6 References ............................................................................................................... 74
CHAPTER 4 STABILIZATION OF LOESS WITH FLY ASH BASED

GEOPOLYMER ............................................................................................................... 79
4.1 Introduction ............................................................................................................. 79
4.2 Materials and methods ............................................................................................ 82
4.2.1 Loess ................................................................................................................. 82
4.2.2 Fly ash .............................................................................................................. 82
4.2.3 Geopolymer ...................................................................................................... 84
4.2.4 Loess stabilization with geopolymer ................................................................ 85
4.3 Results and discussion ............................................................................................. 87
4.3.1 Mechanical properties ...................................................................................... 87
4.3.2 Characterization of microstructure ................................................................... 90
4.3.3 Mineralogical analysis ...................................................................................... 94
4.3.4 Conceptual microstructural model ................................................................... 95
4.4 Conclusions ............................................................................................................. 97
4.5 References ............................................................................................................... 97
CHAPTER 5 NUMERICAL ANALYSIS OF THE STRESS DISTRIBUTION

ALONG ITZS IN RECYCLED AGGREGATE CONCRETE UNDER UNIAXIAL
COMPRESSION............................................................................................................. 101
5.1 Introduction ........................................................................................................... 101
5.2 Representative volume element ............................................................................ 102
5.3 Stress concentration factor .................................................................................... 103
5.4 Numerical model ................................................................................................... 103
5.5 Results and discussions ......................................................................................... 105
5.5.1 SCF distribution along ITZs ........................................................................... 105
5.5.2 Influence of model size .................................................................................. 106
5.5.3 Influence of property of ITZs ......................................................................... 109
5.4.4 Comparison of the maximum of SCF in OITZ and NITZ.............................. 110
5.5 Conclusion ............................................................................................................. 110
5.6 References ............................................................................................................. 111
CHAPTER 6 INVESTIGATION OF THE PROPERTIES OF THE GEOPOLYMERIC

RECYCLED AGGREGATE CONCRETE .................................................................... 114
6.1 Introduction ........................................................................................................... 114
6.2 Materials and methods .......................................................................................... 117
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6.2.1 Recycled aggregates ....................................................................................... 117
6.2.2 Fly ash ............................................................................................................ 119
6.2.3 Alkali solution ................................................................................................ 120
6.2.4 Geopolymeric recycled aggregate concrete.................................................... 121
6.3 Results and discussions ......................................................................................... 125
6.3.1 Physical and mechanical properties................................................................ 125
6.3.2 Characterization of microstructure ................................................................. 129
6.3.3 Mineralogical analysis .................................................................................... 131
6.3.4 Nanoindentation ............................................................................................. 133
6.3.5 Discussion on the mechanism of the non-NITZ formation in RAC ............... 138
6.4 Conclusions ........................................................................................................... 144
6.5 References ............................................................................................................. 145
CHAPTER 7 CONCLUSIONS AND FUTURE RESEARCH ................................... 150

7.1 Conclusions ........................................................................................................... 150
7.2 Future research ...................................................................................................... 152
APPENDIX: LETTER OF PERMISSION FROM THE AMERICAN SOCIETY OF

CIVI ENGINEERS ......................................................................................................... 154
VITA…………. .............................................................................................................. 156
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LIST OF TABLES
Table 2-1 Classification of recycling of by-product ......................................................... 23
Table 3-1 Some basic physical and index properties of the loess sample ........................ 44
Table 3-2 Summary of the mineralogical composition of the studied loess ..................... 56
Table 3-3 Major elements detected by EDXS from the interested spots in the loess ....... 67
Table 4-1 Some basic physical and index properties of the loess sample ........................ 82
Table 4-2 Composition of fly ash (wt.%).......................................................................... 83
Table 4-3 Summary of the sample mixtures and corresponding designations ................. 84
Table 5-1 Material properties defined in the numerical analysis .................................... 105
Table 5-2 Material properties in the extended model ..................................................... 107
Table 5-3 Maximum of SCF in OITZ and NITZ ............................................................ 110
Table 6-1 Percentages of coarse, medium, and fine aggregates in recycled aggregate .. 119
Table 6-2 Composition of fly ash (wt.%)........................................................................ 120
Table 6-3 Mixture combinations for geopolymer synthesis and compressive strength.. 121
Table 6-4 Physical and mechanical properties of recycled aggregates concrete ............ 126
Table 6-5 Reduction rates of the physical and mechanical properties of GRAC samples
with the increase of w/c ratio .......................................................................................... 127
Table 6-6 Mixture design of concrete in the study of Sidorova et al. (2014) ................. 139
Table 6-7 Identification of NITZ in other previous studies of RAC .............................. 141
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LIST OF FIGURES
Figure 2-1 Distribution of loess deposits in Alaska .......................................................... 14
Figure 2-2 Distribution of loess deposits in the northwestern United States .................... 15
Figure 2-3 Distribution of loess deposits in the Midcontinent of North America ............ 16
Figure 2-4 Loess distribution in Europe ........................................................................... 17
Figure 2-5 Loess distribution in Central China................................................................. 18
Figure 2-6 Distribution of loess in China ......................................................................... 19
Figure 2-7 Mechanical behavior of produced concrete with variant ratio of recycled
aggregate with a curing of 28 days ................................................................................... 26
Figure 2-8 Relationship between compressive strength and addition of recycled

aggregates ......................................................................................................................... 27
Figure 3-1 Major occurrence of the Loess Plateau in China and the sampling location at a
construction site in Xi’an. ................................................................................................. 43
Figure 3-2 The plasticity chart showing the classification of different loesses and the
studied loess. ..................................................................................................................... 45
Figure 3-3 Preparation of thin sections of loess samples for SEM characterization: (a) a
vacuum desiccator used for resin impregnation; (b) the hardened sample after
impregnation; and (c) the sectioned and polished sample. ............................................... 49
Figure 3-4 Results of the double oedometer tests ............................................................. 52
Figure 3-5 XRD patterns of loess samples subjected to different treatment .................... 53
Figure 3-6 SEM micrographs showing the overall structure of the loess ......................... 58
Figure 3-7 SEM micrographs showing the microstructure of the loess............................ 60
Figure 3-8 SEM micrographs showing unstable contacts and a pure clay aggregate ....... 61
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Figure 3-9 Comparison of (a) the original SEM micrograph selected for image analysis
and (b) the processed image with identified and isolated silt particles............................. 61
Figure 3-10 Statistical distributions of (a) the ECD, (b) sphericity, (c) HS circularity, and
(d) elongation of the analyzed silt particles ...................................................................... 63
Figure 3-11 SEM micrographs showing the interested spots analyzed by EDXS. ........... 65
Figure 3-12 Selected EDXS spectra showing the elemental compositions of interested
spots shown in Figure 3-11 ............................................................................................... 66
Figure 3-13 A conceptual microstructural model of a four-tired hierarchy...................... 70
Figure 4-1 Particle size distribution curve of the Class F fly ash ..................................... 84
Figure 4-2 Determination of the Young’s Modulus from a typical stress-strain curve .... 86
Figure 4-3 Unconfined compressive strength (UCS) of geopolymer stabilized loess ...... 89
Figure 4-4 Failure strain of geopolymer stabilized loess .................................................. 89
Figure 4-5 The Young’s modulus of geopolymer stabilized loess ................................... 90
Figure 4-6 SEM images of the natural loess, fly ash, and geopolymer stabilized loess ... 92
Figure 4-7 Illustration of the applied locations (sample K-1) in the EDXS characterization
........................................................................................................................................... 92
Figure 4-8 The EDXS spectra of the selected areas in Figure 4-7.................................... 93
Figure 4-9 The XRD patterns of geopolymer stabilized loess samples ............................ 95
Figure 4-10 A conceptual microstructure model of geopolymer stabilized loess ............ 96
Figure 5-1 Representative volume element of RAC ....................................................... 102
Figure 5-2 Schematic of the numerical model with a circular aggregate ....................... 104
Figure 5-3 Finite element model of RAC with a circular aggregate............................... 104
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Figure 5-4 Distributions of SCF along the ITZs in Model 1 .......................................... 106
Figure 5-5 Schematic of the extended model (Model 2 and Model 3) ........................... 106
Figure 6-1 Constitutive phases in the conventional concrete (left) and the recycled
aggregate concrete (right) ............................................................................................... 116
Figure 6-2 Particle size distribution of recycled aggregates ........................................... 118
Figure 6-3 Coarse, medium, and fine recycled aggregates ............................................. 119
Figure 6-4 Particle size distribution of the Class F fly ash ............................................. 120
Figure 6-5 Flow chart of the sample preparation ............................................................ 122
Figure 6-6 Schematic plan view of the nanoindentation test .......................................... 124
Figure 6-7 Failure patterns under compression .............................................................. 128
Figure 6-8 SEM images of the recycled aggregate ......................................................... 129
Figure 6-9 SEM images of the geopolymeric recycled aggregate concrete ................... 129
Figure 6-10 SEM images of the OPC recycled aggregate concrete................................ 130
Figure 6-11 The XRD patterns of OCP from recycled aggregate and NCP from GRAC
specimens ........................................................................................................................ 133
Figure 6-12 Distribution of the elastic modulus for the GRAC-1 specimen .................. 134
Figure 6-15 Distribution of the elastic modulus for the OPC-RAC specimen ............... 135
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Figure 6-16 Distribution of the hardness for the GRAC-1 specimen ............................. 136
Figure 6-19 Distribution of the hardness for the OPC-RAC specimen .......................... 137
Figure 6-20 Illustration of the “wall effect” in concrete ................................................. 138
Figure 6-21 Demonstration of the ITZ identification with nanoindentation in the concrete
with natural aggregates ................................................................................................... 140
Figure 6-22 Illustration of the non-formation mechanism of NITZ in RAC .................. 142
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ABSTRACT
The fast growing population and economic development have resulted in an increasing
demand for residential and commercial buildings and infrastructures. However, there are
problems identified to fulfill this demand, including that (1) problematic soils need to be
treated/improved before the construction of building and infrastructures; (2) the Portland
cement industry, which is used for concrete production and as the conventional soil
stabilizer, is not environment friendly; (3) qualified natural aggregates for concrete
production are being depleted; and (4) great amount of construction & demolition waste
(C&D waste) is being produced every year. This means that green materials and
recycling the C&D waste are of great significance to the civil engineers for the
sustainable development.
Geopolymer, which is an inorganic material formed by alkaline activation of aluminia-
and silica-containing material through a polycondensation process, could be synthesized
from various industrial by-products, such as fly ash and furnace slag, with high
compressive strength, low shrinkage, and other engineering properties. This renders
geopolymer a prospective future in civil engineering applications. This dissertation was
therefore conducted to investigate the feasibility of applying the fly ash based
geopolymer in the loess stabilization and waste concrete recycling.
With the integration of composition and microstructure, a four-tier conceptual
microstructure model is proposed to elucidate the origin of loess collapsibility. Based on
the understanding of the origin of the collapsibility, the feasibility study of loess
stabilization with geopolymer is then conducted. Results indicate that improved
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compressive strength, together with a compact and stable microstructure, has been
rendered by the binding effect of geopolymer gel.
Meanwhile, numerical analysis on recycled concrete shows that the new interfacial
transition zone (NITZ) plays a detrimental role to the performance of recycled aggregate
concrete (RAC), and could even contribute more to the mechanical failure of RAC at the
microscale than the old interfacial transition zone (OITZ). With this observation, how to
produce the RAC more effectively was then investigated in the feasibility study of waste
concrete recycling with geopolymer.
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CHAPTER 1 INTRODUCTION
1.1 Background
Every year, humankind consumes huge amounts of resources and produces vast
quantities of waste and pollution as a result of the consumption process. For example,
about 60 billion tons of raw materials were used annually during the 20th century, and
6000 Mt of mine wastes were generated all over the world due to the production of just
900 Mt of raw materials in 2000 (Jamshidi et al., 2015; Pacheco-Torgal and Labrincha,
2013; Whitmore, 2006). It is predicted that the Earth’s capacity could be exhausted
during the 21st century (Pacheco-Torgal and Labrincha, 2013).
Among all the industries, the construction industry consumes the most raw materials,
including both the renewable and non-renewable resources. Investigation shows that
concrete is the largest volume industrial product on earth (apart from the treated water)
with a production of about 1 t of concrete per capita manufactured every year (Jamshidi
et al., 2015). During the production of concrete, huge quantities of aggregates and
cement are consumed every year. However, the qualified natural aggregates for concrete
production are being depleted, and the manufacture of cement is highly energy-
consuming and emits greenhouse gas CO2. The cement manufacturing now ranks as the
seventh most energy intensive industry in the United States, and up to 7% of global CO2
are produced by the industry of Ordinary Portland Cement (Deb et al., 2014; Jamshidi et
al., 2015; Zhang et al., 2013).
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Meanwhile, the global population increased rapidly during the last century and is still
growing. This calls for an increasing demand for the residential and commercial
buildings and infrastructures. Due to the limited land, lots of the buildings/infrastructures
that are still in their service life have to be demolished for the new constructions.
Together with the regular maintenance and rehabilitation, a great amount of construction
& demolition waste (C&D waste) is being produced every year. On the other hand,
treatment/improvement of the problematic soil is another key issue in the engineering
field to fulfill the increasing demand in infrastructures and residential and commercial
buildings. However, the production of conventional soil stabilizers (such as Portland
cement and lime) consumes a large quantity of energy and emits greenhouse gas CO2.
Hence, exploring green materials, and recycling the C&D waste are of great significance
to the civil engineers for the sustainable development.
1.1.1 Loess soil
Loess is an aeolian, non-stratified deposit that is composed of primarily silt-sized mineral
particles and secondarily clay and sand particles transported by wind. It occurs widely
around the world, including central Asia, central Europe, northwestern and central USA,
Argentina, northern Russia, interior Alaska, and South America (Porter, 2007; Roberts et
al., 2007; Rousseau et al., 2007; Zárate, 2007). The aeolian loess is collapsible and
susceptible to landslides, hydroconsolidation, and seismic settlement (Yuan and Wang,
2009). Due to its collapsible behavior and other associated engineering problems, such as
wetting-induced landslides, hydroconsolidation, and seismic settlement, loess is classified
as one of the problematic soils (Delage et al., 2005; Derbyshire, 2001; Dijkstra et al.,
1994; Dijkstra et al., 1995; Rogers et al., 1994; Xu et al., 2007; Yuan and Wang, 2009).
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Particularly, an immediate and considerable collapse (up to 15%) could occur when the
loess is saturated (Jefferson et al., 2005). The metastable structure of natural loess has
resulted in construction delays and catastrophic failures, even loss of life (Derbyshire et
al., 2000; Jefferson et al., 2005; Zia and Fox, 2000). Therefore, it is of significance to
stabilize the collapsible loess.
Because the production of conventional soil stabilizers is highly energy consuming and
emits greenhouse gas CO2, some methods/techniques have been studied to develop green
alternatives, such as incorporating fly ash, which is an industrial waste, into the loess
stabilization (Viskochil et al., 1958; Zhang and Zhang, 2013; Zia and Fox, 2000).
However, these methods have been characterized with a very long curing time (it can be
several months or even longer) or low strength (Zhang and Zhang, 2013). Hence, the
study of new/green materials for loess stabilization is still under exploration.
1.1.2 Waste concrete recycling
Due to the regular maintenance and rehabilitation, the fast-speed urbanization in the
developing countries, and even natural disasters such as earthquakes, there is a fast-
increasing accumulation of the C&D waste. Traditionally, the C&D waste is disposed as
landfill. However, land that could be used for landfill is becoming more and more limited.
This causes an increase in the cost of dumping C&D waste. Meanwhile, the natural
aggregates keep diminishing as the construction activities move on. In light of making
use of waste materials and resource recovery, incorporation of the recycled aggregates
from the waste concrete recycling into the production of new concrete becomes an
effective way for both the treatment of C&D waste and the preservation of environment
and natural resources.
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In the past years, recycled aggregate concrete (RAC) has attracted tremendous attention
in both engineering practice and academic research (Casuccio et al., 2008; Kawano, 2003;
Li, 2008; Rao et al., 2007; Sagoe-Crentsil et al., 2001; Xiao et al., 2012). Nevertheless,
most of the studies focused on the incorporation of coarse recycled aggregates into the
production of RAC. The development of incorporating all recycled aggregates, i.e., both
coarse recycled aggregates and fine recycled aggregates, into RAC is still lagging. This is
mainly due to the inherent characteristics of fine recycled aggregates, including the
different constituents, the lower particle density, the high water absorption rate, and the
greater angularity as compared to the fine natural aggregates (Chan, 1998; Evangelista
and de Brito, 2007; Katz, 2003; Leite, 2001; Pereira et al., 2012). New methods including
additives and/or new cements are therefore being called for the production of the green
concrete.
1.1.3 Fly ash based geopolymer
Fly ash is a general type of coal combustion byproduct. Due to the limited land for
landfill and the related environmental hazards, the disposal of the huge amount of fly ash
generated around the world has become an engineering problem. A lot of researches have
been proposed and conducted for the potential applications of fly ash, including the
synthesis of geopolymer, based on the characterization of fly ash which consists of
substantial amount of SiO2 , and Al O .
Geopolymer, which was coined by Davidovits in the late 1970’s, is an inorganic material
formed by alkaline activation of aluminia- and silica-containing materials through a
polycondensation process. Through investigations, the fly ash based geopolymer has been
recognized as an effective way to produce eco-friendly materials with desired strength,
4
low shrinkage, fire resistance and other engineering properties (Davidovits et al., 1990;
Demie et al., 2013; Fernandez-Jimenez et al., 2005; Posi et al., 2013; Zhang et al., 2013).
Hence, it would be beneficial to investigate the feasibility of applying the fly ash based
geopolymer to loess stabilization and waste concrete recycling.
1.2 Objective and scope
This research focused on the feasibility study of applying the fly ash based geopolymer to
loess stabilization and waste concrete recycling with the objective to develop and
promote the applications of green materials in civil infrastructures:
(1) Loess is an eolian, non-stratified deposit that is composed of primarily silt-sized
mineral particles and secondarily clay and sand particles transported by wind. It has
been characterized with an immediate and considerable collapse (up to 15%) when it
is saturated. In order to explore the feasibility of stabilizing the loess soil with fly ash
based geopolymer, the mechanism controlling the collapsibility was studied first.
Loess is a particulate earth material and, same as other geomaterials, its behavior and
properties are dominantly and sometimes solely controlled by the mineralogical
composition and structure (including macroscopic texture and microstructure). Hence,
microstructure, composition, and particle morphology were studied for the
characterization of loess. For the study of the loess stabilization, compressive strength,
composition, and microstructure were characterized to investigate the effect of loess
stabilization with fly ash based geopolymer.
(2) Previous studies revealed that there are 3 phases (natural aggregate, interfacial
transition zone, and cement paste) in the conventional concrete and 5 phases (natural
aggregate, old interfacial transition zone, old cement paste, new interfacial transition
5
zone, and new cement paste) in the recycled concrete. Among all the phases, the
interfacial transition zone (ITZ) has been identified as the weakest link in the concrete
mixture. Hence, the stress distribution along the ITZs in the RAC was analyzed first.
Later, the composition-microstructure-strength relationship was investigated for the
geopolymer recycled aggregate concrete (GRAC). Since the new interfacial transition
zone (NITZ) is recognized as one of the most important constitutive phases in RAC,
attentions have been paid to investigate the (non-)formation of NITZ within the
GRAC specimens and the corresponding procedure of production.
1.3 Organization of the dissertation
This dissertation consists of seven chapters. Chapters 3 to 6 are based on papers that have
been accepted, are under review, or are to be submitted to peer-reviewed journals, and are
constructed using the technical paper format that is approved by the Graduate School at
Louisiana State University. Therefore, each chapter is relatively independent. For this
reason, some essential information might be repeated in these chapters. A brief outline of
all the chapters is presented below:
(1) Chapter one, the current chapter, presents the background, research objectives and
organization of the dissertation.
(2) Chapter two covers the literature review from the origin, distribution and related
problems of loess, together with the research progress in the area of recycled
aggregate concrete.
(3) Chapter three presents the investigation of the origin of the loess collapsibility.
Based on the comprehensive investigation, a conceptual microstructural model of a
four-tiered hierarchy (i.e., primary clay and silt particles, clay aggregates and clay-
6
coated silt particles, clay-silt mixture aggregates, and multiple cemented aggregates) is
proposed to account for the structural characteristics of loess and the origin of severe
collapsibility. This conceptual model also implies that the loess stabilization with a
focus on the modification of microstructure would be of efficiency.
(4) Chapter four presents the feasibility study of applying the fly ash based
geopolymer in loess stabilization, including studying the compressive strength,
composition, and microstructure of the stabilized loess. In correspondence to the
conceptual microstructure model proposed in Chapter three, a microstructure model is
applied to demonstrate the difference between the natural loess and the stabilized loess.
(5) Chapter five describes the numerical analysis of the stress distribution along the
ITZs in recycled aggregate concrete under uniaxial compression, which sheds some
lights on the performance of the interface zones.
(6) Chapter six presents the properties of the geopolymeric recycled aggregate
concrete. Due to the great significance of the new interfacial transition zone in
recycled aggregate concrete, nanoindentation, together with the scanning electron
microscopy, was employed to study its formation in geopolymeric recycled aggregate
concrete.
(7) Finally, the main findings in this study and the potential research for the future
study are presented in Chapter seven.
1.4 References
Casuccio, M., Torrijos, M.C., Giaccio, G., Zerbino, R., 2008. Failure mechanism of
recycled aggregate concrete. Construction and Building Materials 22, 1500-1506.
Chan, C., 1998. Use of recycled aggregate in shotcrete and concrete. University of British
Columbia.
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Davidovits, J., Comrie, D.C., Paterson, J.H., Ritcey, D.J., 1990. Geopolymeric concretes
for environmental protection. Concrete International 12, 30-39.
Deb, P.S., Nath, P., Sarker, P.K., 2014. The effects of ground granulated blast-furnace
slag blending with fly ash and activator content on the workability and strength
properties of geopolymer concrete cured at ambient temperature. Materials & Design
62, 32-39.
Delage, P., Cui, Y.J., Antoine, P., 2005. Geotechnical problems related with loess
deposits in Northern France, Proceedings of International Conference on Problematic
Soils. Eastern Mediterranean University Press, Famagusta, North Cyprus, pp. 517-
540.
Demie, S., Nuruddin, M.F., Shafiq, N., 2013. Effects of micro-structure characteristics of
interfacial transition zone on the compressive strength of self-compacting
geopolymer concrete. Construction and Building Materials 41, 91-98.
Derbyshire, E., 2001. Geological hazards in loess terrain, with particular reference to the
loess regions of China. Earth-Science Reviews 54, 231-260.
Derbyshire, E., Wang, J., Meng, X., 2000. A treacherous terrain: background to natural
hazards in northern China, with special reference to the history of landslides in
Gansu Province. Landslides in the thick Loess Terrain of north-west China. Wiley,
New York 19.
Dijkstra, T.A., Rogers, C.D.F., Smalley, I.J., Derbyshire, E., Li, Y.J., Meng, X.M., 1994.
The loess of north-central China: Geotechnical properties and their relation to slope
stability. Engineering Geology 36, 153-171.
Dijkstra, T.A., Smalley, I.J., Rogers, C.D.F., 1995. Particle packing in loess deposits and
the problem of structure collapse and hydroconsolidation. Engineering Geology 40,
49-64.
Evangelista, L., de Brito, J., 2007. Mechanical behaviour of concrete made with fine
recycled concrete aggregates. Cement and Concrete Composites 29, 397-401.
Fernandez-Jimenez, A., Palomo, A., Criado, M., 2005. Microstructure development of

alkali-activated fly ash cement: a descriptive model. Cem. Concr. Res. 35, 1204-
1209.
Jamshidi, A., Kurumisawa, K., Nawa, T., Hamzah, M.O., 2015. Analysis of structural
performance and sustainability of airport concrete pavements incorporating blast
furnace slag. Journal of Cleaner Production 90, 195-210.
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Jefferson, I., Rogers, C., Evstatiev, D., Karastanev, D., 2005. Treatment of metastable
loess soils: Lessons from Eastern Europe, in: Buddhima, I., Jian, C. (Eds.), Elsevier
Geo-Engineering Book Series. Elsevier, pp. 723-762.
Katz, A., 2003. Properties of concrete made with recycled aggregate from partially
hydrated old concrete. Cem. Concr. Res. 33, 703-711.
Kawano, H., 2003. The state of using by-products in concrete in Japan and outline of
JIS/TR on recycled concrete using recycled aggregate, Proceedings of the 1st FIB
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Leite, M., 2001. Evaluation of the mechanical properties of concrete made with recycled
aggregates from construction and demolition waste. PhD Thesis in Civil Engineering
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Li, X., 2008. Recycling and reuse of waste concrete in China: Part I. Material behaviour
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Pacheco-Torgal, F., Labrincha, J.A., 2013. The future of construction materials research
and the seventh UN Millennium Development Goal: A few insights. Construction
and Building Materials 40, 729-737.
Pereira, P., Evangelista, L., de Brito, J., 2012. The effect of superplasticizers on the
mechanical performance of concrete made with fine recycled concrete aggregates.
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Encyclopedia of Quaternary Science. Elsevier, Oxford, pp. 1429-1440.
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10
CHAPTER 2 LITERATURE REVIEW
2.1 Origin of Loess
‘Loess’ was firstly introduced by Karl Caesar von Leonhard in 1820 to name a type of
pale yellow, non-stratified sediment which was discovered in the Neckar River Valley,
Heidelberg, Germany (Smalley et al., 2001). In order to establish a full definition of loess,
some arguments have been proposed in the past years. Smalley and Vita-Finzi (1968)
defined loess as a type of materials mainly consisting of wind-spread quartz particles
with diameters in 20-50µm. Pye (1995) argued that any definition concerning the
thickness, grain size, color, composition and even morphology is unnecessary because all
the above factors could vary from the locations of loess deposits, and there should be
only one essential definition of loess: it is a sub-aerially accumulated deposit and
primarily consists of wind-transported silts. Now it is generally recognized that loess is a
porous and non-stratified deposit consisting of wind-transported silt-sized particles
(Giménez et al., 2012; Muhs, 2007; Porter, 2007).
Since Karl Caesar von Leonhard reported his discovery of loess at the first time in 1820,
more and more scientists started to study this newly found soil and proposed the ‘Loess
Problem’ which aimed to determine how the loess deposits are formed (Smalley et al.,
2001). In 1882, Ferdinand von Richthofen proposed a subaerial theory for the deposition
of loess and concluded 12 essential characteristics of loess (Smalley et al., 2001):
1) It is different from other previously found deposits in petrographical,
stratigraphical and faunistic aspects.
11
2) Both the composition and structure are almost homogeneous.
3) It is distributed at an above sea-level altitude.
4) The large body of loess is in a peculiar shape.
5) The composition is the same for all the pure loess.
6) Quartz is angular shaped.
7) It is non-stratified.
8) The capillary tubes are encrusted with carbonate of lime.
9) It tends to cleave vertically.
10) There are lots of land shells in the loess deposit.
11) There are mammal bones.
12) It is always found that the loess deposits cover the slopes with angular fragments
at the basin area.
In 1890, John Hardcastle proposed a link between the source of the dust and climate. It is
argued that there is no other way but the ice movement during the glacial period could
produce the great quantities of fine materials. Pavel Tutkovskii tried to interpret the
formation of loess with the special environment during the glacial period in 1899, but did
not gain too much attention at that time due to Berg’s promotion of the soil-eluvial theory
(Smalley et al., 2001).
Obruchev published a paper concerning the origin of desert loess in 1952, which was
translated into English in 1986. It is stated that the fine particles of sand and dust which
are produced by weathering and wind erosion are carried away by the dust storm and
latterly deposit on the dry steppe (Obruchev, 1986).
12
Russell (1944) reported his investigation of loess deposits in the lower Mississippi Valley.
It is argued that the initial parent materials of the loess deposit are the terrace deposits
which are similar to the backswamp clays of the Recent Mississippi River and the loess
deposits originates from a loessification process: the parent material is weathered, creeps
downslope, and then accumulates in the valleys.
Liu and Chang (1961) presented a paper about the investigation on Chinese loess at the
6th INQUA Congress in Poland. It was suggested that the origin of loess deposits might
be correlated with some climatic events.
With the further research on the loess deposits, it is accepted that the loess deposits
originate from the eolian silts. However, it is still under debate about the nature of the
particles (Frechen et al., 2003; Muhs, 2007; Smalley, 2008; Stuut et al., 2009).
Generally, the loess deposit areas are located at the down-wind direction from their
source areas such as deserts, periglacial zones and floodplains of meltwater streams
(Porter, 2007). However, it should be noted that loess might be re-transported from its
initial deposition location or re-worked by the environment. For instance, loess would be
from the top of a steep slope and re-accumulate at the toe of slope or the bottom of
adjacent valleys when the slope fails (Pye, 1995). New terms have been developed to
describe these special loess deposits, such as secondary loess (Pécsi, 1990), degraded
loess (Obruchev, 1945), redeposited loess (Smalley and Vita-Finzi, 1968), and reworked
loess (Pye, 1987). Currently, it is recognized by the majority of the scholars that eolian
origin is of characteristic to the primary loess. Hence, the reworked loess is refereed as
loess-like deposits in some papers (Dodonov, 2007).
13
2.2 Distribution of loess around the world
2.2.1 North America
It has been identified that loess is extensively distributed in North America, from high
latitudes such as Alaska (yellow areas in Figure 2-1) and Yukon Territory of Canada,
down to northwestern US (yellow areas in Figure 2-2), and Midcontinent (incorporating
the Great Plains and Central Lowland physiographic provinces) (colored areas in Figure
2-3), with both the glaciogenic and nonglaciogenic origins. The primary areas with loess
deposits in North America are mainly located in the Midcontinent, Lower Missisippi
Valley, the Wabash and Ohio River Valleys, the Pacific northwestern US (such as the
Columbia Plateau, and the Snake River area of southern Idaho), Alaska and the adjacent
Yukon Territory of Canada. With a comparison, it can be seen that United States
significantly prevails Canada in the areas of loess deposits (Roberts et al., 2007).
Figure 2-1 Distribution of loess deposits in Alaska (Roberts et al., 2007)
14
Figure 2-2 Distribution of loess deposits in the northwestern United States (Roberts et al.,
2007)
2.2.2 South America
Although the first loess record in South America can be backed to the nineteenth century,
it is still controversial about the origin of some loess-like deposits. It is widely recognized
that the loess distribution in South America is associated with the extensive Chaco-
Pampean plain, covering southern Brazil, southeastern Bolivia, western Paraguay, and
northern central Argentina. Besides, loess deposits have also been discovered in the
Catamarca mountain area, eastern Andean piedmont of Mendoza, mountain valleys of
Tucuman, and some areas of the Sierras sub-Andinas of northwestern Argentina and
Bolivia (Zárate, 2003, 2007).
15
Figure 2-3 Distribution of loess deposits in the Midcontinent of North America (Roberts
et al., 2007)
2.2.3 Europe
In 1820, Karl Caesar von Leonhard reported his discovery about a type of pale yellow,
unstratified sediment in the Neckar River Valley, Heidelberg, Germany, and a local word
‘loess’ was used to name this new discovered soil. Since then, the loess in Europe has
been investigated widely. In Europe, loess deposits have been found from the maritime
areas of Northwestern Europe over Central Europe to the Ukraine and the Russian Plains
with a few meters in thickness (Figure 2-4) (Haase et al., 2007; Rousseau et al., 2007;
Smalley et al., 2001). Due to the different terrains, different topographic constraints were
formed to the air flow and leaded to different modes in the loess deposition from the east
to the west (Rousseau et al., 2007).
16
Figure 2-4 Loess distribution in Europe (Haase et al., 2007)
2.2.4 China
Central China has been recognized as one of the world’s most extensive, significant
regions with thick loess deposits. Due to the special climate, loess deposits have been
extensively distributed in northern and northwestern China, resulting in a loess-formed
plateau, named Loess Plateau (Figure 2-5) with a coverage of 31.7 × 104 km2. Together
with the distribution in the other areas of China (Figure 2-6), the loess deposits occupy a
total area of 65 × 104 km2 (i.e., more than 6% of the territory of China) (Derbyshire, 2001;
Miao and Wang, 1990; Porter, 2007; Tan, 1988). A large number of distinctive
landscapes have been created because of the natural dissections in these areas, and have
been categorized into three major types by the Chinese. Yuan, meaning high tableland in
17
Chinese, is used to describe the loess plain which retains its original landscapes as the
loess piled up during the deposition process. Mao, which means rounded hills, is applied
to describe the dome-shaped loess hills. Liang, referring to the flat ridge in Chinese,
describes the strip-like loess landform. A Liang, which usually results from the erosion
and dissection in the Yuan landform, could stretch hundreds to thousands of meters in
length, but its width usually is only tens to hundreds of meters. Sometimes, a Liang could
be divided into several Maos by the intensive erosions and incisions (Golany, 1992;
Tsunekawa et al., 2014; Yang et al., 2010).
Figure 2-5 Loess distribution in Central China (Porter, 2007)
18
Figure 2-6 Distribution of loess in China (Derbyshire, 2001)
2.2.5 Central Asia
Due to the special climate in the Quaternary period, huge amounts of dust has been
transported by wind and accumulated to thick loess mantles in Central Asia. Until now,
the dust storm along desert or semi-desert is still impressing. Because of the widespread
distribution and thick accumulation, Central Asia has been recognized as one of the most
classical regions of loess deposits. To the north and west of the Pamirs, loess coverage
has been identified at parts of southern Kazakhstan, Kyrgyzstan, Uzbekistan, Tajikistan,
Turkmenistan, and Northern Afghanistan. In the southern Central Asia, loess deposits are
distributed at the intramontane Kashmir Valley, Siwalik foothills, Punjab, Peshawar basin,
and Potwar plateau. The thickness of loess mantles vary from a few meters to 20-30 m in
the southern Central Asia to 100-200 m in the northern part of Central Asia (Dodonov,
2007).
19
2.3 Problems related to loess
Because of the eolian origin and the arid climate, the sediments were loosely deposited
and cemented, which produces some special properties and problems to loess. Shi and
Shao (2000) reported that there are more than 60% of the land in the Loess Plateau
subjecting to the soil and water loss problems. According to the statistics, the average of
annual soil loss is about 2000-2500 ton/km2, and the soil erosion in some regions could
be as high as 59700 ton/km2 every year.
Seismic stress, together with erosion, usually produces lots of sub-vertical joint systems
which work as conduits and would be enlarged to pipes with a diameter of 1-2 m when
the water flow is repeated. Once the pipe systems are established, the hydraulic
conductivity will be increased by orders of magnitude, which extends the local saturation
of loess and finally results in a loess karst terrain (named “pseudokarst”) due to the
extensive collapse of loess deposits. Under some severe conditions such as intensive
rainfall and earthquake, mass movements could be initiated and lead to landslides which
are associated with loess debris flow and damming of streams. Due to the severe
consequences, loess landslides have been classified as a big and persistent threat to the
communities located in the areas with extensive loess distributions. The identifying and
mapping the hazards, for instance, show that 30% of Gansu province in China is subject
to the potential loess landslides and mudflows (Derbyshire, 2001).
Delage et al. (2005) reported that there are special problems caused to the high speed
railways by the loess deposits in Northern France. Though the climate is wet in Northern
France, some layers of the loess deposits are still unsaturated. With the removal of the top
soil during the construction of railways, the loess was exposed. In 1993, there were 43
20
sinkholes found along a 50 km long section. More sinkholes have been reported later
following two significant rainy periods, i.e., Winter 2001 and Spring 2002.
2.4 Recycled aggregate concrete
2.4.1 Recycling of C&D waste
Natural aggregate has played and is still playing an important role in the construction of
roads, buildings, and other infrastructures for its applications in the construction practice,
such as Portland cement concrete and fills, to provide/increase bulk, strength, and wear
resistance (Barksdale, 1991). However, accelerating urbanization in developing countries,
rehabilitation of old infrastructures (such as roads, airport runways, buildings and bridges)
and persistent expansion in industries around the world are depleting the limited natural
resources and also producing massive solid wastes while they are promoting the
economic development and providing people a better and more convenient life. For
example, 240 million tons of crushed rock and sand were consumed in the United
Kingdom, 1992. Thus, sustainable development is proposed to take care of environment
preservation and conservation of the limited natural resources. Among the total solid
wastes, the construction and demolition waste (C&D waste) holds a significant portion
and is usually disposed as land fill. Investigation shows that readily accessible disposal
sites around major cities in the world has been decreasing and the volume and maximum
sizes of such waste disposal are also being restricted, which poses severe difficulties for
the disposal. On the other hand, the limited natural resources are continuously
diminishing and the demand for aggregates in the world is very huge. Following the
concept of sustainable development, civil engineers are exploring the possible way to
21
reuse the C&D waste as aggregates in the production of new concrete (Khalaf and
DeVenny, 2004; Rao et al., 2007; Topçu and Günçan, 1995).
United States
It is reported that the usage of aggregate in United States keeps growing 2% every year
with 2.7 billon metric tons of aggregate consumed in 1990. Due to the construction and
demolition of infrastructures, i.e., bridges, concrete road beds, buildings, and airport
runways, massive C&D waste has been and is being created. As a better way to treat the
C&D waste and reduce the consumption of limited natural aggregate, recycled aggregate
(RA) has gained great acceptance in the United States. According to statistical analysis,
recycled aggregate in United States from debris recycling centers reaches 14%, with 50%
and 36% from natural aggregate producers and contractors, respectively. However, the
application of RAs is mainly in the pavement construction (Rao et al., 2007; Robinson Jr
et al., 2004).
Japan
It’s been several decades since the first research on the recycling of demolished concrete
for the production of new concrete. However, the application of recycled concrete is very
limited due to the non-compliance of specifications for the ready mixed concrete until
1991 when a Recycling Law was established by the Japanese Government to encourage
and control the application of recycled demolished concrete. Demolished concrete, wood,
and asphalt concrete were then defined as construction by-products by the former
Ministry of Construction (MOC). Specific targets for recycling construction by-products
were subsequently set up via the “Recycle 21” program in 1992 (Kawano, 2003; Rao et
22
al., 2007). The application of by-products is generally classified into three categories,
with the recycling of waste concrete falling into the category 2 (Kawano, 2003). In 1994,
MOC issued another specification named “Tentative quality specifications for reusing
materials from demolished concrete for construction works”, which leads to great
increase in the recycling ratio from 48% in 1990 to 65% in 1995, and then 96% in 2000.
However, most of the applications are limited to sub-base materials for road pavement
(Kawano, 2003; Rao et al., 2007). The difficulty to extend practice applications is
ascribed to the lack of experience, standards, guidelines, and variations in quality.
EU Union
It is estimated that there are about 450 million tons C&D waste generated every year in
EU, which leads C&D waste to be the second largest waste stream. Although most EU
member countries have set up goals to recycle the C&D waste, a research commissioned
by the Scottish Executive Development Department showed that about 44% of land fill
was mixed C&D waste and only 19% of the mixed C&D waste was recycled (Rao et al.,
2007).
Taiwan
During the earthquake in Central Taiwan in 1999, there were about 100,000 dwellings
severely damaged, leaving more than 30 million tons C&D waste. Due to the technology
limitation in the production of recycled aggregate concrete, most of the waste was used as
road base (Huang et al., 2002; Rao et al., 2007).
23
Table 2-1 Classification of recycling of by-product
Category
Description By-product materials
number
Sulfur, fly ash, burned ash of garbage, and
blast furnace slag, mold sand for cast iron,

Recycling the by-product for
etc., can be reused as cement.
1 new concrete from non-
Bricks, roof tiles, pottery, furnace slag, fly
construction industries
ash aggregate, etc., can be recycled as
aggregate.
Recycling by-product for new Sludge from concrete plants, refused
2 concrete from demolished concrete, recycled concrete, stone powder
concrete from recycle treatment of aggregate, etc.
Crushed concrete: which can be used as sub-
Recycling by-product for other base material of pavement, filler for asphalt
3 materials from demolished concrete, ground stabilizer
concrete Demolished concrete: which can be applied
for foot protection of levees, and fish reefs
Mainland of China
A lot of infrastructures have been demolished due to the rapid urbanization in the
Mainland of China, even though their design lives are only shortly fulfilled. Sometimes,
24
the natural disasters such as earthquakes and landslides also contribute a lot to the C&D
waste. It is reported that about 300 million tons of C&D waste generated in the
construction of Shanghai 2010 World Expo. Buildings and other infrastructures destroyed
in the 2008 Wenchuan earthquake and the 2010 Yushu earthquake contributed large
quantities of C&D wastes in a very short time. 30-40% of the total city solid wastes are
the C&D waste. Furthermore, 1/3 of the C&D waste is waste concrete. It is also predicted
that 638 million tons of waste concrete expects to be produced in 2020. The treatment of
C&D waste is becoming a big problem in China. With the development in the past years,
it is now being recognized by the Chinese engineering society and experts that recycled
aggregate concrete is an efficient way to dispose the C&D waste and enhance the
preservation of environment and natural resource. In order to provide a better guide for
the practice, a regional technical code for Application of Recycled Aggregate Concrete
(DG/TJ07-008) was also issued in Shanghai, 2007 (Li, 2008; Shi and Xu, 2006; Xiao et
al., 2012).
To summarize, the recycling of C&D waste is of great significance and has called
attentions around the world.
2.4.2 Recycled aggregate concrete
In contrast to the conventional concrete which is produced with natural aggregates,
recycled aggregate concrete (RAC) refers to concrete made with RAs. Due to the
different characteristics of RAs, such as a lower specific gravity and a higher water
absorption rate than the natural aggregates, the properties of recycled aggregate concrete
is changed consequently (Forster, 1997; Poon et al., 2004b; Robinson Jr et al., 2004;
Topçu and Şengel, 2004).
25
Ravindrarajah and Tam (1985) took an experimental investigation on the concrete with
variant qualities of recycled aggregates from waste concrete. It is found that the RAC
specimens have a lower resistance to mechanical activities, such as impact and crushing,
and a higher drying shrinkage and creep than the conventional concrete. It is also found
that the employment of RAs in the production of concrete leads to a reduction up to 25%
and 30% in compressive strength and modulus of elasticity, respectively.
Topçu and Günçan (1995) studied the mechanical properties of concrete with ASTM
C150 I Portland cement and recycled aggregates from C16 (compressive strength of 16
MPa at 28-day) concrete at ratios of 0, 30, 50, 70, and 100% as the replacement of natural
aggregates. The stress-strain plot is shown in Figure 2-7. Results show that density,
compressive strength, modulus of elasticity, and value of toughness all decrease with the
increasing ratio of RAs in the production of new concrete.
30
No RA
30% RA
Stress (MPa)
20 50% RA
70% RA
100% RA
10
0
0 0.005 0.01 0.015
Strain
Figure 2-7 Mechanical behavior of produced concrete with variant ratio of recycled
aggregate with a curing of 28 days (Topçu and Günçan, 1995)
26
Topçu (1997) further investigated the physical and mechanical properties of recycled
concrete using aggregates recycled from waste C16 concrete. Experiments show that the
slump value decreased from 100 mm for the natural aggregate concrete to 75 mm for the
recycled aggregate concrete, the surface hardness (Schmidt hammer tests) of recycled
aggregate concrete decreased with increasing addition of recycled aggregates from waste
concrete, and wider air voids developed in the specimens. Through compressive strength
test, it is found that introduction of waste concrete aggregates into the production of new
concrete leaded to a lower compressive strength. Impact tests indicate that the damage
depth increases greatly from 20-30 mm for natural aggregate concrete to 100-130 mm for
concrete with addition of aggregates recycled from waste concrete. The relationship
between compressive strength and ratio of recycled aggregates added to concrete is
shown Figure 2-8.
Figure 2-8 Relationship between compressive strength and addition of recycled

aggregates (Topçu, 1997)
27
Sagoe-Crentsil et al. (2001) studied the performance of N25 (25 MPa) concrete using
commercially crushed and graded recycled concrete aggregates. It is stated that there is
little difference between the natural aggregate concrete and recycled aggregate concrete
at a 95% confidence level with similar volumetric mixture proportions and workability.
However, a higher drying shrinkage value and about 12% reduction in abrasion resistance
have been found for the recycled aggregate concrete.
Evangelista and de Brito (2007) conducted an experimental study to evaluate mechanical
behavior of recycled aggregate concrete produced by applying the fine recycled concrete
aggregates to partially or totally substitute the natural fine aggregates. Results indicate
that it is viable to employ fine recycled concrete aggregates into the production of
structural concrete based on the experiment using no more than 30% fine recycled
concrete aggregates. It is well noticed that there are decreases in both tensile splitting
strength and modulus of elasticity with the increasing usage of fine recycled concrete
aggregates.
(Rao et al., 2007) stated that a higher water-cement ratio (0.55) produced 25% higher
strength than the reference concrete with a water/cement ratio of 0.4. It is also pointed out
that the strength reduction rate of recycled concrete depends on various factors, including
the type of concrete used for recycled aggregates, replacement ratio of RAs for natural
aggregates, water/cement ratio, and the moisture condition of recycled aggregates.
Through the literature review, it can be seen that it is viable to produce concrete with
recycled aggregates. However, how to produce RAC with desired strength is still under
exploration.
28
2.4.3 Interfacial transition zone in concrete
It has been generally accepted that there are three constitution phases (natural aggregate,
cement paste, and interfacial transition zone) in the conventional concrete. Among the
three phases, interfacial transition zone (ITZ) has been recognized as the weakest link in
concrete mixtures. As such, attentions have been called to explore the development
mechanism of ITZ. Past studies disclose that it is the wall effect caused by the coarse
aggregates leading to the formation of ITZs (Ollivier et al., 1995; Scrivener et al., 2004).
Because the coarse aggregate has a much larger size than the cement grain, the
aggregates would appear locally flat to the cement grains and hence form a wall effect.
With the help of mixing and vibrating during the production of concrete, a considerable
amount of water would be accumulated around the coarse aggregates. Due to the high
water content at the vicinity of coarse aggregates, an interfacial transition zone is finally
developed as the hydration of cement goes forward. Research found that there are larger
porosity and less cement and calcium silicate hydrate in the ITZs than the cement paste
phase (Agioutantis et al., 2000; Bentz et al., 1994; Garboczi and Bentz, 1996; Garboczi
and Bentz, 1997; Mondal et al., 2009; Rangaraju et al., 2010). It is also found that the
width of ITZ increases with the ratios of water/binder and aggregate/cement (Leemann et
al., 2006).
With the promotion of sustainable development, more and more studies are exploring the
feasibility of incorporating RAs from the waste concrete to the production of new
concrete. It is found that the application of RAs would bring two new constitutional
phases, i.e., old cement paste and new interfacial transition zone (NITZ), and render
different properties to the RAC. In order to investigate the mechanism underlying the
29
different behaviors between conventional concrete and RAC, Poon et al. (2004a)
conducted a study to compare the strength development of different concrete specimens
which were produced with natural aggregates and aggregates recycled from waste
concrete. Compressive strength tests show that the specimens with coarse recycled
aggregates have a lower strength than the specimens produced with natural aggregates.
With the observation of microstructures, the difference in the microstructure of ITZs is
one of the important factors contributing the different macro-behaviors of these
specimens.
Xiao et al. (2013) analyzed the stress distribution around ITZs in recycled aggregate
concrete under uniaxial compression. With the nanoindentation technique, the
mechanical properties of ITZs were measured. Numerical simulation results show that
there are stress concentrations (both tensile stress and shear stress) around the ITZs.
Furthermore, it is found that the concentrations of tensile stress become severer with
increasing elastic modulus of natural aggregates and decreasing elastic modulus of ITZs.
It is concluded that the poor bonding between the cement paste and aggregates lays a
pronounced influence on the macro-behavior of concrete.
2.4.4 Application of fly ash in concrete
Fly ash is a by-product from the thermal power plants which deeply reply on the burning
of coal for the source of power. Due to the high consumption of coal, massive of fly ash
are produced every year. For example, 70 million tons of fly ash were produced in the
United States in 2003 (Crouch et al., 2007). However, the utilization of fly ash is limited
and most of it is disposed as landfill. With the promotion of sustainable development,
how to make use of this waste is gaining increasing attentions.
30
With the composition characterization, fly ash now is being well recognized as a
pozzolanic material for a partial substitution of the Portland cement, the source material
in the production of pozzolanic cement, or additives for the production of concrete.
However, theses utilizations of fly ash are not fully “green”, though some achievements
have been made in these areas in the past years (Berndt, 2009; Kumar et al., 2007;
Malhotra and Mehta, 2002; Mehta, 2004, 2010).
At the same time, the research of geopolymer reaches a new era. Geopolymer, which was
coined by Davidovits in the late 1970’s, is an inorganic material formed by alkaline
activation of aluminia- and silica-containing materials through a polycondensation
process in which the tetrahedral silica (SiO2 ) and alumina (AlO4 ) are linked with each
other via sharing the oxygen atoms (e.g., (-Si-O-Al-O-)n , (-Si-O-Al-O-Si-O-)n , and
(-Si-O-Al-O-Si-O-Si-O-)n ). A general chemical structure of geopolymer could be
expressed as (Khale and Chaudhary, 2007; Ryu et al., 2013; Zhang et al., 2013):
Mn -(SiO2 )q -AlO2 -
n
where denotes an alkali cation, represents the degree of polycondensation, and is
the Si/Al ratio. The reactions involved in the geopolymerisation process could be
demonstrated as:
(Si O. Al O ) + H O + OH → Si(OH) + Al(OH)
Si(OH) + Al(OH) → (-Si-O-Al-O-)n + 4H O

O O
During the geopolymerisation process, water is released, which would play a positive role
to improve the workability of the solid mixture (Singh et al., 2015). This is in contrast to
31
the requirement of water in the hydration of Portland cement. Hence, it could be
rewarding to apply geopolymer into the production of RAC, considering that the high
water absorption rate of RAs is detrimental to the production of Portland cement recycled
concrete.
Previous research revealed that geopolymers/geopolymer-based products with designed
properties could be synthesized via an optimization in the experiment design, including
the selection of source materials, mixing proportion, and even the involved procedure
(Deb et al., 2014; Duxson et al., 2007; Majidi, 2009; Posi et al., 2013; Rangan et al., 2005;
Singh et al., 2015). Li et al. (2010) found that an increasing complex of processing and
water demand of the system could be lead to the metakaolin based geopolyer. Duxson et
al. (2007) reported that the fly ash based geopolymer usually has a higher strength and
better durability than the metakaolin based geopolymer. In order to investigate the
influence of different source materials on the properties of geopolymer products, Yang et
al. (2009) conducted a study on the flow and compressive strength of alkali-activated
mortars. It is found that slag renders a higher compressive strength, but a less flow, to the
geopolymer mortar than fly ash. Chindaprasirt et al. (2007) successfully produced a
geopolymer mortar which has a compressive strength of 52 MPa and a workable flow of
135±5% with a class C fly ash. Hardjito et al. (2004) reported that fly ash based
geopolymer concrete with the compressive strength of 30-80 MPa was achieved. Shi et al.
(2012) found that the compressive strength of RAC was improved when the fly ash based
geopolymer was applied to replace the ordinary Portland cement.
32
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39
CHAPTER 3 ORIGIN OF THE COLLAPSIBILITY OF LOESS
3.1 Introduction
Loess is an eolian, non-stratified deposit that is composed of primarily silt-sized mineral
particles and secondarily clay and sand particles transported by wind. It occurs widely
around the world, including central Asia, central Europe, northwestern and central USA,
Argentina, northern Russia, interior Alaska, and South America (Porter, 2007; Roberts et
al., 2007; Rousseau et al., 2007; Zárate, 2007). Of these regions, China has the most
extensive and thickest distribution of loess (Sun, 2002). The Loess Plateau located in
northern and northwestern China with an arid or semi-arid climate occupies a total area of
about 65 × 104 km2 (i.e., more than 6% of the territory of China) (Miao and Wang, 1990;
Tan, 1988). Recognized as one of problematic soils, loess has been a focus of
geotechnical research and practice since the 1960s, because of its collapsible behavior
and other associated geotechnical engineering problems, such as wetting-induced
landslides, hydroconsolidation, and seismic settlement (Delage et al., 2005; Derbyshire,
2001; Dijkstra et al., 1994; Dijkstra et al., 1995; Rogers et al., 1994; Xu et al., 2007;
Yuan and Wang, 2009).
Loess is a particulate earth material and, same as other geomaterials, its behavior and
properties are dominantly and sometimes solely controlled by the mineralogical
composition and structure (including macroscopic texture and microstructure). The
particulate minerals of a soil make up the essential solid skeleton for load bearing and
force transmission. Furthermore, a soil’s mineralogy also affects the mechanical behavior
40
(e.g., particle crushing strength, hardness or local yielding, elasticity, and interparticle
friction) of individual particles and is the primary factor controlling their morphological
properties (e.g., size, shape, and surface texture) (Mitchell and Soga, 2005). Soil structure
refers to both fabric and the non-frictional interparticle forces between adjacent soil
particles (Lambe and Whitman, 1969). The former is usually defined as the arrangement
and association of particles, particle groups, and pore spaces. Soil structure plays an
important role in affecting the chemical, physical, and biological processes within a soil,
and dominantly affects its mechanical and hydromechanical properties (da Silva and Kay,
2004; Kay et al., 2006; Lin et al., 2005; Mitchell and Soga, 2005; Monroy et al., 2010;
Zhang et al., 2004). In fact, Oda (1972) pointed out that a detailed study of the
morphological and physical properties of a soil’s granular particles and their
configurations (i.e., fabric) should be performed before its mechanical properties can be
realized.
The importance of soil structures to the understanding of loess collapse behavior and
other loess-related geohazards is also demonstrated by some recent efforts. Miao and
Wang (1990) proposed a hypothesis that the collapsibility of loess is caused by the
instability in its microstructure. Assallay et al. (1997) investigated the formation of open
structures in loess deposits and pertinent collapse using artificial specimens, and
concluded that the nature of loess materials and its microstructures play an important role
in the structural collapse. They further stated that particle size, one of the structural
parameters, is also a key control for structural collapse and other related effects. Tu et al.
(2009) developed a method to analyze slope failure in loess based on a full-scale field
experiment and attributed the rainfall-induced landslides to structural collapse. Yuan and
41
Wang (2009) tried to link the collapsibility with seismic settlement in a loess, and
concluded that both the collapsibility and seismic settlement are correlated to its
metastable microstructure, but with different triggering mechanisms. Giménez et al.
(2012) characterized a loess in central Spain with a particular perspective in
microstructure analysis. It is further noted by Rogers et al. (1994) that there is a change in
the packing of particles at the heart of loess collapsibility problems. Deng et al. (2007)
analyzed a series of scanning electron microscopy (SEM) images of loess samples from
six different sites and found that the trellis pore areas and particle size distributions are
well correlated with the seismic subsidence coefficient. However, despite of these efforts,
current understanding of the underlying mechanisms controlling loess collapsibility and
the origin of collapsibility still remain controversial or fragmental.
A comprehensive investigation is conducted herein to probe the fundamental mechanisms
of loess collapsibility based on particle-level characterization (e.g., microstructure,
composition, and particle morphology) and hence elucidate the origin of collapsibility
using a loess from Xi’an, a city situated within the Loess Plateau in northwestern China.
A systematic experimental program was developed to characterize the soil’s collapsibility,
mineralogy, microstructure together with the cementing agents, and silt particle
morphology. It is expected that the results from these characterization can lead to an in-
depth understanding of the collapsible behavior, particularly the trigger of collapse upon
wetting and subsequent evolution of the microstructure.
42
3.2 Materials and methods
3.2.1 Soil samples
Undisturbed block soil samples of typically 20 × 20 × 20 cm were collected at a depth of
11.0 m below the ground surface from an excavation pit in Xi’an, which is located within
the major occurrence of the Loess Plateau in China (Figure 3-1). The groundwater table
in the sampling site was very deep and thus all of the collected intact samples were
unsaturated. Immediately after retrieval from the ground, all sample blocks were
carefully wrapped in situ by multiple layers of plastic film, aluminum foil, and duct tape
to minimize water content change and related disturbance to the soil structure. Particular
care was also taken during transportation to and storage in the laboratory to keep the
disturbance to the structure minimal.
Figure 3-1 Major occurrence of the Loess Plateau in China and the sampling location at a
construction site in Xi’an.
43
Some basic physical and index properties of this loess were obtained in the laboratory by
following the relevant ASTM standard methods (ASTM, 2009), and results are shown in
Table 3-1. Particle size analysis through a combination of wet sieving and hydrometer
shows that the sample consists of dominantly silt particles with a fraction of 73.7% and
secondarily clay particles with a fraction of 26.0%. With a sand fraction of 0.3% that can
be essentially ignored, the loess is made of exclusively clay and silt particles. Its median
particle size (D50) is 9.2 µm, confirming that silts are its dominant mineral particles.
Table 3-1 Some basic physical and index properties of the loess sample
Property Value Determination method
Natural water content, wn 3.3% ASTM D 2216
Liquid limit, wL 35.4%
Plastic limit, wP 21.7% ASTM D 4318
Plasticity index, IP 13.7%
Specific gravity, Gs 2.72 ASTM D 854
In situ void ratio, e0 0.86 Not available
In situ unit weight, γ0 14.7 kN/m3 Not available
Clay fraction 26.0%
Silt fraction 73.7% ASTM D 2217
Sand fraction 0.3% ASTM D 422
Median particle size, D50 9.2 µm
Soil classification CL ASTM D 2487
44
Figure 3-2 shows the classification of different loesses proposed by Gibbs and Holland
(1960). According to this chart, the studied loess belongs to the category of “clayey
loess”. Despite its dominant silt fraction, it is a low-plasticity clay (CL) according to the
Unified Soil Classification System (USCS). Such a classification agrees well with prior
findings that most loesses usually have a low plasticity index (Delage et al., 2005).
25
Plasticity index, Ip (%)
20
15 Clayey loess
10 The studied loess
5 Silty loess
Sandy loess
0
0 10 20 30 40 50 60
Liquid limit, w L (%)
Figure 3-2 The plasticity chart showing the classification of different loesses (Gibbs and Holland,
1960) and the studied loess.
3.2.2 Collapsibility measurement
To assess the collapsibility of the loess sample, the widely used “double oedometer”
method was employed (Clemence and Finbarr, 1981; Jennings and Knight, 1957). Two
oedometer specimens were trimmed from the intact block samples. The first one was
tested at its natural water content during the entire loading stage, while the other one was
completely inundated before the beginning of loading and hence was assumed to be fully
45
saturated during the entire period of testing. Based on the compression curves of these
two specimens, the collapsibility coefficient (δs) is defined as (ASTM, 2009):
"# "#$
= "%
(3-1)
where Hp and Hp' are the stabilized heights (i.e., the heights at the end of a load increment)
of soil specimens at its natural and “saturated” water contents under a given vertical
pressure p, respectively, while H0 is the initial height of the soil specimens. Incremental
loading with pressures ranging from 50 to 2000 kPa was employed in the double
oedometer tests. To better define the compression curves and yielding points, the load
increment ratio used was smaller than 1.0. For each load increment, the load was held
constant for 24 hours for both specimens or until no further deformation occurred,
particularly for the intact, natural specimen.
3.2.3 Mineralogical analysis
X-ray diffraction (XRD) was performed to characterize the mineralogy of the loess
sample. A total of four different samples were analyzed to positively identify its
mineralogy. Since wetting can cause the structural collapse and strength loss of the loess,
an undisturbed sample block was first subjected to wetting with deionized water,
followed by air-drying. Such a sample having been subjected to a cycle of pre-wetting
and air-drying was hence termed “disturbed”. The disturbed sample was then gently
crushed and dry-ground by hand in a mortar with a pestle until all particles passed
through a No. 340 sieve (i.e., a mesh opening size of 44 µm) (which required excessive
grinding), resulting in the first powdery sample (i.e., “disturbed – dry ground”) for XRD
analysis. The disturbed sample was also wet ground for 3 minutes with ethyl alcohol in a
46
McCrone micronizing mill (McCrone Accessories and Components, USA), resulting in
the second powdery sample (i.e., “disturbed – wet ground”). The third sample was
prepared by the same procedures used to prepare the second one, except that the initial
sample was not subjected to pre-wetting with deionized water, but air-drying slowly from
its natural water content. It is thus termed “undisturbed – wet ground”. The fourth one,
termed “clay fraction only”, was the clay (i.e., <2 µm) fraction extracted from the loess
sample using the sedimentation method, which was based on Stokes Law. A side-loading
method was used to mount sample powder into an aluminum sample holder for XRD
analysis. XRD patterns were obtained in a Bruker/Siemens D5000 automated
diffractometer using Cu Kα radiation with an excitation energy of 40 kV and 30 mA, a
step size of 0.02°, a scan speed of 0.02° per 2 seconds, and diffraction angles ranging
from 2° to 42° 2θ. The peaks in the diffraction patterns were analyzed and identified by
the Jade 9.3.3 Program (Material Data, Inc.).
3.2.4 Microstructural characterization
One of the intact block samples was used to prepare specimens for microstructural
characterization. Two small soil blocks with the same dimension of 30 × 30 × 15 mm
(length × width × thickness) were carefully trimmed out of the central part of a relatively
large intact sample at its natural water content, with the orientation clearly marked as “V”
and “H” for vertical and horizontal surfaces, respectively, followed by air-drying slowly
in the laboratory ambient environment. Because their sizes were small, the shrinkage was
expected to be insignificant. In fact, the changes in their three dimensions were all less
than 1.0%, indicating that drying-induced shrinkage and sample disturbance were not a
major concern.
47
The two small soil blocks were then impregnated by a mixture solution containing epoxy
resin, acetone, ethanediamine, and Dibutyl phthalate at a volume ratio of 100 : 200 : 7 : 2.
A soil block was placed inside a clean plastic cup with its bottom pre-covered by a thin
layer of clean coarse sand to facilitate subsequent uniform seepage of the solution into the
sample. Impregnation took place in a sealed desiccator that holds the plastic cup together
with the soil block (Figure 3-3a). A high vacuum pressure of 0.02 MPa was first applied
to remove the air inside the sample, followed by extremely slow dripping the above
mixture solution into the cup. With continuous dripping, the surface of the solution
moved up very slowly inside the cup. This process was stopped when the soil sample
inside the cup became fully submerged with the solution surface exceeding the soil top
surface at least 10 mm. After impregnation, the soil sample was allowed to harden slowly
inside the cup for 3 months (Figure 3-3b). Then the hardened samples were cut into thin
sections with a dimension of 12 × 14 × 4 mm (Figure 3-3c). Both horizontally and
vertically cut thin sections denoted hereafter as “Sample H” and “Sample V”,
respectively, were obtained.
Microstructural characterization was performed on these thin sections in an FEI Quanta
200 3D FEG scanning electron microscope. Chemical elemental analyses were also
performed by a built-in energy-dispersive X-ray spectroscopy (EDXS) detector on
interested areas or spots selected from the observed samples. Particular interests were the
elemental composition of some individual soil particles (e.g., silt particles, clay
aggregates) and the cementing agents among particle contacts. Before SEM scanning, the
surface of the thinly sectioned samples was sputter-coated with a thin layer of platinum
(Pt) coating.
48
(a) (b)
Impregnation
solution
(c)
cm
Soil sample Desiccator
Figure 3-3 Preparation of thin sections of loess samples for SEM characterization: (a) a vacuum
desiccator used for resin impregnation; (b) the hardened sample after impregnation; and (c) the
sectioned and polished sample.
3.2.5 Image analyses
Image analyses were conducted on a selected SEM micrograph to quantify particle
morphology (particularly particle size and shape). Because of aggregation and attachment
to other particles, individual clay particles could not be isolated and identified under
typical SEM magnifications. In addition, clay particles and small silt particles mainly
serve as the cohesive material in the microstructure of loess (Gao, 2011). Therefore,
particle size and shape analyses were focused on relatively large silt particles with a size
of >5 µm. An SEM image containing plenty of silt particles was carefully selected, and
individual silt particles with clear boundaries were isolated manually, resulting in a
49
black-and-white image with the black color being occupied by silts. Then particle
morphology was analyzed by a computer program ExpertShape (V4.09), which can
provide more than 30 different particle properties. Because a great number of silt
particles with varying shapes and sizes were considered, the particle morphology
parameters obtained from ExpertShape were further statistically analyzed by SAS 9.3.
Form (overall shape), roundness (large-scale smoothness), and surface texture (small-
scale smoothness) are three independent properties describing the particle shape (Barrett,
1980). In this study, characterization of surface texture and roundness was not feasible,
owing to the relatively small size of silt particles and the low magnification used in the
selected SEM image. Therefore, four different particle morphology properties were
quantified for the silt particles in the selected SEM image, including sphericity,
elongation, circularity, and equivalent circular diameter (ECD), of which the former three
describe some form aspects of particle shapes, while the last one is related to the particle
size. It should be noted that these shape properties were obtained from a two-dimensional
SEM image and their definitions were also based on two-dimensional measurements.
In this study, sphericity is defined as the ratio of the radius of the inscribing circle to that
of the circumscribing circle. The inscribing and circumscribing circle radii are the
smallest and largest distances from the contour of the particle to its gravity center,
respectively. Elongation is defined as the difference between 1.0 and the aspect ratio,
which is the ratio of the minimum Feret diameter to the maximum Feret diameter. The
maximum and minimum Feret diameters are the largest and smallest distances between
two parallel tangents touching opposite sides of a particle. The high sensitivity (HS)
circularity (fcirc), depending on both the form and roundness, is used to describe the
50
compactness of a particle (e.g., a circle is the most compact shape). It is defined as the
ratio of the area of the particle in its original shape to the area of a circle having the same
perimeter of the particle. For instance, fcirc is 1, π/4, and 0 for a circle, a square, and an
infinitely long and narrow shape, respectively. The value of fcirc ranges from 0 to 1.
Finally, because of the difficulty in providing one single dimension to represent the size
of an irregular particle, the ECD is also selected to quantify silt particle size via image
analysis. It is the diameter of an equivalent circle having the same area (A) as the original
particle:
*
&'( = 2)+ (3-2)
3.3 Analyses of results
3.3.1 Collapsibility coefficient
Figure 3-4 shows the coefficient of collapsibility obtained from the double oedometer
tests. The compression curves (Figure 3-4a) indicate that the soil at its natural water
content and intact structure has a high yield stress of >2000 kPa, compared with the in-
situ overburden pressure of only 161.7 kPa (see Table 3-1 for some in situ soil properties).
Such a high yield stress may result from a combination of different reasons, such as
surface erosion-related unloading, an extremely low water content (or very high suction),
presence of interparticle cementation (including clay and calcite cementations), and
particle morphology (e.g., angularity and sphericity) (Pestana and Whittle, 1995), some
of which will be discussed later. The inundated specimen essentially has a linear normal
compression line without the yielding-related curvature in the studied stress range of 50-
51
2000 kPa. This implies that structural collapse may start at stresses of even less than 50
kPa.
0.9
0.8
Void ratio, e
0.7
0.6
Natural water content

0.5
Inundated
0.4
10 100 1000 10000
Vertical pressure, σ'v (kPa)
(a)
0.2
Collapsibility coefficient, δs
0.15
0.1
0.05
0
0 500 1000 1500 2000
Vertical pressure, σ' v (kPa)
(b)
Figure 3-4 Results of the double oedometer tests

Note: (a) Compression curves obtained from a specimen with natural water content and an
inundated specimen; (b) the collapsibility coefficient.
In Figure 3-4b, the collapsibility coefficient increases dramatically at vertical pressures of
50-1000 kPa, and then approaches asymptotically to ~0.18 at pressures of 1000-2000 kPa.
52
According to the ASTM standard (ASTM, 2009), this loess has a severe collapsibility
that exceeds 0.10 when the applied vertical stress is greater than 400 kPa. To elucidate
the origin of such a severe collapsibility, the soil composition, microstructure, and
particle morphology were further characterized using a variety of techniques, and results
are presented as follows.
3.3.2 Soil mineralogy
Clay fraction only Ca

C M C M M Q Ca Q M Ca Ca
Undisturbed - wet ground Q

Intensity
A Ca
N M N A Q Q Q
Disturbed - wet ground Q Q A

M N Ca Q Q
Q Q Ca
Disturbed - dry ground A Q Q
0 10 20 30 40
2θ (°)
Figure 3-5 XRD patterns of loess samples subjected to different treatment

(M = muscovite, N = nimite, Q = quartz, A = albite, Ca = calcite, C = clinochlore)
Figure 3-5 shows the XRD patterns of the four differently processed loess samples. For
the “disturbed – dry ground” sample, there are no peaks in the range of 2-20 o2θ, while
the peaks in the range of 20-42 o2θ indicate the presence of non-clay minerals, including
quartz (SiO2), albite (a plagioclase feldspar, NaAlSi3O8), and calcite (CaCO3). For the
“disturbed – wet ground” and “undisturbed – wet ground” samples, their XRD patterns
are nearly identical, indicating that simple wetting with deionized water does not cause
detectable changes to the mineralogical composition. In addition to the above three non-
53
clay minerals, two phyllosilicates, nimite and muscovite, are identified. The former is a
chlorite, while the latter is a mica. Dry grinding, particularly high-energy or excessive dry
grinding, can reportedly cause the deterioration and collapse of the crystalline structure of
fine-grained clay minerals (Garcia et al., 1991; Kristof et al., 1993). Thus, the absence of
clay minerals in the smaller diffraction angles of the “disturbed – dry ground” sample is
believed to be caused by excessive dry grinding, which damaged the crystal structure of
phyllosilicates (e.g., muscovite, nimite). Such a collapse of crystal structure usually
results in the clay minerals becoming XRD amorphous.
The XRD pattern of the “clay fraction only” sample shows the presence of both
muscovite and clinochlore, the latter being a chlorite. Noteworthy is that the extraction of
clay fraction results in a much higher concentration of clinochlore in the clay fraction that
may be otherwise too low in the bulk sample to be detectable by XRD. In fact, the
absence of clinochlore in the other three patterns suggest that this chlorite is mainly
present in the <2 µm fraction, while the other chlorite, nimite, is mainly present in the >2
µm fraction. Moreover, the pattern of the fourth sample also suggests that some fine
quartz and calcite are present in the clay fraction. In this pattern, the broad peaks of
clinochlore and muscovite, when compared with those peaks of muscovite and nimite
from the third sample, imply that the muscovite and clinochlore in the <2 µm fraction are
not as well crystalized as those in the bulk sample.
Regarding their origins, quartz and albite are most likely inherited from the initial wind
deposition. Calcite can be both primary and secondary. The primary one is inherited from
initial wind deposition and usually is present as solid mineral particles, while the
secondary one is post-depositionally formed or reprecipitated in-situ and is usually

54
believed to be a cementing agent. Two hypotheses can be used to explain the formation
of calcite cementation: (1) groundwater (even at a great depth) that contains dissolved
Ca2+ may move upward due to extensive drying and evaporation from the ground surface,
and after water evaporates Ca2+ can react with atmospheric CO2, resulting in the
reprecipitation of CaCO3 on particle surfaces and between particle contacts (Righi and
Meunier, 1995); and (2) weathering of the primary calcite and dolomite minerals results
in the leaching of Ca2+ to the groundwater, which can then react with atmospheric CO2 to
precipitate as calcareous cements. This synergetic process is also called “loessification”
(Delage et al., 2005; Derbyshire, 2001; Derbyshire et al., 1998). The newly formed or
secondary calcite can then act as a cementing mineral that exists on the surfaces of other
particles as coating or between particle contacts as bridging. These formations can then
lead to an increase in soil’s stiffness and strength. This is possibly one type of
mechanisms contributing to the remarkably high yield stress of the intact loess.
According to the literature, another type of mechanisms responsible for the high yield
stress of usually unsaturated in situ loess is clay cementation whose identification will be
discussed later. For this specific loess, clinochlore and nimite are the identified clay
minerals present in the soil. Despite the very dry condition in the field, the net negative
surface charges of clay minerals can still induce electrostatic interactions with other
mineral particles. Together with van der Waals forces, the electrostatic interaction can act
as bonding forces holding clay particles and other silt particles together. Thus, the in-situ
intact soil can gain further enhancement in yield and stiffness via clay cementation, in
addition to calcite cementation.
55
In summary, the loess sample contains quartz, albite, muscovite, and calcite as the non-
clay or silt minerals, and two chlorites, nimite and clinochlore, as the clay minerals
(Table 3-2). Noteworthy is that iron oxides were not identified from these XRD patterns,
despite the soil exhibits a light brown and yellowish color. One possible reason is that
their concentrations are too low to be detected by XRD. However, prior studies
concluded that two widely occurring iron oxides, hematite and goethite, are present in a
loess in China (Jiang et al., 2012). In fact, it is the iron oxides that render the loess a
yellowish to brownish color (Schwertmann and Taylor, 1989; Zhang et al., 2004).
Table 3-2 Summary of the mineralogical composition of the studied loess
Classification Name Ideal formula
Quartz SiO2
Non-clay phases Albite (a plagioclase feldspar) NaAlSi3O8
or silt minerals Muscovite KAl2(Si3Al)O10(OH,F)2
Calcite (both primary and secondary) CaCO3
Nimite (Ni,Mg,Fe2+)5Al(Si3Al)O10(OH)8
Clay minerals
Clinochlore (in the <2 µm fraction) (Mg,Fe2+)5Al(Si3Al)O10(OH)8
3.3.3 Microstructure
The microstructural characterization discussed in this section is mainly observational and
qualitative in nature. The focus is on the particle association and arrangement, porosity,
and interparticle contacts. Quantitative analysis of particle morphology (i.e., shape and
size) is presented in next section.
56
Overview of Microstructure: Figure 3-6 are four selected SEM images showing the
overview of the loess microstructure. First of all, angular or subangular silt particles that
can be clearly identified by their size and solid texture are randomly oriented and
distributed, and the interparticle zones are either voids or filled by much smaller clay
particles. Occasionally, a silt particle shows chipped edges or impact cracks. Although it
has been reported that most loesses are homogeneous (Delage et al., 2005), the studied
soil shows certain heterogeneity in the smaller scale. Some areas are densely packed,
while others are very porous. Clearly, bedding planes are absent in both the horizontal
and vertical surfaces. The lack of bedding and a random orientation and distribution of
different sized particles together with their subangular and angular shapes are
characteristic to the nature of this soil’s eolian deposition.
Particle Association: A careful examination of the images in Figures 3-6c and 3-6d and
Figure 3-7 can find that the clay and silt particles are typically associated together to form
aggregates. The size of aggregates varies significantly, ranging from a few tens to
hundreds of micrometers. In fact, aggregates with a size of 100-300 µm can be seen in
Figure 3-6c. While most aggregates consist of both silt and clay particles, some are made
up of only clay particles (Figure 3-8a). Moreover, it appears that the surface of most silt
particles is covered by a thin layer of coating (as indicated by the white external
boundary on these particles), which could be secondary carbonates (BeczeDeak et al.,
1997) or amorphous silica (Delage et al., 2005). In addition, clay particles can also exist
as coatings over silt particles (Clemence and Finbarr, 1981), which forms a distinct
association promoting the connection of silt particles by clay cementation. Some clay
aggregates are also mixed with or sandwiched by muscovite particles.
57
Figure 3-6 SEM micrographs showing the overall structure of the loess
Note: (a) and (b) refer to Sample V; (c) and (d) refer to Sample H. (d) is a magnified view of the
box in (c). B1 and D2: metastable particle chains; C1, C2, and C3: clay-silt mixture aggregates;
D1: a silt particle with clay coating.
Porosity: Pores with a wide variety of sizes can also be observed in Figure 3-6 (note that
the dark zones are the pore space). Large pores of >150-200 µm can be clearly observed
in Figures 3-6a and 3-6b, while smaller pores of a few to tens of micrometers are shown
in Figures 3-6c and 3-6d. In general, large pores are formed between aggregates, while
smaller ones exist within aggregates.
58
Particle Contact: Another important microstructural feature is particle contact, which
controls the onset of relative movement between particles. Two distinct features should
be pointed here: (1) a metastable structure formed by a thin chain of relatively small silt
and clay particles (Figures 3-6b and 3-6d); and (2) unstable points or contacts, which are
an important aspect of initial microstructure formation because they could collapse more
easily and contribute to the structural breakdown or evolution (Assallay et al., 1997).
Figure 3-8a shows the unstable point, while a higher resolution with some details is
shown in Figure 3-8b. With a small disturbance or the collapse of the pure clay aggregate
beneath Particle P1, then the contact point of the three silt particles, P1, P2, and P3,
becomes unstable, leading to the local collapse of this region.
Cementation: It is well known that loess usually contains both calcite and clay
cementations to support its stability at its unsaturated state. While direct observation of
calcite cementation is difficult due to its very small dimension or special morphology as
coatings or bridging, clay cementation is clearly observable (Figure 3-7). In general, silt
particles are randomly and loosely distributed, and bridged to each other by clay-based
connectors (i.e., clay cementation). In some occasions, clay coating on silt particles and
clay cementation are not differentiable (e.g., the curved chain of clay and smaller silt
particles, Figure 3-7a). The presence of calcite was identified by XRD, and the possible
mechanisms for the formation of calcite cementation are also discussed previously.
Therefore, both calcite and clay cementations act as bridging and bonding between silt
particles.
59
Figure 3-7 SEM micrographs showing the microstructure of the loess
Note: (a) Sample V; (b), (c), and (d) Sample H. (c) is a magnified view of the box in (b), and (d)
is a magnified view of the box in (c). M: muscovite particles.
60
Figure 3-8 SEM micrographs showing unstable contacts and a pure clay aggregate
(Note that clay coating around Particles P1 and P3. A1: a pure clay aggregate of 30-40 µm in
size; B1: an unstable particle contact.)
3.3.4 Particle morphology
Figure 3-9 Comparison of (a) the original SEM micrograph selected for image analysis and (b)
the processed image with identified and isolated silt particles.
61
Figure 3-9a shows the SEM image selected for silt particle morphology analysis, because
it contains a large amount of silt particles but much less pores. Figure 3-9b shows the
pertinent image where all silt particles of ≥5 µm in size were individually identified and
isolated, but clays are pores were excluded. It should be noted that the particles touching
the border were removed to avoid treating parts of a particle as a whole one. A total of
197 silt particles were identified and analyzed. Clearly, these particles are mainly angular
to subangular in roundness (Mitchell and Soga, 2005), and some are even lanky with a
large aspect ratio (e.g., the ratio of length to width). Given that the overall void ratio is e0
= 0.86 (Table 3-1), the total area of all silt particles and all clay particles in Figure 3-9b
are estimated to be 33,880 and 48,523 µm2. Thus, the ratio of the area occupied by silt to
that by clay is estimated to be 0.69, indicating that the silt particles only occupy about
two-thirds of the area occupied by clay particles. It also implies that the deformation of
the entire loading-bearing skeleton of this loess is controlled by clay fraction, although its
weight fraction is only 26.0% and the silt weight fraction is 73.7%. Such a phenomenon
may suggest that the collapsibility be mainly controlled by the clay particles and their
associations (e.g., pure clay aggregates, clay coating on silt particles, and clay
cementation).
Figure 3-10 summarizes the statistical results of particle shape parameters (i.e., sphericity,
HS circularity, and elongation) together with the size parameter (i.e., ECD) in terms of
probability density function (PDF) and cumulative distribution function (CDF) curves.
The ECD follows a lognormal distribution, while the other three shape parameters obey
arithmetic normal distributions. In fact, most particle size distributions (PSDs) exhibit a
62
lognormal distribution. In a critical review, Barrett (1980) also concluded that most shape
parameters of rock particles have arithmetic normal distributions.
0.12 100 0.35 100

90 90
0.1 0.3
80 80
0.25 Frequency
Cumulative (%)
Cumulative (%)
0.08 70 70
Frequency
Frequency
60 Cumulative 60
0.2
0.06 Frequency 50 50
40 0.15 40
Percent finer by number
0.04 Percent finer by weight 30 30
0.1
20 20
0.02 0.05
10 10
0 0 0 0
4 8 12 16 20 24 28 32 36 40 44 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
ECD (μm) Sphericity
(a) (b)
0.35 100 0.3 100

90 90
0.3 Frequency 0.25 Frequency
80 80
0.25 Cumulative
Cumulative (%)
70 Cumulative 70
Cumulative %
0.2
Frequency
Frequency
0.2 60 60
50 0.15 50
0.15 40 40
0.1 30
0.1 30
20 0.05 20
0.05 10
10
0 0 0 0
0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Circularity Elongation
(c) (d)
Figure 3-10 Statistical distributions of (a) the ECD, (b) sphericity, (c) HS circularity, and
(d) elongation of the analyzed silt particles
As shown in Figure 3-10a, the ECD ranges from 5 to 44 μm with a median of 13.6 μm,
demonstrating that all isolated particles in Figure 3-9b are indeed silt particles (i.e., a size
range of 2 to 75 µm). The PSD CDF curve (i.e., the plot of percent finer by weight vs.
particle size for silt particles only) obtained by the ASTM standard method (Table 3-1) is
also plotted in Figure 3-10a, with a coefficient of curvature Cc = 0.93 and a coefficient of
uniformity Cu = 4.21. If the Unified Soil Classification System (USCS) criteria developed
for the sand gradation are valid for silts, then the silt particles in this loess are poorly
graded. Similarly, another parameter, a sorting coefficient (S0), defined as the square root
63
of the ratio of the larger quartile to the smaller quartile, is also used to define the degree
of sorting (i.e., a measure of the spread of PSD). The silt particles shown in Figure 3-9b
has an S0 = 1.32 < 2.5, indicating that they are well sorted (Trask, 1932). Therefore, the
two criteria used to determine the gradation of silt particles yield consistent results.
Moreover, the well sorting of silt particles also supports the nature of eolian deposition of
this loess.
Regarding the shape of silt particles, the HS circularity has a mean value of 0.71,
showing that they are more close to a square (which has an HS circularity of π/4), in
terms of form and roundness. The value of elongation ranges from 0 to 1. For instance, a
particle with a shape symmetrical in all axes (e.g., a square or circle) has an elongation of
0, and a particle for which the difference between the minimum and maximum Feret
diameters is large yields an elongation value of ~1. For the silt particles, the mean value
of elongation is 0.39, which is closer to the lower range (i.e., 0) than to the higher range
(i.e., 1.0). To some extent, this also suggests that the silt particles are more close to a
square, consistent to the results of HS circularity. A mean sphericity of 0.44 indicates that
a considerable percentage of particles have a shape of concave polygon, although the
overall form is close to a square. Such a particle geometry is most likely caused by the
particle-to-particle collisions during transport by wind, which results in chipped or
indented edges (Delage et al., 2005). In summary, quantitative particle shape analyses
show that the silt particles are more of a square in terms of form and angular and
subangular in terms of roundness. However, some particles have a shape of concave
polygon resulting from particle collisions during eolian transport.
64
3.3.5 EDXS elemental analysis
Figure 3-11 shows the spots of EDXS chemical analysis performed on two different
zones selected from the Samples V and H, and corresponding results are summarized in
Table 3-3. Figure 3-12 shows some selected EDXS spectra to demonstrate the elemental
compositions of interested spots.
Figure 3-11 SEM micrographs showing the interested spots analyzed by EDXS.
65
O Si
Pt
O Spot 7
Al Si
C Na
Intensity
Pt
K Ca Spot 17
O Al Si Ca
C Pt Spot 18
Mg K Ca Fe
CO Pt
Mg Ca Spot 2
Ca
CO Pt Cl Spot 1
0 1 2 3 4 5 6 7
X-ray energy (keV)
(a) Sample V
Si
O
Spot H6
Intensity
Si
O Al
Na
Spot H5
C
Pt
Cl Spot H4
0 1 2 3 4 5 6 7
X-ray energy (keV)
(b) Sample H
Figure 3-12 Selected EDXS spectra showing the elemental compositions of interested spots
shown in Figure 3-11
66
Table 3-3 Major elements detected by EDXS from the interested spots in the loess
Sample V Sample H
Description
Spots Elements Spots Elements
Dark zone 1 C, O, Cl H4 C, Cl
Si, O
2, 3, 7, 8, C, O, Mg, Ca, Na, Al, Si, H1, H5, H6,
except H5 (O, Na,
Particles 12, 15, 16 H10, H13, H17
K, Ni, F, Fe
Al, Si)
Strip-like
10 C, O, Mg, Al, Si, K, Fe H7, H11 Si, O
particles
Particle tips 11, 17 C, O, Mg, Al, Si, K, Fe H8 Si, O
Bright particle C, O, Na, Mg, Al, Si, K, C, O, Al, Si, K, Ca,

4, 9, 13 H2, H3, H9, H16
boundaries Ca, Fe Ti, Fe
Zones between C, O, F, Na, Mg, Al, Si, H12, H14, H15,

6, 14, 18
Si, Ca, Fe, O, Al
particles P, K, Ca, Fe, Cr H18, H19
C, O, Na, Mg, Al, Si, P,

Clay aggregate 5
K, Ca, Fe
Note: The element Pt is not included because it is from the artificially introduced coating layer.
From Figure 3-12, Spot 1 in Sample V and Spot H4 in Sample H only contain C, O, and
Cl. These two spots are the dark zones or voids filled with epoxy resin (C21H25ClO5), one
of the major chemicals used for sample impregnation. Because of its very low atomic
weight, H in the clay minerals and epoxy resin cannot be detected by EDXS (Garratt-
Reed and Bell, 2005). Therefore, the dark zones are epoxy resin. Spot 2 in Sample V is a
particle and its EDXS spectrum shows the presence of C, O, and Ca, indicating that it
67
may be a primary calcite; the trace Mg indicates some substitutions of Ca by Mg in the
calcite. Spot 18 has a complex spectrum that shows the presence of C, O, Mg, Al, Si, K,
Ca, and Fe, suggesting that it may be clay minerals with calcite cementation. Finally
Spots 17 and 7 may be an albite (NaAlSi3O8) with calcite coating and quartz, respectively.
Similarly, for Sample H (Figure 3-12b), Spots H5 and H6 can be an albite and quartz
particle, respectively.
As shown in Table 3-3, C, O, Mg, Ca, Na, Al, Si, K, Ni, F, and Fe from the EDXS
analysis match well with the composition of those minerals identified by the XRD,
including chlorides, muscovite, quartz, albite, and calcite. Cr has been found to exist in
clinochlore (Phillips et al., 1980), which belongs to the chlorites; Ti has also been
detected in clinochlore and nimite (Phillips et al., 1980; Zhan and Guggenheim, 1995).
For the bright spots that are the external boundary of particles (it should be noted that not
all particle boundaries are shown as bright spots), the elements detected by EDXS
suggest that there are clay minerals acting as coating on the surface of silt particles. That
is why there exist more chemical elements (e.g., Na, Mg, Al, and K) as well as Si and O
for the particles, strip-like particles, and tips of particles (Spot 17) in Sample V. The
elements in the interparticle zones are identified as Si, Ca, Fe, O, and Al, which are the
main chemical elements of clay minerals. Together with the result of the bright spots, it
can be concluded that the filling material between silt particles are clay minerals. The
result from an aggregate-like spot (Spot 5 in Sample V) supports this statement.
68
3.4 Discussion
3.4.1 A conceptual microstructure model
An integrated synthesis of the above results on the mineralogy, elemental composition,
microscopy observations, and particle morphology provides a clear understanding of the
microstructure. Based on the developed understanding, a conceptual microstructure
model of a four-tiered hierarchy with an increasing length scale and complexity is
proposed to delineate the particle-level interactions and associations within a
representative volume element (RVE) (Figure 3-13). The proposed microstructure model
is established via a bottom-up (i.e., from smaller to larger length scales) approach to ease
interpretation and understanding. At the smallest length scale, Tier I contains the basic,
primary clay particles of <2 µm in size and silt particles of 2-75 µm in size that occur
occasionally as separate, functional units (e.g., load-bearing for structural stability). Here
a silt particle with carbonate or silica coating is treated the same as the monolith particle.
However, a majority of these particles do not exist as individually functioning units, but
form pure clay aggregates and clay-coated silts, which are the two major, relatively larger
and complex units defined in Tier II (Figure 3-13). In Tier III, even larger clay-silt
mixture aggregates form, which may consist of pure clay aggregates, silt particles, and
clay-coated silt particles as well as the clay and calcite cementations among these units.
Tier IV deals with the overall representative structure as represented by the RVE where
all of the units in Tiers I to III may all occur randomly. Noteworthy are the presence of
relatively small intraaggregate pores in the pure clay aggregates and clay-silt mixture
aggregates and the formation of relatively large interaggregate pores. Such porosity
features render the soil a highly porous structure. Finally, calcite and clay cementations
69
exist within individual aggregates and between adjacent aggregates, rendering the loess a
relatively stiff and stable structure in its intact state. Such a structure model can also takes
into account explicitly the mineralogical composition of the loess. The clay particles are
mainly two chlorites, nimite and clinochlore, and the silt particles are quartz, albite,
muscovite, and calcite (Table 3-2). Both clay minerals and secondary calcite can be the
interparticle and interaggregate cementations.
Figure 3-13 A conceptual microstructural model of a four-tired hierarchy

(Insets (a) and (b) show a silt particle with clay coating and clay-silts aggregates, respectively.)
70
3.4.2 Origin of collapsibility
The above conceptual microstructure model clearly demonstrates that the loess possesses
a metastable or collapsible structure. In its natural, intact state (i.e., usually unsaturated),
the high suction within the clay aggregates, clay and carbonate cementation, and the
angularity of silt particles provide sufficient cohesion and friction, resulting in a
metastable structure with considerably high strength and stiffness.
However, upon inundation or wetting, hydration of clay particles begins, resulting in the
expansion of electrical double layer on their surfaces. It is well known that fully hydrated
clays with expanded electrical double layer exhibit much smaller internal friction angle
than clays with less hydration. Such a process of clay hydration is also usually
accompanied by slaking of clay aggregates and clay cementation (i.e., detachment and
separation of clay coating from silt particles) (Mitchell and Soga, 2005), leading to the
first step in structural collapse (i.e., slaking of clay aggregates and breakdown of clay
cementations). Such an initial collapse may not be severe if the calcite cementation is not
totally broken. Within increasing loss of high suction stress (i.e., decrease in effective
stress) and/or an increase in external loading, calcite cementation can then breakdown,
resulting in further damage to the intact structure. The corresponding macroscopic
phenomenon is the collapse of the entire structure, accompanied with large surface
settlement (Figure 3-13).
In summary, the severe collapsibility originates from both the compositional and
microstructural characteristics of the loess. The former consists of a low water content
(i.e., an unsaturated state) and a significant volume occupied by clay and clay
associations (e.g., individual clay particles, clay coatings on silt particles, and clay
71
cementation), while the latter includes mainly the presence of weakly cemented pure clay
and clay-silt mixture aggregates and the high porosity (including relatively larger
interaggregate pores and smaller intraaggregate pores), as well as calcite cementation
(which also supports a metastable structure in its intact state).
3.4.3 Engineering implications
Because of its collapsibility, loess is regarded as one of the worst problematic soils that
geotechnical engineers have to deal with in engineering practice. The elucidation of the
loess microstructure and its mineralogical composition can help understand some peculiar
engineering behavior and properties of loesses, and such a developed understanding can
be exploited by engineers in the design and construction of buildings and facilities built
on or in the loess deposits, as well as for future research activities.
The high suction associated with the extremely dry state (i.e., a very low nature water
content of ~3.0%), the presence of calcite and clay cementations, and the distinct
morphology of dominant silt particles (i.e., the high angularity and high sphericity)
provide a synergy for the high one-dimensional yield stress (or apparent preconsolidation
pressure) exhibited by the loess in its natural, intact state. However, caution must be
taken in applying the results obtained from intact, unsaturated samples to situations
where the loess can have free access to water. In addition, the severe collapsibility of the
loess originates from a combination of several major structural features, including the
presence of pure clay and clay-silt mixture aggregates, clay cementation, high porosity,
and metastable and unstable particle contacts. However, the trigger is the hydration and
wetting of clay aggregates and clay cementation, leading to the slaking, detachment, and
breakdown of clay aggregates, clay coating, and clay cementation, respectively. Only
72
does after this first step of collapse occur, progressive failure followed by structural
avalanche can then take place to augment the collapsibility. In fact, such a characteristics
has not been so well documented in the literature.
The above conceptual microstructure model of a four-tier hierarchy also suggests some
peculiar features for the loess microstructure. First of all, although the loess consists of
exclusively clay and silt particles (i.e., Tier I), they usually are not present as separate,
individually functioning units. Instead, they form larger aggregates of varied composition
and length scales (i.e., Tiers II and III). Such a hierarchical structure also indicates high
porosity, and its metastable fabric with interparticle cementation implies high
compressibility upon structural collapse. Such a better delineation of the loess
microstructure may provide a detailed basis for the formulation of constitutive soil
models as well as the modeling of soil behavior under different loading conditions using
prevailing numerical analysis techniques, such as finite element and discrete element
methods (Jiang et al., 2012).
3.5 Conclusions
A series of laboratory testing was performed to characterize the collapse potential,
mineralogy, microstructure, and silt particle morphology of a loess in Xi’an, China, to
identify and elucidate the origin of its collapsibility. The integration of experimental
results, observations, and analyses leads to the following major conclusions:
(1) The loess exhibits a severe collapse potential, as indicated by its high collapsibility
coefficient that exceeds 0.10 under a vertical stress of 400 kPa and asymptotically
approaches 0.18 at ~2000 kPa.
73
(2) The soil consists of two chlorites, nimite and clinochlore, as the major clay
minerals and muscovite, quartz, albite, and calcite as the non-clay phases. Both
primary and secondary phases of calcite may be present in the soil, and the latter is
likely the major cementing agent. Other non-clay minerals (except muscovite) are
present as silt particles of angular and subangular in roundness.
(3) While occasionally clean silt particles are presented, the majority of silt particles
are covered with clay coating and/or associated with clay particles to form hybrid silt-
clay aggregates. In addition to calcite cementation, clay particles also act as bridging
(i.e., clay cementation) between silt particles and clay aggregates.
(4) Regarding the morphology of silt particles, the mean values of the ECD, HS
circularity, sphericity, and elongation are 13.56 μm, 0.71, 0.44, and 0.39, respectively.
These data indicate that the silt particles are more close to a square in the view of form
and are well sorted.
(5) The proposed conceptual microstructure model of a four-tiered hierarchy with an
increasing length scale and complexity can be used to delineate the particle-level
associations and interactions and to elucidate the origin of this loess’ collapsibility.
This conceptual model also indicates that the loess stabilization with a focus on the
modification of the microstructure would be of efficiency.
3.6 References
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metastable particle packings and open structures in loess deposits. Engineering
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Barrett, P.J., 1980. The shape of rock particles, a critical review. Sedimentology 27, 291-
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Garratt-Reed, A.J., Bell, D.C., 2005. Energy-Dispersive X-Ray Analysis in the Electron
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central Spain: a microstructural study. Environ Earth Sci 65, 2125-2137.
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structured loess in oedometer and triaxial wetting tests. Canadian Geotechnical
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TREATMENT ON THE CRYSTAL-STRUCTURE AND THERMAL-BEHAVIOR
OF KAOLINITE. Clays and Clay Minerals 41, 608-612.
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Elsevier Academic Press Inc, San Diego, pp. 1-89.
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Instability of Microstructure. Science in China,Ser.B, 86-96.
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Wiley & Sons, Inc., Hoboken, New Jersey.
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Pestana, J.M., Whittle, A.J., 1995. Compression model for cohesionless soils.
Geotechnique 45, 611-631.
Phillips, T.L., Loveless, J.K., Bailey, S.W., 1980. Cr (super 3+) coordination in chlorites;
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Velde, B. (Ed.), Origin and Mineralogy of Clays. Springer-Verlag, Berlin, pp. 43-161.
Oxford, pp. 1456-1466.
Rogers, C.D.F., Dijkstra, T.A., Smalley, I.J., 1994. Hydroconsolidation and subsidence of
loess - studies from China, Russia, North-America and Europe. Engineering Geology
37, 83-113.
Oxford, pp. 1440-1456.
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Wisconsin.
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Chinese Loess Plateau. Earth and Planetary Science Letters 203, 845-859.
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NORTHWESTERN CHINA. Engineering Geology 25, 103-122.
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rainfall infiltration in a loess slope and analysis of failure mechanism of rainfall-
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77
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Gongcheng Xuebao/Chinese Journal of Rock Mechanics and Engineering 26, 1297-
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78
CHAPTER 4 STABILIZATION OF LOESS WITH FLY ASH
BASED GEOPOLYMER
4.1 Introduction
Loess is an eolian, non-stratified deposit that is mainly composed of silt-sized mineral
particles and clay particles transported by wind. It occurs widely around the world,
including central Asia, central Europe, northwestern and central USA, northern Russia,
interior Alaska, and South America (Porter, 2007; Roberts et al., 2007; Rousseau et al.,
2007; Zárate, 2007). Classified as one of the problematic soils, loess has been a focus of
research and practice since the 1960s (Delage et al., 2005; Derbyshire, 2001; Dijkstra et
al., 1994; Dijkstra et al., 1995; Rogers et al., 1994; Xu et al., 2007; Yuan and Wang,
2009). The loess has been characterized with an open structure, in which the primary
quartz particles are connected with each other by bonding. The bonds would be broken
down when the applied stress or water content increases. Particularly, an immediate and
considerable collapse (up to 15%) could occur when the loess is saturated (Jefferson et al.,
2005). The metastable structure of natural loess has resulted in construction delays and
catastrophic failures, even loss of life (Derbyshire et al., 2000; Jefferson et al., 2005; Zia
and Fox, 2000). Therefore, it is of significance to stabilize the collapsible loess.
Aiming to solve or prevent the problems caused by collapsible loess, a variety of
measures have been developed or applied by the scientists and engineers. The current
mitigation and site improvement techniques include removal, replacement, compaction,
chemical stabilization, grouting, and pile foundations (Houston et al., 2001). The
treatment of loess with cement or lime has been widely applied (Arrua et al., 2012;
79
Jefferson et al., 2008; Li et al., 2011; Mei et al., 2014; Metelková et al., 2012). However,
the production of conventional soil stabilizers (such as cement and lime) consumes a
large quantity of energy and emits greenhouse gas CO2. Approximately 5-7% of global
CO2 are produced by the industry of Ordinary Portland Cement (OPC) (Deb et al., 2014;
Zhang et al., 2013). With the promotion of sustainable development, attentions have been
drawn to the loess stabilization with fly ash which is a general type of coal combustion
byproduct. For instance, Zia and Fox (2000) studied the engineering properties of fly ash
stabilized Indiana loess for a roadbase construction; White et al. (2005) investigated the
application of fly ash to improve Iowa loess. It is proposed that the durability and long-
term strength of the stabilized loess are not desirable, though the engineering properties
have been partially improved.
Geopolymer is an inorganic material formed by alkaline activation of aluminia- and
silica-containing material through a polycondensation process in which the tetrahedral
silica (SiO2 ) and alumina (AlO4 ) are linked with each other via sharing the oxygen atoms
(e.g., (-Si-O-Al-O-)n , (-Si-O-Al-O-Si-O-)n , and (-Si-O-Al-O-Si-O-Si-O-)n ). A general
chemical structure of geopolymer could be expressed as (Khale and Chaudhary, 2007;
Ryu et al., 2013; Zhang et al., 2013):
n
the Si/Al ratio. Research has revealed geopolymers with high compressive strength, low
shrinkage, acid resistance, and fire resistance could be synthesized from a variety of low
cost materials or industrial wastes, such as metakaolin, fly ash, rice husk ash, and furnace
80
slag. These characteristics render geopolymer a promising potentials in civil engineering,
including soil stabilization (Cristelo et al., 2012; Cristelo et al., 2011; Deb et al., 2014;
Duxson et al., 2007; Majidi, 2009; Posi et al., 2013; Rangan et al., 2005; Zhang, 2013;
Zhang et al., 2013). Moreover, Kim et al. (2011) developed a loess paste via
geopolymerization with natural loess and alkali solutions, which implies the feasibility
study of applying geopolymer in loess stabilization could be rewarding.
Therefore, as a part of research on the development of “green” material in civil
engineering, this papers describes a potential application of geopolymer in loess soil
stabilization (such as for subgrade, subbase or base in pavement). Fly ash, which contains
large quantities of reactive silicon dioxide and aluminum dioxide, was selected as the raw
material to synthesize geopolymer. Because the mechanical properties of geopolymer
depend on the selection of raw materials, precursors with variant Si/Al molar ratios,
water content, and types of alkaline activator (i.e., potassium hydroxide and sodium
hydroxide) were prepared to synthesize geopolymers. Based on the results, a Si/Al molar
ratio of 2.56 with a water/fly ash ratio of 0.3 for the potassium hydroxide activator and a
Si/Al molar ratio of 2.5 with a water/fly ash ratio of 0.35 for the sodium hydroxide
activator were selected in this study, due to the better quality of geopolymers, i.e., higher
compressive strength. The feasibility of loess stabilization with fly ash based
geopolymers is explored with samples at three fly ash/loess ratios (i.e., 10%, 20%, and
30%). Unconfined compressive strength (UCS), failure strain (,- ), and Young’s Modulus
(& ) were applied to characterize the mechanical properties. The microstructure and
mineralogy were investigated with the aid of scanning electron microscopy (SEM),
energy dispersive X-ray spectroscopy (EDXS), and X-ray diffraction (XRD).
81
4.2.1 Loess
Among all these regions with loess deposits, China has the most extensive and thickest
distribution of loess (Porter, 2007; Sun, 2002). The Loess Plateau located in northern and
northwestern China with an arid or semi-arid climate occupies a total area of 65×104 km2
(i.e., more than 6% of the territory of China) (Miao and Wang, 1990; Tan, 1988). Hence,
loess samples from the Loess Plateau are selected for this study. The basic physical and
index properties of this loess were obtained in the laboratory by following the ASTM
standard methods (ASTM, 2009), and results are shown in Table 4-1. Particle size
analysis shows that the sample consists of dominantly silt particles with a fraction of 73.7%
and secondarily clay particles with a fraction of 26.0%. With a sand fraction of 0.3% that
can be essentially ignored, the loess is made of exclusively clay and silt particles. Its
median particle size (D50) is 9.2 μm, confirming that silts are its dominant mineral
particles. According to the Unified Soil Classification System (USCS), this loess is a
low-plasticity clay (CL). Such a classification agrees well with prior findings that most
loess soils usually have a low plasticity index (Delage et al., 2005). The mineralogical
composition of the original loess sample is shown in the later comparison with the
geopolymer stabilized loess. The double oedometer test shows that the collapsibility
coefficient approximates to 0.18 at pressures of 1000-2000 kPa, which indicates this loess
has a severe collapsibility.
4.2.2 Fly ash
A Class F fly ash from Boral Material Technologies, Inc. (Monticello, Texas, USA) was
used as the raw material for synthesis of geopolymer. Based on its chemical composition
82
analysis (Table 4-2), the Si/Al molar ratio in this class F fly ash is 2.15, with a specific
gravity of 2.46. The particle distribution analyzed through hydrometer test is shown in
Figure 4-1.
Table 4-1 Some basic physical and index properties of the loess sample
Property Value Determination method
Liquid limit, wL 35.4%
Plastic limit, wP 21.7% ASTM D 4318
Plasticity index, IP 13.7%
Clay fraction 26.0%
Silt fraction 73.7% ASTM D 2217
Sand fraction 0.3% ASTM D 422
Median particle size, D50 9.2 μm
Soil classification CL ASTM D 2487
Table 4-2 Composition of fly ash (wt.%)
SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2O K2O Loss of ignition Moisture
52.06 20.54 5.50 14.07 3.29 0.57 0.94 0.69 0.10 0.01
83
100
90
80
70
Percent finer (%)

60
50
40
30
20
10
0
0.00010 0.00100 0.01000 0.10000
Particle size D (mm)
Figure 4-1 Particle size distribution curve of the Class F fly ash
4.2.3 Geopolymer
The properties of geopolymer vary with the raw materials and processing conditions
(Duxson et al., 2007). In order to compare the stabilization effect of different
geopolymers, two different precursors were prepared for the synthesis of geopolymers by
mixing a commercial sodium silicate solution consisting of 9.07 wt.% Na2 O and 29.35
wt.% SiO2 (Aqua Solutions Inc, USA) with a potassium hydroxide (88% purity quotient,
Sigma–Aldrich Co., USA) and a sodium hydroxide (purity quotient: 99%, Sigma-
Aldrich Co., USA), respectively. A summary of the sample mixtures is shown in Table 4-
3.
84
Table 4-3 Summary of the sample mixtures and corresponding designations
Water/FA FA/Loess Alkaline

Precursor
Samples Si/Al Si/Na Si/K (w%)
(w%) (w%) activator FA+Loess
K-1 2.56 1.77 0.3 10 KOH 40
K-2 2.56 1.77 0.3 20 KOH 40
K-3 2.56 1.77 0.3 30 KOH 40
Na-1 2.5 1.0 0.35 10 NaOH 40
Na-2 2.5 1.0 0.35 20 NaOH 40
Na-3 2.5 1.0 0.35 30 NaOH 40
Note: FA refers to fly ash.
4.2.4 Loess stabilization with geopolymer
4.2.4.1 Sample preparation
The loess soil was pre-mixed with fly ash before the introduction of precursor. When a
homogeneous mixture was made, the geopolymer stabilized loess was casted into
cylindrical molds which have an inner diameter of 20mm and a height/diameter ratio of
2.5 to minimize the end effects. The samples were demolded after 48 hours. Samples
were always wrapped with plastic film and cured at the ambient temperature (23 ℃). Five
replicates were casted for each group to ensure the repeatability.
4.2.4.2 Characterization
After cured for 7 days, the geopolymer stabilized loess samples were unwrapped for the
unconfined compression tests using an automated GeoTac loading frame (Trautwein Soil
85
Testing Equipment, Inc., USA) at a constant strain rate of 2%/min. The mechanical
properties of the samples in each group are averaged with eliminations of the largest and
lowest values. Figure 4-2 shows a typical stress-strain curve of the stabilized loess from
the UCS test. According to ASTM E 111(ASTM, 2009), the Young’s modulus could be
determined by the tangent modulus with the stress-strain curve from UCS test. Due to the
uneven end surfaces of the sample, there is an stiffening effect at the initial stage and a
tangent modulus of the following linear part of the curve should be used for the
determination of the Young’s modulus (Zhang et al., 2013).

Stress
Young's Modulus
Strain
Figure 4-2 Determination of the Young’s Modulus from a typical stress-strain curve
In order to investigate the composition-microstructure-strength relationship, the crushed
samples were taken for further investigations after the UCS test. The microstructural
86
characterization was performed with the aid of a FEI Quanta 3D FEG scanning electron
microscope. Chemical elemental analyses were also performed by a built-in energy-
dispersive X-ray spectroscopy (EDXS) detector on interested areas or spots of the
observed samples. Particular interests include the elemental composition of individual
particles and the cementing agents bonding particles. For each group of stabilized loess,
small pieces from the cylindrical specimens after the UCS test were selected to prepare
samples for SEM examination. The internal surface of the failed specimens was selected
to ensure the typical microstructure of the geopolymer stabilized loess. The samples were
sputter-coated with a thin layer of gold-palladium alloy before the SEM examination.
X-ray diffraction (XRD) was performed to characterize the mineralogical changes. Both
the original loess sample and the stabilized loess samples were analyzed to positively
identify their mineralogy. All the samples were ground by hand in a mortar with a pestle
before passing through a No.340 sieve (i.e., a mesh opening size of 44 μm). The ground
powder samples were then separately side-loaded into a sample holder for the XRD test.
A Cu Kα radiation was employed to scan the powder samples. The diffraction patterns
were analyzed and identified by the Jade 9.3.3 Program (Material Data, Inc.).
4.3 Results and discussion
4.3.1 Mechanical properties
It is recognized that the natural loess with low moisture content is of good engineering
properties, unless wetted or saturated (Dijkstra et al., 1995; Mansour et al., 2008; Muñoz-
Castelblanco et al., 2012; Parsons et al., 2009). Hence, the UCS testing applied in this
study is mainly used to investigate the composition-microstructure-strength relationship
87
in the stabilized loess samples and a comparison of the mechanical properties between
natural loess and stabilized loess are not made here.
UCS, failure strain ,- , and the Young’s modulus E of the stabilized loess samples with a
curing of 7 days are shown in Figures 4-3, 4-4, and 4-5. From Figure 4-3, it is indicated
that the UCS value of geopolymer stabilized increases with the addition of precursor for
the same alkaline activator. This could be attributed to the production of geopolymer
which provides a strong cementation between the loess particles and contributes to the
strength of stabilized loess. It is noticed that the increase in UCS values is
disproportionate, i.e., (UCS5 − UCS57 ) < (UCS5 − UCS5 ) and (UCS9: −
UCS9:7 ) < (UCS9: − UCS9: ). This is probably because the precursor is
consumed in the geopolymerization process by the increasing addition of fly ash while
the quantity of precursor is the same for all the samples. In other words, more precursor
maybe need to be added if a high fly ash/loess ratio is applied. With a comparison
between the two different precursors, potassium hydroxide activated geopolymer (PHG)
renders a higher UCS value than the sodium hydroxide activated geopolymer (SHG) to
the mixtures with the same fly ash/loess ratio. However, it can also be seen that the
difference between the UCS values of K-1 and Na-2 is very small, which means that an
approximate value of UCS could be rendered to the stabilized loess by increasing the
ratio of fly ash/loess though different alkaline activators are used.
Figure 4-4 shows that the failure strain of geopolymer stabilized loess decreases with the
ratio of fly ash/loess for both PHG and SHG. By comparing K-1 and Na-2, it can be seen
that the failure strain of K-1 is higher than Na-2 (their UCS values are comparative),
88
which means that potassium hydroxide renders a more ductile mixture than sodium
hydroxide when the strength is relative low.
8
7
6
UCS (MPa)
5
4
3
2
1
0
K-1 K-2 K-3 Na-1 Na-2 Na-3
Soil Samples
Figure 4-3 Unconfined compressive strength (UCS) of geopolymer stabilized loess
4
Failure Strain εf (%)
0
K-1 K-2 K-3 Na-1 Na-2 Na-3
Soil Samples
Figure 4-4 Failure strain of geopolymer stabilized loess
89
0.6
Young's Modulus E (GPa) 0.5
0.4
0.3
0.2
0.1
0
K-1 K-2 K-3 Na-1 Na-2 Na-3
Soil Samples
Figure 4-5 The Young’s modulus of geopolymer stabilized loess
Figure 4-5 shows the Young’s moduli of the geopolymer stabilized loess samples. It can
be seen that the Young’s modulus increases with the ratio of fly ash/loess for both two
different precursors. This is due to the increasing amount of geopolymer synthesized in
the mixture. The significant difference between K-3 and K-2 means that a much more
uniform structure frame was formed by the geopolymer in K-3 while the geopolymer
synthesized in K-2 was inadequate for the formation of such strong structure frame. For
the SHG stabilized samples, a preliminary structure frame might have been formed in Na-
2 and the further addition of fly ash enhances the formation of geopolymer gel frame in
Na-3.
4.3.2 Characterization of microstructure
Figure 4-6 shows the micromorphology of the natural loess, fly ash, and geopolymer
stabilized loess samples. The micro-cracks shown in the images of stabilized samples
could be due to the stress during UCS testing or the shrinkage during curing. It can be
90
observed that the geopolymer stabilized loess is of a much denser microstructure than the
natural loess sample in which a metastable open structure has been widely recognized.
With the increasing ratio of fly ash/loess, a more and more compact microstructure was
rendered in the mixture. The higher degree of binding and more compact microstructure,
which agree well with the increase in UCS values and Young’s modulus, testify the
improvement of stabilization with a higher fly ash/loess ratio. Considerable quantities of
unreacted fly ash particles were noticed in K-3 with a comparison to K-2 and K1. This
helps explain the disproportionate increase of UCS, failure strain and Young’s modulus
in the stabilized loess samples. To further improve the mechanical properties of the
stabilized loess, efforts are required to ensure the full reaction of fly ash in the synthesis
of geopolymer.
The EDXS was applied to characterize the chemical compositions of the particles and the
cementation between particles to enhance the understanding of the microstructure of
geopolymer stabilized loess samples. An illustration of the characterization on K-1 is
demonstrated by Figures 4-7 and 4-8, though all the samples were studied with EDXS.
Due to the coating on the stabilized samples, the elements gold Au and palladium Pd are
eliminated from the results and not listed in the EDXS spectra.
Figure 4-8 (a) shows the EDXS spectrum of the selected area a in Figure 4-7. The
spectrum identifies that this area mainly contains the element O, Na, Al, Si, K, Ca, and Fe.
These elements are the primary ingredients of the potassium hydroxide activated (with
sodium silicate solution) fly ash geopolymer gel, which indicates that the area a is the
synthesized geopolymer.
91
Figure 4-6 SEM images of the natural loess, fly ash, and geopolymer stabilized loess
Figure 4-7 Illustration of the applied locations (sample K-1) in the EDXS characterization
92
a
×1000
120
Si
90
60 O
Al
30 Na
K
Ca
Fe
0 KeV
0 1 2 3 4 5 6 7 8
b
×1000
200
Si
150
100
50
O
0 KeV
0 1 2 3 4 5 6 7 8
c
×1000
90
Si
60
Al
O Ca
30
Mg
K
Na Ti Fe
0 KeV
0 1 2 3 4 5 6 7 8
Figure 4-8 The EDXS spectra of the selected areas in Figure 4-7
93
By comparing with SEM images of natural loess and fly ash which are shown in Figure
4-6, the selected area b and c in Figure 4-7 for the EDXS characterization is probably the
quartz particle from loess and fly ash particle, respectively. As identified by the EDXS
spectrum in Figure 4-8 (b), the chemical compositions of area b are mainly Si and O. For
the selected area c, the identified elements in the spectrum (Figure 4-8 (c)) match well
with the compositions of fly ash. These results validate that the selected area b and c in
Figure 4-7 is the quartz particle from loess and fly ash particle, respectively. From this
illustration, it can be observed that the synthesized geopolymer gel works as a binder
between the particles to form a compact microstructure in the stabilized loess.
Figure 4-9 shows the XRD patterns of geopolymer stabilized loess samples. A broad
hump, which identifies the synthesis of geopolymer, is characterized at XRD patterns of
all the geopolymer stabilized loess samples from 5º to 32º 2θ. There is no significant
difference between the XRD patterns of the geopolymer stabilized loess samples. It
means that there is no new/different mineral produced by the different alkaline activators,
though the synthesized amorphous geopolymers are different. By comparing with the
original loess sample, the peaks of N and M almost disappeared in the XRD patterns of
geopolymer stabilized loess samples. This is because of their low intensities and the
masking effect of the broad hump. It could hence be concluded that it is the binding
effect of geopolymer that renders the improvements in the mechanical properties of
stabilized loess.
94
Na-3
Na-2
Intensity
Na-1
K-3
K-2
K-1 Q
M Q A
N A Ca Q Q
N
Loess
0 10 20 30 40
2θ (°)
Figure 4-9 The XRD patterns of geopolymer stabilized loess samples

(M = muscovite, N = nimite, Q = quartz, A = albite, Ca = calcite)
4.3.4 Conceptual microstructural model
An integrated synthesis of the results on the mineralogy, elemental composition, and
microscopy observations provides a clear understanding of the microstructure. Based on
the developed understanding, a conceptual microstructure model is proposed to
demonstrate the mechanism of geopolymer loess stabilization within a representative
volume element (RVE) (Figure 4-10). A RVE of natural loess is illustrated to ease
interpretation and understanding. Clay particles and silt particles, which are the primary
components of natural loess, usually agglomerate together to form clay aggregates or
clay-silt aggregates to provide load bearing capacity. Due to its special formation process,
95
the natural loess has been characterized with an open metastable structure and the
mechanical properties depend significantly on the suction or the cementation between
particles. However, clay bond/cementation and suction will be deteriorated and finally
leads to a collapsing behavior when loess is wetted or subjected to increasing applied
stresses (Assallay et al., 1997; Delage et al., 2005; Jefferson et al., 2005; Muñoz-
Castelblanco et al., 2012; Phien-wej et al., 1992; Wang et al., 2014; Wen and Yan, 2014).
With the introduction of fly ash and precursor (alkali + sodium silicate solution), a
cementitious aluminosilicate gel, which bonds its surrounding particles, is synthesized in
the mixture. During the curing period, the geopolymer gel grows and forms a solid binder.
Due to the high binding energy of geopolymer gel, a compact and stable structure is
finally rendered in the stabilized loess.
Clay particle Silt particle Fly ash Precursor
Cementation Unreacted fly

ash particles
Synthesized
Interaggregate geopolymer
pore
A RVE of natural loess A RVE of geopolymer stabilized loess
Figure 4-10 A conceptual microstructure model of geopolymer stabilized loess
96
4.4 Conclusions
This papers presents an experimental feasibility study of applying fly ash based
geopolymer for the stabilization of collapsible loess soil. Two alkaline activators were
employed to synthesize the fly ash based geopolymers. To investigate the effectiveness,
three fly ash/loess ratios were applied for the loess stabilization. The mechanical tests,
microstructure characterization, and mineralogical analysis showed that a compact and
stable microstructure was developed in the stabilized loess by the synthesis of
geopolymer.
The compression test shows that PHG renders a higher UCS value, higher failure strain,
and Young’s modulus than SHG for the samples with the same fly ash/loess ratio. For
both PHG and SHG, an increase in the UCS value and Young’s modulus, and a decrease
in the failure strain have been observed for the increasing fly ash/loess ratio. However,
the increase/decrease is disproportionate to the increase of fly ash/loess ratio. It is due to
the inadequacy of precursor in the mixture with a high portion of fly ash. This is
validated by the increasing quantities of unreacted fly ash particles in the microscopical
characterization. It is unveiled by the XRD analysis that the there was no new/different
mineral introduced to the mixtures, except the amorphous geopolymer gel. All the
test/analysis results indicate that it is the binding effect of geopolymer gel that renders the
improvements in the mechanical properties of stabilized loess samples.
4.5 References
Arrua, P., Aiassa, G., Eberhardt, M., 2012. Loess soil stabilized with cement for civil
engineering applications. International Journal of Earth Sciences and Engineering 5,
10-17.
97
Assallay, A.M., Rogers, C.D.F., Smalley, I.J., 1997. Formation and collapse of
metastable particle packings and open structures in loess deposits. Engineering
Geology 48, 101-115.
ASTM, 2009. Annual Books of ASTM Standards. ASTM International, West

Conshohocken, PA.
Cristelo, N., Glendinning, S., Fernandes, L., Pinto, A.T., 2012. Effect of calcium content
on soil stabilisation with alkaline activation. Construction and Building Materials 29,
167-174.
Cristelo, N., Glendinning, S., Pinto, A.T., 2011. Deep soft soil improvement by alkaline
activation, Proceedings of the ICE - Ground Improvement, pp. 73-82.
62, 32-39.
540.
Derbyshire, E., Wang, J., Meng, X., 2000. A treacherous terrain: background to natural
hazards in northern China, with special reference to the history of landslides in
Gansu Province. Landslides in the thick Loess Terrain of north-west China. Wiley,
New York 19.
49-64.
2917-2933.
Houston, S., Houston, W., Zapata, C., Lawrence, C., 2001. Geotechnical engineering
practice for collapsible soils. Geotechnical and Geological Engineering 19, 333-355.
Jefferson, I., Evstatiev, D., Karastanev, D., 2008. The treatment of collapsible loess soils
using cement materials. ASCE Geo Congr 2008, 662-669.
98
Jefferson, I., Rogers, C., Evstatiev, D., Karastanev, D., 2005. Treatment of metastable
loess soils: Lessons from Eastern Europe, in: Buddhima, I., Jian, C. (Eds.), Elsevier
Geo-Engineering Book Series. Elsevier, pp. 723-762.

Kim, B., Choi, H., Kang, K., Yi, C., 2011. Characteristics of Natural Loess (Hwangtoh)
Paste Subjected to Geopolymerization. Journal of the Korea Concrete Institute 23,
121-127.
Li, P., Li, H., Liu, H., Wang, X., 2011. Application for quick lime improving strength of
loess subgrade, 2011 International Conference on Structures and Building Materials,
ICSBM 2011, January 7, 2011 - January 9, 2011. Trans Tech Publications,
Guangzhou, China, pp. 2678-2682.

Mansour, Z., Chik, Z., Taha, M., 2008. On Soil Collapse Potential Evaluation, ICCBT,
Kuala Lumpur, pp. 21-31.
Mei, L.H., Min, W.L., Peng, G., 2014. The mechanical properties of cement reinforced
loess and pore microstructure characteristics, 2013 2nd International Conference on
Mechatronics and Computational Mechanics, ICMCM 2013, December 30, 2013 -
December 31, 2013. Trans Tech Publications, Frankfurt, Germany, pp. 25-30.
Metelková, Z., Boháč, J., Přikryl, R., Sedlářová, I., 2012. Maturation of loess treated with
variable lime admixture: Pore space textural evolution and related phase changes.
Appl. Clay Sci. 61, 37-43.
Muñoz-Castelblanco, J.A., Pereira, J.M., Delage, P., Cui, Y.J., 2012. The water retention
properties of a natural unsaturated loess from northern France, Géotechnique, pp. 95-
106.
Parsons, R.L., Johnson, R.M., Brown, D.A., Dapp, S., Brennan, J.J., 2009.
Characterization of Loess for Deep Foundations. DFI Journal: The Journal of the
Deep Foundations Institute 3, 14-24.
Phien-wej, N., Pientong, T., Balasubramaniam, A.S., 1992. Collapse and strength
characteristics of loess in Thailand. Engineering Geology 32, 59-72.
99
Wang, X., Zhu, Y., Huang, X., 2014. Field Tests on Deformation Property of Self-
Weight Collapsible Loess with Large Thickness. International Journal of
Geomechanics 14, 04014001.
Wen, B.-P., Yan, Y.-J., 2014. Influence of structure on shear characteristics of the
unsaturated loess in Lanzhou, China. Engineering Geology 168, 46-58.
White, D., Harrington, D., Thomas, Z., 2005. Fly ash soil stabilization for non-uniform
subgrade soils, Volume I: Engineering properties and construction guidelines. Iowa
Highway Research Board Report: IHRB Project TR-461.
Zhang, L., 2013. Production of bricks from waste materials – A review. Construction and
Building Materials 47, 643-655.
Materials 47, 1468-1478.
Zia, N., Fox, P.J., 2000. Engineering properties of loess-fly ash mixtures for roadbase
construction. Transportation Research Record: Journal of the Transportation
Research Board 1714, 49-56.
100
CHAPTER 5 NUMERICAL ANALYSIS OF THE STRESS
DISTRIBUTION ALONG ITZS IN RECYCLED AGGREGATE
CONCRETE UNDER UNIAXIAL COMPRESSION*
5.1 Introduction
As an effective way to preserve environment and natural resources, recycled aggregate
concrete (RAC) has attracted tremendous attention from engineering practice and
academic research in treating the construction and demolition waste throughout the world
(Casuccio et al., 2008; Kawano, 2003; Li, 2008; Rao et al., 2007; Sagoe-Crentsil et al.,
2001; Xiao et al., 2012a). Differences between the conventional concrete and RAC have
been characterized by the previous studies. For example, Poon et al. (2004) conducted an
experimental investigation on both RAC and conventional concrete and found that the
microstructure of RAC is different from that of conventional concrete. With the
increasing studies of RAC, it has been generally recognized that at the micro/mesoscale,
there are five constitutional phases (natural aggregate, old ITZ, old cement paste, new
ITZ, and new cement paste) in the recycled concrete, in contrast to that there are only
three phases (natural aggregate, ITZ, and cement paste) in the conventional concrete.
This recognition has led to an argument that the failure mechanism of RAC could be
changed due to the introduction of the two additional phases in the constituents. For the
conventional concrete, the failure mechanism has been attributed to the initiation,
propagation, and coalescence of the microcracks and the ITZ has been identified as the
weakest link in the concrete mixture (Agioutantis et al., 2000; Bentz et al., 1994; Gao et
*
Material partially reprinted from Liu et al. (2015) with permission from ASCE Journal
of Materials in Civil Engineering.
101
al., 2014; Garboczi and Bentz, 1996; Garboczi and Bentz, 1997; Mondal et al., 2009;
Ramesh et al., 1998; Rangaraju et al., 2010; Xiao et al., 2013a; Xiao et al., 2012b; Zhou
and Hao, 2008). This means that investigation of the stress distribution within the
composite, especially along the ITZs would be beneficial to the understanding of the
failure mechanism of RAC. As such, a numerical analysis of the stress distribution along
ITZs is conducted in this study, based on the representative volume element of RAC.
5.2 Representative volume element
Previous studies unveiled that there are five phases in RAC, i.e., natural aggregate, OITZ,
old cement paste, NITZ, and new cement paste (Li et al., 2012; Tam et al., 2005; Xiao et
al., 2013a; Xiao et al., 2012b). Based on this understanding, a representative volume
element of RAC is illustrated in Figure 5-1.
New
Cement Paste
Figure 5-1 Representative volume element of RAC
In order to investigate the failure mechanisms of concrete, there are two general ways, i.e.,
experimental and numerical. Numerical investigations can usually be divided into three
scales, i.e., macroscale, mesoscale, and microscale. The present study is concerned with
102
the microscale, at which concrete is defined as a composite consisting of aggregates,
ITZs, and cement paste(s), using the representative volume element to understand the
mechanical behavior of RAC. It should be noticed that an aggregate in the circle shape is
employed in this investigation for the sake of simplicity, though the shape of aggregates
varies in the real concrete.
5.3 Stress concentration factor
Studies show that a mechanical failure often correlates with the stress concentration in
the material, which prompts the stress concentration factor (SCF) to be an effective way
to demonstrate the localized stress variations (Adom-Asamoah and Owusu Afrifa, 2013;
Dai et al., 2012; Deng and Lee, 2007; Kobelev, 1992; Varellis and Norman, 1994; Xiao
et al., 2013a). SCF is therefore chosen to characterize the stress distribution in this study.
According to the definition, the SCF is the ratio of the localized stress to the nominal
stress along the path, as shown in Eq. (5-1).
; = <=>?@=ABCD /<E (5-1)
where F is the stress concentration factor (SCF), GHIJ:HKLMN is the localized stress, and GO
is the nomial stress along the path.
5.4 Numerical model
Previous investigations indicate that the thickness of ITZs in the concrete has significant
effects on the mechanical behavior of the concrete, such as the compressive strength and
the development of cracks in concrete under compression (Bentz et al., 1994; Demie et
al., 2013). Xiao et al. (2013a) studied the amount effect of old hydrated cement paste in
103
RAC and found that the mechanical properties of the entire concrete sample could be
changed by various amount of old hydrated cement paste. In order to eliminate these
effects, the thickness of ITZs and old hydrated cement paste in RAC is set as constant
throughout the study, i.e., 50 µm and 5mm, respectively. The schematics of numerical
models are shown in Figure 5-2 and Figure 5-3. Quadrilateral plane stress elements
(CPS4R) is employed in meshing, as demonstrated by Xiao et al. (2013a). A uniaxial
loading pressure of 20 MPa is applied to the numerical model for the investigation. The
material properties defined in the numerical analysis are list in Table 5-1, as provided in
Xiao et al. (2013a) and is designated as Model 1 in the present study.
9 mm
56 mm
Figure 5-2 Schematic of the numerical model with a circular aggregate
Figure 5-3 Finite element model of RAC with a circular aggregate
104
Table 5-1 Material properties defined in the numerical analysis
Natural Old hydrated New hydrated

Sample OITZ NITZ
Model aggregate cement paste cement paste
dimension
number E E E E E
(mm) υ υ υ υ υ
(GPa) (GPa) (GPa) (GPa) (GPa)
1 56×56 70 0.16 17.5 0.2 25 0.22 16.1 0.2 23 0.22
5.5 Results and discussions
5.5.1 SCF distribution along ITZs
Figure 5-4 shows the result of SCF along the ITZs in RAC. It can be observed that the
SCF varies smoothly along both the OITZ and NITZ, though different characteristics
could be identified. For the OITZ, the maximum SCF is located around 150° and 210°.
However, the maximum SCF is located at 180° in the NITZ. It can also be observed that
a slightly larger value of SCF is developed at the bottom than that at the top for both the
OITZ and NITZ. From the top and bottom, the SCF decreases smoothly to the horizontal
center symmetric axis along the ITZs with the minimum value located at the most right
point (90°) and the most left point (270°) of the circle. This means that the bottom part of
the circle tends to crack first, which agrees with the results by Zhou and Hao (2008) that
the cracks always initiate at the bottom part of the specimen and subsequently propagate
vertically. The reason for a higher value of SCF at the bottom than the top will be
discussed later with the analysis of the influence of the model size.
105
Figure 5-4 Distributions of SCF along the ITZs in Model 1
5.5.2 Influence of model size
15 mm
68 mm
Figure 5-5 Schematic of the extended model (Model 2 and Model 3)
106
Table 5-2 Material properties in the extended model
Natural
OITZ Old hydrated NITZ New hydrated
Model Sample
aggregate
number dimension cement paste cement paste
E υ E υ E υ E υ E υ
(GPa) (GPa) (GPa) (GPa) (GPa)
2 68mm×68mm 70 0.16 17.5 0.2 25 0.22 16.1 0.2 23 0.22
3 68mm×68mm 70 0.16 17.5 0.2 25 0.22 17.5 0.2 23 0.22
In order to investigate the influence of model sizes, the model is extended from
56mm×56mm (Model 1) to 68mm×68mm (Model 2) as shown in Figure 5-5, with the
material properties being given in Table 5-2. It should be noticed that the recycled
aggregate (including all four phases: natural aggregate, OITZ, old hydrated cement paste,
and NITZ) remains the same dimension during the size extension. Figure 5-6 shows the
distributions of SCF along the ITZs in Model 2 with a circular aggregate. With a
comparison between Figure 5-4 and Figure 5-6, it can be found that the SCFs are almost
the same except at the bottom of the ITZs (165°-195°), which means that the larger value
of SCF at the bottom of the ITZs in Figure 5-4 is mainly caused by the smaller distance
between the aggregate and the bottom boundary of the model. In other words, the top part
of ITZs could have the same priority for crack initiation if the distance from the
aggregate to the boundaries is increased.
107
108
5.5.3 Influence of property of ITZs
Since the strength ratio of OITZ and NITZ may be of significance to the behavior of
recycled aggregate concrete and some studies have been focused on the improvements in
the mechanical properties of NITZ (Xiao et al., 2013b), the Young’s modulus of the
NITZ is increased to analyze the influence from the properties of ITZs (Model 3 in Table
109
5-2). The results of SCF along the ITZs in Model 3 with a circular aggregate are
presented in Figure 5-7. A comparison between Figure 5-4 and Figure 5-7 indicates that
this change in the Young’s modulus of the NITZ has limited influence on the
distributions of SCF. A similar finding has also been reported by Xiao et al. (2013a).
5.4.4 Comparison of the maximum of SCF in OITZ and NITZ
Table 5-3 summarizes the maximum of SCF in OITZ and NITZ for all the three models.
It can be observed that the NITZ has a higher value of the maximum of SCF than the
OITZ for the single circular aggregate model applied in this study. It means that the
introduction of NITZ in the RAC is detrimental to the performance of RAC, and could
even contribute more to the mechanical failure of RAC at the microscale than the OITZ.
This promotes that how to recycle the waste concrete without the introduction of NITZ
would be of great significance to the improvement of RAC.
Table 5-3 Maximum of SCF in OITZ and NITZ
OITZ NITZ
Model 1 1.286 1.370
Model 2 1.270 1.320
Model 3 1.270 1.325
5.5 Conclusion
A microscale model of recycled aggregate concrete is employed to investigate the stress
distribution factor along both the new interfacial transition zone (NITZ) and the old
110
interfacial transition zone (OITZ) under uniaxial compression. Based on the results, the
following observations have been made.
(1) The bottom part of ITZ is characterized with a higher SCF for the Model 1,
which means that the bottom part may crack earlier than the other locations of the
ITZs. However, the same crack initiation could be developed at the top of ITZs by
increasing the distance between the aggregate and boundaries.
(2) It is observed that the NITZ has a higher value of the maximum of SCF than
the OITZ for all the single circular aggregate models applied in this study. It
means that the introduction of NITZ in the RAC plays a detrimental role to the
performance of RAC, and could even contribute more to the mechanical failure of
RAC at the microscale than the OITZ. This implies that how to recycle the waste
concrete while reducing or avoiding the development of NITZ would be of great
significance to the improvement of RAC.
5.6 References
Adom-Asamoah, M., Owusu Afrifa, R., 2013. Shear behaviour of reinforced phyllite
concrete beams. Materials & Design 43, 438-446.

111
Dai, Q., Ng, K., Zhou, J., Kreiger, E.L., Ahlborn, T.M., 2012. Damage investigation of
single-edge notched beam tests with normal strength concrete and ultra high
performance concrete specimens using acoustic emission techniques. Construction
and Building Materials 31, 231-242.
Demie, S., Nuruddin, M.F., Shafiq, N., 2013. Effects of micro-structure characteristics of
interfacial transition zone on the compressive strength of self-compacting
geopolymer concrete. Construction and Building Materials 41, 91-98.
Deng, J., Lee, M.M.K., 2007. Behaviour under static loading of metallic beams
reinforced with a bonded CFRP plate. Composite Structures 78, 232-242.
Gao, Y., De Schutter, G., Ye, G., Tan, Z., Wu, K., 2014. The ITZ microstructure,
thickness and porosity in blended cementitious composite: Effects of curing age,
water to binder ratio and aggregate content. Composites Part B: Engineering 60, 1-13.
Kobelev, V.V., 1992. Microstructural Model of a Fibrous Composite Fracture. Mechanics

of Structures and Machines 20, 1-16.
Li, W., Xiao, J., Sun, Z., Shah, S.P., 2012. Failure processes of modeled recycled
aggregate concrete under uniaxial compression. Cement and Concrete Composites 34,
1149-1158.
315-320.
Ramesh, G., Sotelino, E., Chen, W., 1998. Effect of Transition Zone on Elastic Stresses
in Concrete Materials. Journal of Materials in Civil Engineering 10, 275-282.
112
707-712.
Tam, V.W.Y., Gao, X.F., Tam, C.M., 2005. Microstructural analysis of recycled
aggregate concrete produced from two-stage mixing approach. Cem. Concr. Res. 35,
1195-1203.
Varellis, I., Norman, T.L., 1994. Failure of unnotched and notched composites with
adhesive strips. Composites Science and Technology 51, 367-376.
Xiao, J., Li, W., Corr, D., Shah, S., 2013a. Simulation Study on the Stress Distribution in
Xiao, J., Li, W., Corr, D.J., Shah, S.P., 2013b. Effects of interfacial transition zones on
the stress–strain behavior of modeled recycled aggregate concrete. Cem. Concr. Res.
52, 82-99.
Xiao, J., Li, W., Poon, C., 2012a. Recent studies on mechanical properties of recycled
Xiao, J., Li, W., Sun, Z., Shah, S.P., 2012b. Crack propagation in recycled aggregate
concrete under uniaxial compressive loading. ACI Materials Journal 109, 451-462.
Zhou, X.Q., Hao, H., 2008. Mesoscale modelling of concrete tensile failure mechanism at
high strain rates. Computers & Structures 86, 2013-2026.
113
CHAPTER 6 INVESTIGATION OF THE PROPERTIES OF THE
GEOPOLYMERIC RECYCLED AGGREGATE CONCRETE
6.1 Introduction
Every year there is huge amount of construction and demolition waste (C&D waste)
produced around the world due to the demolition and rehabilitation of civil infrastructures.
Among the C&D waste, waste concrete accounts a significant portion, which could be up
to 33% (Li, 2008). On the other hand, qualified aggregates for the production of concrete
are becoming depleted, which prompts the incorporation of recycled aggregates in the
production of concrete to be an effective way for both the treatment of C&D waste and
the preservation of environmental and natural resources. In the past years, recycled
aggregate concrete (RAC) has attracted tremendous attention in both engineering practice
and academic research (Casuccio et al., 2008; Kawano, 2003; Li, 2008; Rao et al., 2007;
Sagoe-Crentsil et al., 2001; Xiao et al., 2012a). However, most of the studies focused on
the incorporation of coarse recycled aggregates into the production of RAC. The
development of incorporating all recycled aggregates, i.e., both the coarse recycled
aggregates and fine recycled aggregates, into RAC is still lagging. This is mainly due to
the inherent characteristics of fine recycled aggregates, including the different
constituents, the lower particle density, the high water absorption rate, and the greater
angularity as compared to the fine natural aggregates (Chan, 1998; Evangelista and de
Brito, 2007; Katz, 2003; Leite, 2001; Pereira et al., 2012). New methods including
additives, new cements, and/or new procedures are therefore being called for the
recycling of waste concrete.
114
At the same time, the study of geopolymer materials reaches a new era. Geopolymer,
which was coined by Davidovits in the late 1970’s, is an inorganic material formed by
alkaline activation of aluminia- and silica-containing materials through a
polycondensation process in which the tetrahedral silica (SiO2 ) and alumina (AlO4 ) are
linked with each other via sharing the oxygen atoms (e.g., (-Si-O-Al-O-)n ,
(-Si-O-Al-O-Si-O-)n , and (-Si-O-Al-O-Si-O-Si-O-)n ). A general chemical structure of
geopolymer could be expressed as (Khale and Chaudhary, 2007; Ryu et al., 2013; Zhang
et al., 2013):
n
the Si/Al ratio.
Previous research revealed that geopolymers with high compressive strength, low
shrinkage, good acid resistance, and good fire resistance could be synthesized from a
variety of low cost materials or industrial wastes, such as metakaolin, fly ash, rice husk
ash, and furnace slag (Deb et al., 2014; Duxson et al., 2007; Majidi, 2009; Posi et al.,
2013; Rangan et al., 2005). These characteristics render geopolymers promising
potentials in civil engineering applications. With the incorporation of geopolymers, the
production of RAC could be turned into a full “green” process while recycling the wastes
and reducing the greenhouse gas emissions caused by the industry of Portland cement at
the same time. Furthermore, it has been unveiled that water is not involved in the
chemical reaction but only works to facilitate the workability of the concrete mixture
(Davidovits, 2011; Lloyd and Rangan, 2009), which is contrary to the involvement of
115
water in the hydration process when ordinary Portland cement is applied for the
production of concrete. This leads to a new perspective for the incorporation of fine
recycled aggregates in the production of concrete if proper design is applied.
Figure 6-1 Constitutive phases in the conventional concrete (left) and the recycled
aggregate concrete (right)
Previous studies also revealed that there are 3 phases (natural aggregate, ITZ, and cement
paste) in the conventional concrete and 5 phases (natural aggregate, old ITZ, old cement
paste, new ITZ, and new cement paste) in the recycled concrete as shown in Figure 6-1.
Among all the phases, the ITZs have been identified as the weakest link in the concrete
mixture and the new ITZ (NITZ) is recognized as one of the most important constitutive
phases in RAC for its contribution to the failure mechanism of RAC (Agioutantis et al.,
2000; Bentz et al., 1994; Gao et al., 2014; Garboczi and Bentz, 1996; Garboczi and Bentz,
1997; Mondal et al., 2009; Ramesh et al., 1998; Rangaraju et al., 2010; Xiao et al., 2013a;
Xiao et al., 2012b; Zhou and Hao, 2008). However, an updated study by Sidorova et al.
(2014) found that NITZ is not well formed in their RAC samples. This would lead to two
116
research interests in RAC: improving the properties of RAC by avoiding the formation of
NITZ and its corresponding failure mechanism.
Therefore, as a research effort on the development of “green” materials in civil
engineering applications, this paper describes an experimental study of a geopolymeric
recycled aggregate concrete in which the natural aggregates were fully replaced by the
coarse recycled aggregates and the fine recycled aggregates. Fly ash, which is an
industrial byproduct and contains large quantities of reactive silicon dioxide and
aluminum dioxide, was selected as the raw material to synthesize geopolymer. Because it
has been found by the previous studies that the characteristics of ITZ are closely
associated with the water/cement (w/c) ratio (Gao et al., 2014; Sidorova et al., 2014;
Yang and Su, 2002), three different w/c ratios were designated in this study to explore the
properties of GRAC specimens, including both the mechanical behavior and the
microstructure. RAC specimens produced with ordinary Portland cement (OPC) were
also studied as a comparison with the GRAC specimens. Compressive strength, Young’s
Modulus, Poisson’s ratio, and density were studied to characterize the physical and
mechanical properties. The microstructure and mineralogy were investigated with the aid
of scanning electron microscopy (SEM) and X-ray diffraction (XRD) technologies. The
technique of nanoindentation was also applied to further discriminate the formation of
NITZ in the RAC specimens.
6.2.1 Recycled aggregates
All the recycled aggregates used in this study were supplied by a local company (Red
Stick Crushed Concrete) where the LADOTD Specification 1003.03 is followed for the
117
production of crushed concrete. Because it is required by the ASTM C192 that the
diameter of a cylindrical specimen should be at least three times the nominal maximum
size of the coarse aggregates, a sieving was conducted to remove the unqualified
aggregates. The final particle size distribution of the employed aggregates is shown in
Figure 6-2. The particle size analysis shows that the recycled aggregates employed in this
study covers a range from fine aggregate to coarse aggregate. With a three-tier
classification, the recycled aggregates consist of 55% coarse aggregate, 18% medium
aggregate, and 27% fine aggregates, as shown in Figure 6-3 and Table 6-1.
100
90
80
70
Percent finer (%)

60
50
40
30
20
10
0
0.1 1 10
Figure 6-2 Particle size distribution of recycled aggregates
118
Figure 6-3 Coarse, medium, and fine recycled aggregates
Table 6-1 Percentages of coarse, medium, and fine aggregates in recycled aggregate
Coarse aggregate Medium aggregate Fine Aggregate
Particle size (mm) 4.75 ≤ d < 20 1.19 ≤ d < 4.75 d < 1.19
Percentage (wt.%) 55 18 27
6.2.2 Fly ash
A Class F fly ash from Boral Material Technologies, Inc. (Monticello, Texas, USA) was
used as the raw material for the synthesis of geopolymer. Based on its chemical
composition analysis (Table 6-2), the Si/Al molar ratio in this class F fly ash is 2.15, with
a specific gravity of 2.46. The particle distribution analyzed through the hydrometer test
is shown in Figure 6-4, which indicates a medium size of approximately 20 µm.
119
Table 6-2 Composition of fly ash (wt.%)
SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2O K2O Loss of ignition Moisture
52.06 20.54 5.50 14.07 3.29 0.57 0.94 0.69 0.10 0.01
100
90
80
70
Percent finer (%)

60
50
40
30
20
10
0
0.00010 0.00100 0.01000 0.10000
Figure 6-4 Particle size distribution of the Class F fly ash
6.2.3 Alkali solution
The properties of geopolymers vary with the raw materials and processing conditions
(Duxson et al., 2007). A preliminary study was therefore conducted to investigate the
properties of geopolymers synthesized from different alkali solutions (i.e., variant Si/Al
molar ratios and water content). A commercial sodium silicate solution consisting of 9.07
wt.% Na2 O and 29.35 wt.% SiO2 (Aqua Solutions Inc, USA) and a sodium hydroxide
(purity quotient: 99%, Sigma-Aldrich Co., USA) were used to prepare the alkali solutions.
120
According to the unconfined compressive strength (28 days curing) test results (Table 6-
3), the sodium hydroxide activated geopolymer synthesized from mixture 3 renders the
highest strength (29.5 MPa). The mixture 3 is hence selected as alkali solution in this
study to investigate the properties of geopolymeric recycled aggregate concrete.
Table 6-3 Mixture combinations for geopolymer synthesis and compressive strength
Water/Fly ash Alkaline Compressive

Mixture Si/Al Si/Na
(wt%) activator strength (MPa)
1 2.50 1.0 0.30 NaOH 28.2
2 2.50 0.67 0.30 NaOH 18.6
3 2.50 1.0 0.35 NaOH 29.5
4 2.50 0.67 0.35 NaOH 19.7
5 2.50 1.0 0.40 NaOH 19.5
6 3.00 0.67 0.74 NaOH 6.4
6.2.4 Geopolymeric recycled aggregate concrete
6.2.4.1 Sample preparation
The recycled aggregates were pre-mixed with fly ash before the introduction of alkali
solution. During the premixing, a value of 2.5 for the ratio of aggregate/fly ash was
applied. When a homogeneous mixture was achieved, the alkali solution and solid
mixture were then mixed and casted into cylindrical molds (4 in. × 8 in.) to prepare the
geopolymeric recycled aggregate concrete (GRAC) specimens by following the ASTM
procedure (ASTM C192). The samples were demolded after 24 hours and further cured
121
for another 27 days at the ambient temperature (about 23 ℃). The full procedure for the
specimen preparation is shown in Figure 6-5. The minimum value of the w/c ratio (w/c is
the ratio of water over fly ash or ordinary Portland cement where it is applied) was
determined by a preliminary study to assure the workability for specimen preparation.
According to the study, the minimum value of the w/c ratio is 0.40 and 0.50 for GRAC
and ordinary Portland cement recycled aggregate concrete (OPC-RAC), respectively. The
w/c ratio was then increased (from 0.40 to 0.45, then to 0.50) to investigate the
characteristics of the mechanical behavior and the microstructure of the GRAC
specimens and the formation of NITZ in GRAC.
Sodium silicate
solution
Sodium Mix
Precursor
hydroxide
Deionized water
Mix
RAC
Cast
Fly ash
(or OPC) Mix
Solid Mixture
Recycled
Aggregates
Figure 6-5 Flow chart of the sample preparation
6.2.4.2 Characterization
The density was measured at a curing of 28 days followed by the compressive strength
tests which were performed on the Forney LT-8061-FTS compression testing machine in
accordance with the ASTM C39 (ASTM, 2014). Triplicate cylinder specimens were
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tested for each designated mixture group. Both the results of density and compressive
strength were averaged for a further analysis.
In order to investigate the composition-microstructure-strength relationship, the crushed
samples were taken for further investigations after the compression test. A
microstructural characterization was performed with the aid of a FEI Quanta 3D FEG
scanning electron microscope. For each group of mixtures, small pieces from the
cylindrical specimens after the compression test were selected to prepare samples for
SEM examinations. The internal surface of the failed specimens was selected to ensure
the typical microstructure of the concrete specimens. The samples were sputter-coated
with a thin layer of gold-palladium alloy before the SEM examination.
X-ray diffraction (XRD) was applied to investigate the mineralogical characteristics of
the fine recycled aggregate and the cement paste in RAC specimens. The cement paste
blocks were ground manually in a mortar with a pestle before passing through a No.340
sieve (i.e., a mesh opening size of 44 μm). The ground powder samples were then
separately side-loaded into a sample holder for the XRD test. A Cu Kα radiation was
employed to scan the powder samples. The diffraction patterns were analyzed and
identified by the Jade 9.3.3 Program (Material Data, Inc.).
The nanoindentation test was conducted to further characterize the interface between the
old cement paste (OCP) and the new cement paste (NCP). Blocks with a dimension of 10
mm × 20 mm × (10-15) mm were cut with a diamond saw disc and then impregnated
with an epoxy resin to prepare the specimens for nanoindentation tests. Afterwards, the
specimens were ground with the silicon carbide papers followed by a fine polishing
123
procedure using a polishing cloth and diamond suspensions. The nanoindentation tests
were performed with an MTS Nano XP indenter with a Berkovich tip. The schematic of
the nanoindentation test is shown in Figure 6-6.
X New Cement Paste

Natural Aggregate
……
……
……
Old Cement Paste
Figure 6-6 Schematic plan view of the nanoindentation test
During the process of nanoindentation, the mechanical properties are measured by
establishing a contact between a diamond tip and the material of interest. With the
records of the indentation load P and the indentation depth h, the indentation modulus & ∗
and the indentation hardness H can be calculated by the eq. (6-1) and eq. (6-2).
7 √+ NT
&∗ = S V (6-1)
Q √* NU UWUXYZ
TX\]
[= *
(6-2)
where ^ is a correction factor for the indentation tip, and _ is the projected contact
area of the indenter tip on the sample surface at the peak load. Finally the elastic
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modulus & of the tested material could be derived through the relationship shown in
eq.(6-3) (Fischer-Cripps, 2011):
7 a7bc d a7b$c d
= + (6-3)
`∗ ` `$
where & e and f e is the elastic modulus and Poisson’s ratio of the indenter, respectively,
and f is the Poisson’s ratio of the tested material.
6.3 Results and discussions
6.3.1 Physical and mechanical properties
Table 6.4 shows the physical and mechanical properties of the recycled aggregate
concrete produced in the present study. For the geopolymeric recycled aggregate concrete,
the highest value of 27.15 MPa, 14.13 GPa, 0.25, and 2124.89 kg/m3 was achieved at the
w/c ratio 0.40 for the compressive strength, Young’s modulus, Poisson’s ratio, and
density, respectively. For the OPC-RAC produced with the ASTM Portland Type I
cement and a w/c ratio of 0.50, in comparison, the value is 25.68 MPa, 21.20 GPa, 0.22,
and 2082.74 kg/m3 for the compressive strength, Young’s modulus, Poisson’s ratio, and
density, respectively.
The comparison between the GRAC and the OPC-RAC specimens shows that the
compressive strength of OPC-RAC is approximately equal to that of GRAC-2, which has
a w/c ratio of 0.45. The highest value of compressive strength achieved by the GRAC
specimen at the w/c ratio of 0.40 is about 6% higher than that of the OPC-RAC
specimens. This means that the fly ash based geopolymer is favorable to reduce the water
content required for the production of recycled aggregate concrete while even rendering a
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higher compressive strength. However, the Young’s moduli for the mixtures GRAC-1
and GRAC-2 are smaller than that of the OPC-RAC specimens. This means that the
GRAC specimens have a more ductile behavior than the OPC-RAC, which could be
helpful when a reduction of the structure brittleness is needed for some specific
applications in civil infrastructures. The results also show that higher values of the
Poisson’s ratio and mass density were obtained to the recycled aggregate concrete by the
fly ash based geopolymer than the ordinary Portland cement.
Table 6-4 Physical and mechanical properties of recycled aggregates concrete
E d
Mixtures w/c gJ (MPa) ν gJ /&
(GPa) (kg/m3)
GRAC-1 0.40 27.15 14.13 0.25 2124.89 1.92
GRAC-2 0.45 25.51 11.03 0.22 2099.09 2.31
GRAC-3 0.50 18.04 1.86 0.17 2081.84 9.70
OPC-RAC 0.50 25.68 21.20 0.22 2082.74 1.21
Note: w/c is the ratio of water over fly ash or ordinary Portland cement where it is applied,
gi is the compressive strength of concrete at 28 days, E is the Young’s modulus, ν is the
Poisson’s ration, and d is the density.
As indicated in Table 6-4, the compressive strength, the Young’s modulus, and the
Poisson’s ratio decrease with the increase of w/c ratio. In order to further investigate this
change, the reduction rates corresponding to the two increases in w/c ratio are herein
compared. Table 6-5 shows that the reduction rates of the physical and mechanical
properties of the GRAC specimens increase with the increase of the w/c ratio. It can be
126
observed that the reduction rate of the compressive strength and Young’s modulus in the
second increase of the w/c ratio (from 0.45 to 0.50) is 29% and 83%, respectively, which
are 3~4 times more than these values rendered by the first increase (from 0.40 to 0.45)
which is 6% and 22%, respectively. It is also observed that the ratio of gJ /& (shown in
Table 6-4) increases dramatically from 1.92 to 2.31 and then to 9.70 when the w/c ratio
increases. The increase rate of gJ /& (Table 6-4) shows that the Young’s modulus is much
more vulnerable to the change of the w/c ratio than the compressive strength. The
reduction rate of the Poisson’s ratio changes from 12% to 23% during the two increases
of the w/c ratio. These significant changes to the geopolymeric recycled aggregate
concrete could be due to the deteriorated properties rendered to the geopolymer by the
increase of w/c ratio, as can be seen in Table 6-3, though the Young’s modulus and the
Poisson’s ratio were not measured during the preliminary study. For the mass density, the
resulted reduction rates are only 1.2% and 0.8%.
Table 6-5 Reduction rates of the physical and mechanical properties of GRAC samples
with the increase of w/c ratio
w/c: 0.40 → 0.45 w/c: 0.45 → 0.50
gJ 6% 29%
& 22% 83%
ν 12% 23%
d 1.2% 0.8%
gJ /& 0.20 3.2
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Figure 6-7 Failure patterns under compression
Figure 6-7 shows the failure patterns of RAC samples under uniaxial compression. The
failure planes are usually developed along inclined planes which have angles ranging
from 50°-80° with respect to the horizontal plane. The major failures were observed to
develop at the bottom of the samples for both the geopolymeric recycled aggregate
concrete and the OPC recycled aggregate concrete. Failures through the coarse recycled
aggregates (i.e., natural aggregates, and the attached old cement paste) have been
observed for all the samples. This may be attributed to: (1) the damage rendered to the
recycled aggregates during the crushing of recycling process; and (2) the lower strength
of the waste concrete. Through the compression test, it is found that GRAC-1 and
GRAC-2 rendered a better integrity to the failed specimens than GRAC-3 and OPC-RAC,
though the compressive strength of GRAC-2 and OPC-RAC are close. For the
geopolymeric recycled aggregate concrete, more and more cracks initiating at the bottom
develop towards the center of the top surface of the GRAC specimens and vertical cracks
128
were observed with the increase in the w/c ratio. The integrity of the failed specimens
becomes more deteriorated as the w/c ratio increases.
6.3.2 Characterization of microstructure
Figure 6-8 SEM images of the recycled aggregate
Figure 6-9 SEM images of the geopolymeric recycled aggregate concrete
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Figure 6-10 SEM images of the OPC recycled aggregate concrete
Figure 6-8 shows the SEM images of the recycled aggregate crushed from waste cement
concrete in the magnifications of 65X and 500X. From the SEM images, it can be seen
that there is an interfacial transition zone, which has a higher porosity, between the OCP
and natural aggregate. Previous research unveiled that the interfacial transition zone (ITZ)
in the conventional natural aggregate concrete is the weakest link with regarding to the
mechanical performance and durability of concrete and its formation is attributed to the
wall effect caused by the natural aggregates (Agioutantis et al., 2000; Bentz et al., 1994;
Gao et al., 2014; Garboczi and Bentz, 1996; Garboczi and Bentz, 1997; Mondal et al.,
2009; Ollivier et al., 1995; Ramesh et al., 1998; Rangaraju et al., 2010; Scrivener et al.,
2004; Xiao et al., 2013a; Xiao et al., 2012b; Zhou and Hao, 2008). During the production
of concrete, mixing and vibration usually lead to an accumulation of water at the vicinity
of the coarse natural aggregates which are several orders bigger in size than the fine
particles in the mixture and acts as walls regarding to the water and fine particles.
Figure 6-9 shows the micromorphology of the geopolymeric recycled aggregate concrete.
The micro-cracks shown in the images could be due to the stress during the compression
130
testing or the shrinkage during the curing process. The interface between the OCP and the
geopolymer cement paste could be clearly identified by the boundary where the spherical
fly ash particles start to absent from one of the two different phases, as indicated by the
dashed lines in the SEM images. It can be observed that the OCP and the synthesized
geopolymer paste are so tightly bonded together that a more porous interfacial transition
zone is hardly to be identified. It means that there might be no NITZ formed between the
OCP and the synthesized geopolymer paste. Because the ITZs have been characterized as
the weakest link in concrete and play an important role in the failure mechanism of
concrete, a further investigation with the technology of nanoindentation is conducted and
discussed later to study the properties of this bonding area.
Figure 6-10 shows the SEM images of the ordinary Portland cement recycled aggregate
concrete. The dashed lines in the images indicate the interface between the OCP and the
NCP. The right picture shows an amplified view of the area marked by the rectangle in
the left picture. From the SEM images, it is hard to observe the porous transition zone
between the OCP and NCP. The only difference between the OCP and the NCP is that
the NCP is darker in color than the OCP. This also potentially indicates that the NITZ
may not be formed in the OPC-RAC specimens.
Figure 6-11 shows the XRD patterns of the OCP from crushed waste concrete and the
NCP from the GRAC specimens. From the XRD pattern of recycled aggregate, it can be
identified that the OCP from the crushed waste concrete mainly consists of quartz and
calcium carbonate, which is different from the composition of the cement paste in the
conventional concrete (i.e., quartz, calcium silicate hydrate, and calcium hydroxide). For
131
the conventional concrete, the hydration products have been identified as calcium silicate
hydrate (C-S-H) and calcium hydroxide. The difference between the composition of the
cement paste in the conventional concrete and the identified composition of the OCP
from the crushed waste concrete could be attributed to two reasons. The calcium silicate
hydrate has been characterized with a notable complexity in its structure. The C-S-H
prepared at a room temperature usually is of a semi-crystalline phase to almost
amorphous phase (Chen et al., 2004). Small humps, instead of the peaks, are herein
granted in the XRD pattern by this characteristic. For the identification of calcium
carbonate, rather than the calcium hydroxide, in the XRD pattern, it could be due to the
carbonation process: Ca(OH)2 + CO2 → CaCO3 + H2 O. During the practice, the waste
concrete is generally crushed and then dumped at an open site. Both the increased
specific area caused by crushing and the environment in the open site would facilitate the
carbonation process of calcium hydroxide.
By comparing the XRD patterns of the OCP from recycled aggregate and the NCP from
the GRAC specimens, it can be seen that there is a broad peak rendered to the XRD
patterns of the NCP in the GRAC specimens from 12º to 40º 2θ. This is due to the
combination of the hump caused by the amorphous geopolymer and the peaks of the
crystalline phases in the NCP. In other words, the amorphous geopolymer has been
successfully synthesized in the GRAC samples. By comparing all the three GRC samples,
there is no significant difference between the XRD patterns of the NCP, which means
that there is no new/different mineral produced in these three GRAC concrete specimens.
132
Calcite
Calcite
Quartz
Quartz
Quartz
GRAC-3
Intensity
GRAC-2
GRAC-1
RA
0 10 20 30 40 50 60 70 80
2θ (°)
Figure 6-11 The XRD patterns of OCP from recycled aggregate and NCP from GRAC
specimens
6.3.4 Nanoindentation
Figures 6-12 to 6-14 show the elastic modulus distributions of the geopolymer cement
paste located around the interface between the NCP and OCP in GRAC samples. Figure
6-15 shows the distribution of elastic modulus around the interface of NCP and the OCP
in the OPC-RAC specimens. From the distribution maps, it could be observed that there
is no significant ITZ identified around the interface of the OCP and the NCP (both the
geopolymer cement paste and ordinary Portland cement paste). The distributions of
hardness (H) (shown in Figures 6-16 to 6-19) of the NCP at the vicinity of the interface
with the OCP also lead to the same observation.
133
Unit: GPa
Figure 6-12 Distribution of the elastic modulus for the GRAC-1 specimen
Unit: GPa
134
Unit: GPa
Unit: GPa
Figure 6-15 Distribution of the elastic modulus for the OPC-RAC specimen
135
Unit: GPa
Figure 6-16 Distribution of the hardness for the GRAC-1 specimen
Unit: GPa
136
Unit: GPa
Unit: GPa
Figure 6-19 Distribution of the hardness for the OPC-RAC specimen
137
6.3.5 Discussion on the mechanism of the non-NITZ formation in RAC
Formation mechanism of ITZ in conventional concrete:
In the conventional concrete, there are quantities of particles which are named as
aggregates and cement grains. The size of cement grains ranges from less than a micron
to several hundred microns, while the aggregate particles are usually several orders larger
than the cement grains. When particles with different sizes are mixed together, the large
ones could not physically cut through the small ones. In other words, the normal packing
of the small grains is disrupted when mixed with the aggregates during the production of
concrete and a new packing of the particles will be created (Figure 6-20): the aggregates
lie beside the small grains as walls with a higher porosity at the vicinity of aggregates.
Moreover, the wall effect usually leads to an accumulation of considerable water at the
vicinity of coarse aggregates during the process of mixing and vibrating the concrete.
Consequently, an interfacial transition zone with higher porosity and higher w/c ratio is
developed between the coarse aggregate and the cement paste (Ollivier et al., 1995;
Scrivener et al., 2004).
Figure 6-20 Illustration of the “wall effect” in concrete

(Adopted from Scrivener et al. (2004): (a) physically impossible packing; (b) aggregate
lies as wall beside the small grains)
138
Recent studies on microstructure of RAC
Table 6-6 Mixture design of concrete in the study of Sidorova et al. (2014)
Moisture ITZ between
Aggregate type Condition of w/c ratio cement paste and
aggregates NA (or RA)
recycled concrete aggregates No
0.3 No
recycled ceramic aggregates
natural aggregates 50 µm
recycled ceramic aggregates Air dried 0.4 No
recycled ceramic aggregates 0.5 No
Sidorova et al. (2014) used the air dried natural aggregates and recycled aggregates to
prepare concrete specimens. The identification of ITZ through nanoindentation in their
study is demonstrated in Figure 6-21. It is found that there is an ITZ developed between
the natural aggregate (NA) and the cement paste, but there is no ITZ well-formed
139
between the recycled aggregate (RA) and new cement paste in the RAC samples though
the same procedure is applied. The design of the mixtures is listed in Table 6-6. It can
also be seen that the increase of w/c ratio from 0.3 to 0.5 has no positive influence on the
development of NITZs in the RAC specimens. This means that the wall effect of recycled
aggregate might disappear or be weakened in this study for the RAC specimens.
Figure 6-21 Demonstration of the ITZ identification with nanoindentation in the concrete
with natural aggregates (adapted from Sidorova et al. (2014))
Table 6-7 shows the identification of the NITZ in other previous studies of RAC. With a
presoaked condition of the recycled aggregates, the NITZ was well formed in all the
listed studies. Based on the formation mechanism of ITZ in conventional concrete, it
could be concluded that the wall effect of recycled aggregate is playing actively in these
studies. It is noted that the TSMA in Table 6-7 refers to the Two-stage mixing approach,
which applies the required water to the mixture in two stages: half of the water is used to
help the cement slurry penetrate into the old cement mortar attached to recycled
aggregates during the first stage, and the other half is added for the complete mixing
(Tam et al., 2005). With the above information, the first stage in the TSMA procedure
could also be considered as a pre-wetting process of the recycled aggregates before the
final mixing.
140
Table 6-7 Identification of NITZ in other previous studies of RAC
ITZ between
Moisture
References cement paste and
Condition of aggregates
RA
(Xiao et al., 2013b; Yes

Presoaked
Xiao et al., 2012b) (60 µm)
Presoaked with a Yes

(Xiao et al., 2013c)
TSMA mixing procedure (55-65 µm)
(Shi et al., 2012) Presoaked Yes
Mixed with a TSMA

(Tam et al., 2005) Yes
procedure
(Cui et al., 2015) Presoaked Yes
Because the formation of ITZ is of non-reference to the chemical composition, the
difference in the raw materials such cement types could be excluded. It could be therefore
concluded that the preparing procedure of RAC specimens plays a significant role in the
development of NITZ between the recycled aggregates and the new cement paste
according to the literature review of the previous studies on RAC, together with the study
presented in this dissertation.
141
a b
Old cement paste

NA
NA
Water accumulates around the aggregate RA Water goes into the old cement paste
Figure 6-22 Illustration of the non-formation mechanism of NITZ in RAC

Note: (a) water accumulates around natural aggregate (NA) in conventional concrete; (b)
water penetrates into the old cement paste in RAC
With the formation mechanism of ITZ in conventional concrete and the representative
volume element of recycled aggregate, the reason why NITZ is not well formed in RAC
could be further explained (Figure 6-22): when the aggregate is presoaked, the capability
of high water absorption of the recycled aggregate will be forfeited. This leads to a
situation that the water and the recycled aggregate work together to form a “wall effect”
which is similar to the one caused by the natural aggregate. During the RAC production,
considerable amount of water is accumulated at the vicinity of recycled aggregate (Figure
6-22(a)). However, with an application of air-dried aggregate, the porous old cement
paste would provide ways for the water to dissipate, i.e., water penetrates into the old
cement paste (Figure 6-22(b)). Hence, the “wall effect” caused by the aggregate is
weakened, which finally inhibits the formation of ITZ between the new cement paste and
the recycled aggregate.
142
Recommendation of the procedure for the GRAC preparation
Most of the previous studies on the recycled aggregate concrete used the presoaked
recycled aggregates during the production of new concrete. This is mainly because of the
high water absorption rate of recycled aggregates caused by the attached old cement paste
and the requirement of water for the hydration reaction of the cement. However, this
situation is different for the geopolymer recycled concrete because water is not involved
in the chemical reaction of the geopolymer synthesis process but only works to facilitate
the workability of the concrete mixture (Davidovits, 2011; Lloyd and Rangan, 2009),
which leads to a lower requirement of w/c ratio for the waste concrete recycled with
geopolymer. Furthermore, it is discovered that the dry mixing of aggregates plays a
positive role in waste concrete recycling by removing the loose particles from the
attached cement paste and helping render a higher compressive strength and elastic
modulus to the RAC (Chan, 1998). Hence, based on the discussion of the developing
mechanism of NITZ in RAC, the following procedure is recommended for the
preparation of the GRAC specimen:
(1) mix the air-dried recycled aggregates, including both the coarse recycled
aggregates and fine recycled aggregates until they are even distributed;
(2) add other solid ingredients for the production of concrete into the dry-mixed
aggregates and keep mixing until all the solid ingredients, such as fly ash, are well
distributed in the mixture;
(3) add the precursor into the prepared mixture and agitate them until a homogenous
mixture is made; and
(4) cast the RAC specimens following the requirement of conventional concrete.
143
6.4 Conclusions
This paper describes an experimental study of the geopolymeric recycled aggregate
concrete which incorporates both the coarse recycled aggregates and the fine recycled
aggregates. Three different w/c ratios were applied in this study to explore the properties
of GRAC. RAC specimens produced with ordinary Portland cement were also studied as
a comparison with the GRAC samples. Compressive strength, Young’s Modulus,
Poisson’s ratio, and density were studied to characterize the physical and mechanical
properties. The mineralogy, microstructure, and interfacial transition zone were
investigated with the aid of X-ray diffraction, scanning electron microscopy, and
nanoindentation techniques. Based on the experimental study, the following conclusions
have been drawn:
(1) The old cement paste from the crushed waste concrete mainly consists of quartz
and calcium carbonate. The absence of calcium hydroxide, which is one of the
common compositions in the cement paste of conventional concrete, could be due to
the carbonation process which is promoted by the combination of the increased
specific area caused by the crushing of waste concrete and the open environment in
the storage site.
(2) The fly ash based geopolymer is capable to render a lower w/c for the production
of RAC than the ordinary Portland cement while even producing a higher compressive
strength.
(3) The compressive strength, Young’s modulus, and the Poisson’s ratio decrease with
the increase of w/c ratio for the GRAC specimens. The reduction rates of the physical
144
and mechanical properties of the GRAC specimens increase with the increase of the
w/c ratio. The Young’s modulus is much more vulnerable to the increase of w/c ratio
than the compressive strength. These significant changes to the GRAC specimens
could be due to the deteriorated properties rendered to the geopolymer by the increase
of w/c ratio.
(4) With the aid of scanning electron microscopy and nanoindentation technologies, it
is found that there is no interfacial transition zone well detected/formed between the
old cement paste and new geopolymer/cement paste. This is attributed to the old
cement paste attached on the aggregates and the application of air-dried aggregates in
concrete production.
6.5 References

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Chen, J.J., Thomas, J.J., Taylor, H.F.W., Jennings, H.M., 2004. Solubility and structure
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Cui, H., Shi, X., Memon, S., Xing, F., Tang, W., 2015. Experimental Study on the
Influence of Water Absorption of Recycled Coarse Aggregates on Properties of the
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thickness and porosity in blended cementitious composite: Effects of curing age,
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Leite, M., 2001. Evaluation of the mechanical properties of concrete made with recycled
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in Concrete Materials. Journal of Materials in Civil Engineering 10, 275-282.
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Scrivener, K., Crumbie, A., Laugesen, P., 2004. The Interfacial Transition Zone (ITZ)
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Shi, X.S., Collins, F.G., Zhao, X.L., Wang, Q.Y., 2012. Mechanical properties and
microstructure analysis of fly ash geopolymeric recycled concrete. Journal of
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Sidorova, A., Vazquez-Ramonich, E., Barra-Bizinotto, M., Roa-Rovira, J.J., Jimenez-

Pique, E., 2014. Study of the recycled aggregates nature’s influence on the
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677-684.
Tam, V.W.Y., Gao, X.F., Tam, C.M., 2005. Microstructural analysis of recycled
aggregate concrete produced from two-stage mixing approach. Cem. Concr. Res. 35,
1195-1203.
Xiao, J., Li, W., Corr, D., Shah, S., 2013a. Simulation Study on the Stress Distribution in
Xiao, J., Li, W., Corr, D.J., Shah, S.P., 2013b. Effects of interfacial transition zones on
the stress–strain behavior of modeled recycled aggregate concrete. Cem. Concr. Res.
52, 82-99.
Xiao, J., Li, W., Poon, C., 2012a. Recent studies on mechanical properties of recycled
Xiao, J., Li, W., Sun, Z., Lange, D.A., Shah, S.P., 2013c. Properties of interfacial
transition zones in recycled aggregate concrete tested by nanoindentation. Cement
and Concrete Composites 37, 276-292.
148
Xiao, J., Li, W., Sun, Z., Shah, S.P., 2012b. Crack propagation in recycled aggregate
concrete under uniaxial compressive loading. ACI Materials Journal 109, 451-462.
Yang, C.C., Su, J.K., 2002. Approximate migration coefficient of interfacial transition
zone and the effect of aggregate content on the migration coefficient of mortar. Cem.
Concr. Res. 32, 1559-1565.
Materials 47, 1468-1478.
Zhou, X.Q., Hao, H., 2008. Mesoscale modelling of concrete tensile failure mechanism at
high strain rates. Computers & Structures 86, 2013-2026.
149
CHAPTER 7 CONCLUSIONS AND FUTURE RESEARCH
7.1 Conclusions
Construction practice consumes a large quantity of materials, including both the
renewable and non-renewable resources. Portland cement, which is one of the most
important materials in construction industry, is highly energy consuming during its
production. Moreover, up to 7% of the global greenhouse gas is produced by the Portland
cement industry. Meanwhile, the maintenance, rehabilitation, and demolition of
infrastructures and residential and commercial buildings, sometimes even the natural
disasters, produce massive waste concrete every year. For the sake of sustainable
development, the research presented in this dissertation was aimed to investigate the
feasibility of applying the fly ash based geopolymer in the loess stabilization and waste
concrete recycling. Through the investigation, the following conclusions could be made:
(1) The loess soil consists of two chlorites as the major clay minerals and muscovite,
quartz, albite, and calcite as the non-clay phases. The majority of silt particles are
covered with clay coating and/or associated with clay particles to form hybrid silt-clay
aggregates. In addition to calcite cementation, clay particles also act as bridging (i.e., clay
cementation) between silt particles and clay aggregates. With the integration of the
composition and microstructure, a four-tier conceptual microstructure model with
increasing length scale and complexity can be used to delineate the particle-level
associations and interactions and to elucidate the origin of the collapsibility of loess.
(2) Two alkaline activators were employed to synthesize the fly ash based geopolymers.
150
The microstructure characterization showed that a compact and stable microstructure was
developed in the stabilized loess by the synthesis of geopolymer. It is unveiled by the
XRD analysis that the there was no new/different mineral introduced to the mixtures,
except the amorphous geopolymer gel. All the test/analysis results indicate that it is the
binding effect of geopolymer gel that renders the improvements in the mechanical
properties of stabilized loess samples. For both two alkaline activators (NaOH and KOH),
increases in the compressive strength and the Young’s modulus, together with a decrease
in the failure strain, have been observed as the fly ash/loess ratio increases. Comparison
between the two different geopolymers shows that the potassium hydroxide activated
geopolymer renders a higher UCS value, higher failure strain, and Young’s modulus than
the sodium hydroxide activated geopolymer if the same fly ash/loess ratio is applied.
(3) A microscale model of recycled aggregate concrete is employed to investigate the
stress distribution factor along both the NITZ and the OITZ under uniaxial compression.
It is observed that the NITZ has a higher value of the maximum of stress concentration
factor than the OITZ for all the three single circular aggregate models applied in this
study. It means that the introduction of NITZ in the RAC plays a detrimental role to the
performance of RAC, and could even possibly contribute more to the mechanical failure
of RAC at the microscale than the OITZ. This implies that how to recycle the waste
concrete while reducing or avoiding the development of NITZ would be of great
significance to the improvement of RAC.
(4) Aiming to prepare a full green concrete, both the coarse recycled aggregates and the
fine recycled aggregates were used to produce the geopolymeric recycled aggregate
concrete. The fly ash based geopolymer is successful to achieve a lower w/c for the
151
production of RAC than the ordinary Portland cement while even producing a higher
compressive strength. The compressive strength, Young’s modulus, and the Poisson’s
ratio decrease with the increase of w/c ratio for the GRAC specimens. The reduction rates
of the physical and mechanical properties of the GRAC specimens increase with the
increase of w/c ratio. The elastic modulus is much more vulnerable to the change of w/c
ratio than the compressive strength. With the aid of scanning electron microscopy and
nanoindentation technique, it is found that there is no interfacial transition zone well-
formed/identified between the old cement paste and new geopolymer/cement paste and
this should be attributed to the application of air-dried recycled aggregates during the
production of concrete.
7.2 Future research
Based on the study presented in this dissertation, the following recommendations could
be made for the future research:
(1) study the performance of GRAC with recycled aggregates crushed from different old
concrete, such as light weight concrete and high performance concrete;
(2) develop an experimental procedure to enhance the mechanical properties of the old
cement paste for waste concrete recycling with geopolymer;
(3) model the mechanical behavior of GRAC at micro/mescoscale with the four-phase
RVE and apply the results for experiment design;
(4) study the properties of the geopolymer stabilized loess and GRAC under the
particular engineering conditions, such as freeze-thaw cycles and other long-term effects;
and
152
(5) investigate the mechanical/engineering properties of GRAC beams and slabs for
structural applications.
153
APPENDIX: LETTER OF PERMISSION FROM THE AMERICAN
SOCIETY OF CIVI ENGINEERS
Zhen Liu <zliu21@tigers.lsu.edu> Mon, Jun 22, 2015

at 10:52 AM
to permissions@asce.org
Dear ASCE Editor,
I am a Ph.D. student at LSU and am working on my dissertation. I am writing to see if I

would have the copyright permission to use one paper published in ASCE Journal of
Materials in Civil Engineering. If possible, a letter from ASCE that provides permissions
would be very helpful, as stated by the dissertation manual of LSU: "All previously
copyright material included in the document must be web viewable and permission to use
the material on the web must be included in the letter of permission."
The published paper is:
Liu, Z., Peng, H., and Cai, C.(2015). "Mesoscale Analysis of Stress Distribution along
ITZs in Recycled Concrete with Variously Shaped Aggregates under Uniaxial
Compression." Journal of Materials in Civil Engineering. Just released.
Thank you very much for your great help.
Sincerely,
Zhen Liu
_________________________________
Dept. of Civil & Environmental Engineering
Louisiana State University
Baton Rouge, LA 70803
154
PERMISSIONS <permissions@asce.org> Mon, Jun 29,
2015 at 8:26 AM
to me <zliu21@tigers.lsu.edu>
Dear Zhen Liu,
Thank you for your permission request. Permission is granted for you to reuse your paper
in your dissertation, under the condition that the paper makes up less than 25% of your
new work. A full credit line must be added to the material being reprinted. For reuse in
non-ASCE publications, add the words "With permission from ASCE" to your source
citation. For Intranet posting, add the following additional notice: "This material may be
downloaded for personal use only. Any other use requires prior permission of the
American Society of Civil Engineers.”
Regards,
Joann
Joann Fogleson
Manager, Product and Subscription Services
American Society of Civil Engineers
1801 Alexander Bell Drive
Reston, VA 20191
PERMISSIONS@asce.org
703-295-6112
E-mail: jfogleson@asce.org
Internet: www.asce.org/pubs | www.ascelibrary.org |

http://ascelibrary.org/page/rightsrequests
155
VITA
Zhen Liu received his Bachelor Degree in Civil Engineering and Master Degree in
Geotechnical Engineering from China University of Geosciences in June 2007 and June
2009, respectively. After that, he attended New Mexico State University and received the
degree Master of Science in Civil Engineering in December 2010.
Zhen Liu has worked as a Graduate Research Assistant at Louisiana State University
since June 2011. He has been involved in several research areas, such as problematic
soils, geopolymer, and recycled aggregate concrete. Several journal articles and
conference papers have been completed based his research. His publications during the
study in Louisiana State University are listed below:
• Liu, Z., Cai, C.S., Liu, F., and Fan, F.. Feasibility study of loess stabilization with
fly ash based geopolymer, ASCE Journal of Materials in Civil Engineering (under
review).
• Liu, Z., Liu, F., Ma, F., Wang, M., Bai, X., Zheng, Y., Yin, H., and Zhang, G..
Collapsibility, composition, and microstructure of a loess in China. Canadian
Geotechnical Journal (under review).
• Liu, Z., Peng, H., and Cai, C.S. (2015). Mesoscale Analysis of Stress Distribution
along ITZs in Recycled Concrete with Various Shaped Aggregates under Uniaxial
Compression, ASCE Journal of Materials in Civil Engineering (Accepted).
• Xin, P., Wu, S., Liu, Z., Shi, J., and Wang, T. (2015). Kinematics and Dynamic
Mechanism of Large-scale Landslides on the North Bank of the Baoji Stream
156
Segment of the Wei River in Loess Plateau, Bulletin of Engineering Geology and the
Environment (under review).
• Yin, H., Zhang, G., Reed, A.H., Furukawa,Y., and Liu, Z. (2013). Influence of
Exopolymer Concentration and Hydrodynamic Forcing on the Size Distribution of
Ca-Montmorillonite Flocs. 35th IAHR World Congress, Chengdu, China.
• Liu, Z., Liu, F., Bai, X., and Zhang, G. (2012). Particle Characterization of
Collapsible Loess in Xi’an, China. The 4th International Conference on Problematic
Soils, Wuhan, China.
157

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APPLICATIONS OF GEOPOLYMER IN CIVIL ENGINEERING：

FEASIBILITY STUDY OF LOESS STABILIZATION AND WASTE

Submitted to the Graduate Faculty of the

The Department of Civil and Environmental Engineering

expertise, dedication and patience benefited me considerably during my Ph.D. study in

investigation of the origin of collapsibility for the loess samples.

comments and suggestions on my research. Technical supports of Dr. V.P. Singh,

CAMD-LSU, Dr. Dongmei Cao, Material Characterization Cementer, Ms. Wanda

have encouraged me and provided me strength to pursue my dreams.

ACKNOWLEDGEMENTS ............................................................................................... iii

LIST OF TABLES ............................................................................................................ vii

LIST OF FIGURES ......................................................................................................... viii

ABSTRACT…. ................................................................................................................. xii

CHAPTER 2 LITERATURE REVIEW........................................................................ 11

CHAPTER 3 ORIGIN OF THE COLLAPSIBILITY OF LOESS ............................... 40

CHAPTER 4 STABILIZATION OF LOESS WITH FLY ASH BASED

CHAPTER 5 NUMERICAL ANALYSIS OF THE STRESS DISTRIBUTION

CHAPTER 6 INVESTIGATION OF THE PROPERTIES OF THE GEOPOLYMERIC

CHAPTER 7 CONCLUSIONS AND FUTURE RESEARCH ................................... 150

APPENDIX: LETTER OF PERMISSION FROM THE AMERICAN SOCIETY OF

VITA…………. .............................................................................................................. 156

Table 2-1 Classification of recycling of by-product ......................................................... 23

Table 4-2 Composition of fly ash (wt.%).......................................................................... 83

Table 5-2 Material properties in the extended model ..................................................... 107

Table 5-3 Maximum of SCF in OITZ and NITZ ............................................................ 110

Table 6-2 Composition of fly ash (wt.%)........................................................................ 120

Figure 2-1 Distribution of loess deposits in Alaska .......................................................... 14

Figure 2-4 Loess distribution in Europe ........................................................................... 17

Figure 2-5 Loess distribution in Central China................................................................. 18

Figure 2-6 Distribution of loess in China ......................................................................... 19

Figure 2-8 Relationship between compressive strength and addition of recycled

Figure 3-4 Results of the double oedometer tests ............................................................. 52

Figure 3-7 SEM micrographs showing the microstructure of the loess............................ 60

Figure 3-13 A conceptual microstructural model of a four-tired hierarchy...................... 70

Figure 4-4 Failure strain of geopolymer stabilized loess .................................................. 89

Figure 4-5 The Young’s modulus of geopolymer stabilized loess ................................... 90

Figure 4-10 A conceptual microstructure model of geopolymer stabilized loess ............ 96

Figure 5-1 Representative volume element of RAC ....................................................... 102

Figure 6-2 Particle size distribution of recycled aggregates ........................................... 118

Figure 6-5 Flow chart of the sample preparation ............................................................ 122

Figure 6-7 Failure patterns under compression .............................................................. 128

Figure 6-8 SEM images of the recycled aggregate ......................................................... 129

Figure 6-20 Illustration of the “wall effect” in concrete ................................................. 138

Geopolymer, which is an inorganic material formed by alkaline activation of aluminia-

and silica-containing material through a polycondensation process, could be synthesized

geopolymer a prospective future in civil engineering applications. This dissertation was

geopolymer in the loess stabilization and waste concrete recycling.

With the integration of composition and microstructure, a four-tier conceptual

microstructure model is proposed to elucidate the origin of loess collapsibility. Based on

stabilization with geopolymer is then conducted. Results indicate that improved

rendered by the binding effect of geopolymer gel.

concrete recycling with geopolymer.

during the 21st century (Pacheco-Torgal and Labrincha, 2013).

al., 2015; Zhang et al., 2013).

treatment/improvement of the problematic soil is another key issue in the engineering

buildings. However, the production of conventional soil stabilizers (such as Portland

to the civil engineers for the sustainable development.

1.1.1 Loess soil

Loess is an aeolian, non-stratified deposit that is composed of primarily silt-sized mineral

susceptible to landslides, hydroconsolidation, and seismic settlement (Yuan and Wang,

wetting-induced landslides, hydroconsolidation, and seismic settlement, loess is classified

stabilize the collapsible loess.

study of new/green materials for loess stabilization is still under exploration.

substantial amount of SiO2 , and Al O .