GEOPOLYMER AS MATRIX APPLIED IN COMPOSITES WITH

NATURAL FIBERS
E. A. S. Correia1, M. E. O. Alexandre2
1
2

Universidade Federal da Paraba - UFPB, Joo Pessoa/PB Brazil

Instituto Federal de Educao, Cincia e Tecnologia da Paraba-IFPE, Joo Pessoa, Brasil

ABSTRACT
The development of new technologies has boosted searches for obtaining competitive and
ecologically viable materials cost benefit attractive to the market. The main goal of this work
was to develop and study geopolimrica matrix composites reinforced with fibres of vegetable,
for application as alternative non-conventional material in several areas. Noted the technical
feasibility of such materials through the results achieved when subjected to mechanical and
physic-chemical associated with the modern techniques of microestruturais characterizations.
The bursting and compression module, array and composite material, was compatible with the
minimum established resistance and validated in the market when compared to the similar hues
screeds. When subjected to pressure, low energy composites showed outstanding degree of
packaging, lower porosity, resistivity and better ductility and excellent stage of deformation.
Keywords: Geopolymer1, Natural Fibers2, Composites 3.
1. INTRODUCTION
Advances in the development of composite materials have brought significant results as to
its applicability (MATTOSO,1996). However it is notable that some reinforcements traditional
expose their limitations and compromises its mechanical performance. This is because with time,
these materials lose their tenacity and endurance due to the alkalinity of the array. The relentless
quest for the most versatile building materials, with greater economic potential and low cost,
have targeted searches to work with natural fibres (AZIZ, 1987), which in addition to improving
the mechanical performance of the array, has good resistance to chemical instability establishing
a greater resistance to the matrix, however still exists the need to find satisfactory conditions for
optimizing the interface, as well as enhance operationalization in productive scale.
The technique of applying natural fibres such as strengthening agent in arrays slabs have
been used since the mid-1940s when James Hardie and Copy Pty Ltd has replaced asbestos by
pulp cellulose as strengthening agent in cement-based laminates. In Brazil, this technique began
to be developed by the research and Development Center in Bahia, applying natural fibers in
concrete matrix (SIVARAJA, 2009). This new line of research brings to light a new variable for
composite materials, opening up new fields of application, in addition to using renewable
resources, which contribute to the reduction of contamination of the environment.

Compound as aluminosilicates form a matrix resistant high temperature (BARBOSA,2003;

COLEMAN,2005), have high power to accession and satisfactory ability to cure at room
temperature, the Geopolymer (DAVIDOVITS,2002; DUXTON,2006) like most arrays screeds,
has a low mechanical strength, which limits its scope. To obtain a significant gain in strength,
especially when subjected to mechanical tests, inserting vegetable fiber composite qualities
raises and extends its scope.
2. MATERIALS AND METHODS
2.1. Materials
As a source of silicon and aluminum matrix used the supplied by Caulisa SA kaolin, kaolin
processing industry located in the municipality of Juazeirinho, PB; the vegetable fibres were
provided by COSIBRA Company Sisal of Brazil. Sodium silicate was provided by
Pernambuco Chemistry S/A with a silica (SiO2/Na2O ratio, by mass) roughly 2.5 and pH around
13.
2.2. Synthesis process
The process of synthesis occurred in two steps. In the first stage was calcined
kaolin(DUXTON2006), in a muffle furnace at 750 C for 2 h, so that the entire exercised by
kaolinite in metacaulinita(PALOMO,2003; VAN JAARSVELD,2002), then use the sodium
silicate in appropriate proportion with Activator alkaline, the bubbles have been eliminated
through intermittent vibration. In the second step the fibers with approximately 60 mm in length
were arranged in two layers of 3 mm and interspersed by matrix in the ratio of 3%, until filling
mold, this process was repeated until all layers were released by filling in a uniform manner
throughout the mold cavity.
Again, the bubbles have been eliminated by placing the template fully populated on a
shaking platform. After the molding process, shapes underwent a process of cure in an oven at 55
C for 48 hours. After this period, the mold rested for over 48 hours under ambient temperature,
so that ultimately were subjected to the tests of characterization.

(a)

(b)
Figure 1: Three-point bending test during and after the break

(a)

(b)
Figure 2: Tests simple and diametric compression

2.3. Characterization of materials

The characterization of materials, precursors and of the bodies evidence instrumental
techniques was carried out as described below:-the determination of the moisture content of the
fibres(LADCHUMANANANDASIVAM,2005; GHAVAMI,1999) of the Agave Sisalana was
conducted according to standard (American Society for Testing and Materials) ASTM 1413-76;
the analyses via wet (titration) were held in order to determine the concentration of acidic groups
of samples; The content of water-soluble extractives was determined by standard TAPPI T212
om-98. -Images of the surfaces of vegetable fibres were obtained from secondary electrons and
Spread in a scanning electron microscope JSM 5800 LV a JEOL brand.
The accelerating voltage of the electron beam generated from a tungsten filament was equal
to 10 kV.
Compression test, conducted in the laboratory of Rural Constructions Seals/UFCG, was
used the Universal type compression machine. Test compression was accomplished using the
cylindrical body of evidence with the following dimensions: 5 cm in diameter and 10 cm in
height, as in Figure 2. The test of resistance to traction in bending Universal Machine was used
for the testing of 03 points, as shown in Figure 1, with the following schedule: 03 batches with 5
bodies of evidence each with dimensions 4cmx4cmx16cm, at the age of 30 days, both tests with
speed 2 mm s-1.Chemical analysis was held at the Rapid laboratory Scale of UFPB in Sequential
x-ray Fluorescence Spectrometer XRF-1800 model of Shimadzu.
3. RESULTS AND DISCUSSION
3.1. Geopolymer Formulations of folder
The
chemical
composition(PALOMO,2003)
of
metacaulinita
activated
alkaline(FERNNDEZ-JIMNEZ,2005; GLUKHOVSKY, 1980; and GOMES,2007) with
sodium silicate PQ-1.65, was analyzed by x-ray Florescence (XRF) in laboratory scale rapid
UFPB.

Table1: Chemical compositions of the Geopolymer folder.

constituents SiO2
%

72.7895

Na2O
12.9737

Al2O
12.8665

K2O
0.4329

Cl
0.3769

Fe2O3
0.3008

CaO
0.1291

TiO2
0.0537

SO3
0.0409

P2O5
0.0295

NiO
0.0064

3.2. Physico-chemical properties of fibres

As the Lignocellulosic are highly hygroscopic materials is very important to the
determination of the moisture content of The soluble in cold water include organic salts, sugars,
resins and tannins.
Table 2: Physico-chemical properties of vegetable fibres

Parameters
Moisture content (%)
Acidic groups (mol/l)
Water-soluble extractives (%)
pH
Density (g/m3)
Lignin (%)
Cellulose(%)
Hemicellulose(%)
Diameter (m)
Hygroscopicity (%)
L/D
Angle expiral()
Length (cm)

Agave Sisalana
10,48
0, 00186
6,84
7,69
1,32-1,45
6-11
65-73
13,33
50-300
10-13
103
20
30-140

Anans Comosos
10,11
0,00146
7,19
6,96
1,30-1,44
5-12
70-83
18
50-105
9-11
460
15
20-120

Uma das limitaes das fibras vegetais no obteno de compsitos a elevada

higroscopicidade e o alto teor de extrativos solveis presentes na superfcie,o que dificulta a
interao fsica da matriz com o agente de reforo, a baixa densidade da fibra de anans em
relao a fibra de agave, proporciona elevada razo de aspecto (L/D), favorvel a ancoragem da
fibra de anans na matriz geopolimrica, outro aspecto positivo o elevado teor de lignina nesta
fibra, que age como agente plastificante, otimizando a estabilidade da interface.

3.3. Mechanical strength properties

3.3.1. Three point bending tests
Been tested 45 bodies of evidence, 15 in 3 batches of five and 30 in 6 batches of five
following batches for array, matrix, with agave sisalana and matrix with pineapple comosos at a
ratio of 3% by volume for randomly distributed reinforcing agent with approximately 25 mm in
length. Bending tests were conducted at three points on a machine SHIMADZU AG-X , with
load cell of 50 kN, where the body of evidence was positioned with the load applied at the center

of even with going to encyclopedia of 120 mm and with a speed of 2 mm/min, defined by NBR
13279 (2005) and temperature about 25 C. Figure 1 (a) shows the outline of the test. The results
obtained are represented in the form of graph (Stress x Strain), figures 3 and 4.

Stress (MPa)

Mdia

Strain (%)
Figure 3: Array behavior in three-point bending tests.

Mdia
Tenso (MPa)

Stress (MPa)

Mdia

(a) Strain (% )

(b) Strain (%)

Figure 4: Behavior of composites with agave sisalana (a) and with pineapple comosos (b) for the three points
bending tests.

Compression tests were conducted on a machine SHIMADZU AG-X 100, with load cell of
100 kN, where the bodies of evidence were positioned as Figure 2 (a) (b) and with a speed of 2
mm/min, defined by NBR 7215 (1991), and temperature about 25 c. The results obtained are
represented in chart form (Stress x Strain), figures 5, 6,7 and 8.
3.3.2. Axial compresso tests

Stress (MPa)

Mdia

Strain(%)
Figure 5: Average curve for simple compression test with the array.

Mdia

Stress (MPa)

Stress (MPa)

Mdia

(a) Strain(%)

(b)Strain(%)

Figure 6: Average curves for simple compression tests with composites of agave sisalana pineapple (a) and
anans comosos (b)

3.3.3 Diametral compression test

Stress (MPa)

Mdia

Strain(%)
Figure 7: Average curve to diametral compression test with the array.

Mdia

TStress (MPa)

TStress (MPa)

Mdia

(a) Strain (%)

(b) Strain (%)

Figure 8: Average curves for compression tests with diametral composites agave sisalana pineapple (a) and
anans comosos (b)

Analisando o comportamento da Figura 3, verifica-se que o valor mdio obtido para tenso
de flexo foi 1,4Mpa para matriz, valor razovel para os padres encontrados na literatura para
materiais cermicos, na figura 4, podemos perceber valores entre 2 e 3 Mpa para matrizes
reforadas com fibras vegetais, os valores alcanados para mdulos de ruptura tambm so
expressivos e ocorrem com uma taxa de deformao superior aos da matriz sem agente de
reforo.
3.4. Micro-structural studies

Figure 5: Microstructure of the surface of the

fibres of sisal in natura.

Figure 6: Microscopy in composite with

leaf of sisal fiber in Geopolymer.

Figure 7: Microstructure of the surface of the

fibres of anans in natura.

Figure 8: Microscopy in composite with

leaf of anans fiber in Geopolymer

As alteraes morfolgicas observadas nas fibras vegetais inseridas na matriz foram

observadas atravs de MEV, nesse trabalho utilizamos fibra in natura pois a matriz j possui
elevada alcalinidade (pH=13), logo evitamos a fragilizao do agente de reforo por tratamento
qumico excessivo; na figura 6, observamos espaos vazios na interface fibra-matriz, todavia
estes espaos esto minimizados na figura 8, onde foi utilizados fibra de anans como reforo,
isto ocorre em funo do baixo teor de extrativos solveis presentes nessa fibra do abacaxizeiro
que menor em torno de 11% aproximadamente.

3.5. Termogravimtricas Analyses

0,3

TGA - FLS
TGA - FLSM

12

DTG-FLS
DTG-FLSM
0,2

Weight (% mg)

10
0,1

0,0

4
-0,1

Deriv.Weight(% mg/min)

14

0
0

100

200

300

400

500

600

700

800

-0,2
900

A figura 9, mostra as
curvas de TG/DTG para
fibras de sisal in natura e
tratadas com NaOH(2%)
durante 48h e expostas ao
ar por 15dias, podemos
perceber dois estgios de
decomposio de 10-12%
de gua, 50-65% de
polissacardeos
e
aproximadamente 30% de
resduos.
Observamos
atravs dos resultados que a
amostra sem tratamento
apresentou maior taxa de
decomposio no entorno
de 300-400C.

Temperature (C)

Figure 9: TG and DTG curves for fibers of agave sisalana in natura and mercerizadas

FLS
FLSM

60
50

Weight (% mg)

40
30
20
10
0
-10
-20
0

100

200

300

400

500

600

700

800

900

Temperature (C)

Figure 10: DTA curves for agave sisalana in natura and mercerizadas

Constatamos atravs da
curva DTA (figura 10) para
fibra de sisal, um evento
endotrmico entre 65-75C e
outro no intervalo de 400420C,
dois
picos
exotrmicos na temperatura
mxima de 360C e 460C,
na regio de transio, a
degradao
trmica
acentuada ocorreu entre 300400C e coincide com a
anlise TG/DTG.

14

DTG - FLA
DTG - FLAM

TGA - FLA
TGA - FLAM

12

0,00

-0,05

6
-0,10
4

Deriv.Weight(%/min)

0,05

10

-0,15
2
0

100

200

300

400

500

600

Temperature (C)

700

800

-0,20
900

Figure 11: TG and DTG curves for fibers of anans comosos in natura and mercerizadas.

20

Temperature difference (C/mg)

Weight (%)

0,10

A figura 11 mostra as
curvas de TG/DTG para fibra de
anans comosos, nas mesmas
condies
relatadas
anteriormente, onde podemos
observar dois estgios de
decomposio, o primeiro a
60C, referente perda de gua
e o segundo a365C, referente a
decomposio principal. Foi
notado um resduo de 1, 5 a 2,
5% a 800C. A curva DTG
apresentou dois estgios de
decomposio, o primeiro a
60C, correspondente ao calor
de vaporizao e o segundo a
355C, onde a decomposio foi
mxima

DTA - FLA
DTA - FLAM

A anlise de curva DTA,

apresentou pequenos eventos
trmicos positivos e escassos
pontos calorficos significativos
conforme a figura 12, a fibra in
natura apresentou resultados
exotrmicos
discretos
e
negativos, todavia para fibras
mercerizadas observamos um
pico mximo em torno de 415C.

-20

-40

300

600

900

Temperature (C)

Figure 12: DTA curves for anans comosos in natura and mercerizadas

4. CONCLUSIONS
A presena de fibras vegetais na matriz confere tendncia de crescimento na resistncia
flexo, at um teor timo, com posterior reduo desta propriedade, a capacidade de absorver
energia (tenacidade) foi a propriedade mais sensvel influenciada pelo acrscimo das fibras. Os
compsitos com fibras de anans comosos apresentaram valores elevados para energia especfica
(tenacidade) e resistncia flexo em relao aos corpos de prova com fibras de agave sisalana,
para todos os esforos utilizados. Isto se deve, provavelmente, ao maior nmero de fibras por
unidade volumtrica da matriz, pois as fibras de anans comosos apresentam maior relao de
aspecto (L/D) devido ao menor dimetro, e a maior concentrao de fibras na regio de interface,
o maior teor de lignina destas fibras tambm proporciona maior rigidez e elasticidade.
A curvas termoanaliticas mostraram que as fibras apresentam estabilidade em torno de
300C, podendo ser aplicadas em materiais refratrios, isolantes trmicos e acsticos. As fibras
da folha do abacaxizeiro tm grande potencial na aplicao na engenharia mecnica em materiais
compsitos para a fabricao de carcaa de automveis, pra-choques, painis de carros, em
barcos, caixas de gua, cabine telefnica, caixas de correio, depsito de lixo, etc., ainda
despertam particular interesse da construo civil para compsitos de matriz geopolimrica
desenvolvidos para design de interiores ecologicamente corretos.

5. ACKNOWLEDGMENTS
We acknowledge all the partners and friends who collaborated to the development that job,
providing us every necessary material to confection our specimens between them, the COSIBRA
S.A., Caulisa S.A. and Chemistry S.A. Acknowledge too, all the laboratories who collaborated to
analyzes and characterizations our specimens made in the LABEME and LSR in the Federal
University of Paraba. The characterization was made in the LACOM on UFPB, and a
mechanical test was executed in mechanical laboratory of the IFPB and Rural Constructions
laboratory LaCRA/UFCG.
.
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