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Composites Science and Technology 65 (2005) 18401850
www.elsevier.com/locate/compscitech
b,*
School of Materials Science and Engineering, Nanyang Technological University, Nanyang Avenue, Singapore 639798, Singapore
b
Department of Mechanical Engineering, University of Akron, Akron, OH 44325-3903, USA
Received 14 March 2005; accepted 23 March 2005
Available online 28 April 2005
Abstract
Studies were performed on the specic strength, moduli and fracture toughness of varied microstructures of syntactic foam. The
dierent microstructures were created by using three dierent types of microspheres, namely 3M Scotchlite K15 and K46 glass bubbles, and Phenoset BJO-093 hollow phenolic microspheres, and by changing the volume fractions of microspheres from 0 to
50 vol%. Tension, compression, exural and fracture tests were performed. Results showed that the tensile and exural strengths
decreased with increasing ller content. The behavior of the tensile and exural strength was not aected by the component microspheres. Interestingly, the tensile and exural moduli showed dierent trends for each type of microspheres with increasing ller
content. Results of the compression tests revealed superior behavior of the high density microspheres. The specic fracture toughness data yielded maximum values at 30 vol% for each type of microspheres investigated. Scanning electron microscope studies were
performed to determine the failure mode for each loading condition.
2005 Elsevier Ltd. All rights reserved.
TM
1. Introduction
Syntactic foam is a ternary material system made in
a mechanical way by mixing hollow particles (the ller)
with a resin system (the binder). The hollow particles
may be made of polymer, ceramic, carbon, or metal.
Most often thermoset resins are used as the binder.
Dispersion of the hollow particles creates a porous
material with closed cells. By changing the amount of
hollow ller particles, dierent densities and thus
microstructures of syntactic foam can be created. Syntactic foams are known to possess low density, high
stiness, excellent compressive and hydrostatic
strength, and good impact behavior [16]. Unlike most
*
Most studies on the mechanical and fracture properties of syntactic foams are based on the maximum ller
content of microspheres as this elicits the lowest possible
weight of the composites [13]. This study investigates
the inuence of dierent compositions of syntactic foam
on its specic mechanical and fracture properties. A
comprehensive understanding of the structureproperty
relationship is lacking. Dierent compositions will be
created by varying the type and volume fraction of
microspheres. This route is dierent from that reported
by Gupta et al. [4] whereby dierent microstructures
were created by using dierent types of microspheres
with similar size distributions. However, only the volume fraction of microspheres was kept constant for each
type of microspheres. Bunn and Mottram [5] also reported on the eect of the volume fraction on phenolic
microspheres on the compressive properties. The present
paper compares the results derived from phenolic microspheres to those made of glass shells. It is expected the
interfacial adhesion between phenolic microspheres
and polymers could be stronger.
It is essential that specic properties be discussed in
this paper because the density of syntactic foam changes
with the amount of microspheres introduced. Specic
properties allow for the comparison of the performance
of syntactic foams to other potential foam materials in
sandwich composites such as PU, PVC and aluminum
foams. Furthermore, specic properties aid the comparison between the dierent microspheres used in this
study. By normalizing mechanical and fracture properties against the density, it is believed the results would
be fruitful for guiding future design for syntactic foams
based on specic properties. Results from tension, compression, exure and fracture tests will be discussed in
relation to their microstructures.
2. Experimental work
2.1. Materials and equipment
The syntactic foams for this research were produced
by mechanical dispersion of hollow microspheres in
epoxy resin. Three dierent types of hollow microspheres, namely 3M Scotchlite Glass Bubbles K15
and K46 and Phenoset BJO-093 phenolic microspheres
TM
1841
Table 1
Physical properties of the studied microspheres
Type of microsphere
Thickness-to-radius ratio
BJO-093
K15
K46
0.25
0.15
0.46
3.44
2.07
41.37
71.5
70a
43.6
1.84b
0.70
1.37
0.052
0.02
0.063
a
b
From [17].
From SEM measurement.
1842
1.25
Theoretical density
Density (g/cm3)
Measured density
1.00
0.75
0.50
0
10
20
30
40
50
vol% microspheres
Fig. 2. Density variation with microsphere content for syntactic foam
containing (j) K15, (m) K46 and (d) phenolic microspheres.
Three types of mechanical tests, namely tension, atwise compression and exure were performed with different microstructures of syntactic foam. For the
tensile tests, the syntactic foam was machined into a
standard dog-bone bar by means of a TensilKut machine. The specimens were loaded at an ambient temperature using an Instron Model 5567 at a cross-head speed
of 5 mm/min. For each test the tensile strain was recorded with a clip-on strain gauge. The Youngs modulus, Et, was measured from the initial region of
deformation. The results are based on an average of ve
tests. The error bar is the standard deviation for ve
measured values.
Andrews et al. [9] report about the eect of the
specimen size on the mechanical properties. According
to Andrews et al., for closed-cell aluminum foam having a cell diameter of 23 mm, the length of a tensile
specimen should be at least six times the cell diameter
to avoid the specimen dimensions from aecting the
mechanical properties. Because of the small cell size
of syntactic foams, see Fig. 1, all specimens comply
with the requirements set by Andrews et al. and the
specimen sizes used do not aect the mechanical
properties.
For the atwise compression test, syntactic foam was
machined to blocks of 25 25 12 mm3. The length and
width were chosen according to ASTM C365-00 [10].
Due to the short of supply for K46 microspheres, compression tests for K46 specimens were conducted from 0
to 30 vol% microspheres only. In our future work, the
syntactic foam would be used as the core material in
sandwich composites. The height of the specimen was
chosen based on earlier studies [1]. Low aspect ratio
specimens were used to minimize the eect of the shear
stress. The tests were carried out at room temperature
using an Instron Model 4206 with a maximum capacity
of 100 kN. The cross-head speed was 0.5 mm/min. The
atwise compressive yield strength of syntactic foam
was calculated by [10]:
rc
P
;
A
mt
;
A
1843
Table 2
Mechanical properties and void content of the studied compositions of syntactic foam
Tensile
strength
(MPa)
Youngs
modulus
(GPa)
Compression yield
strength
(MPa)
Compression
modulus
(GPa)
Flexure
strength
(MPa)
Flexure
modulus
(GPa)
Fracture
toughness
p
(MPa m)
Epoxy
10% K15
20% K15
30% K15
40% K15
50% K15
29.81
37.32
32.95
23.68
18.96
17.45
2.68
2.76
2.55
2.23
2.07
1.99
85.54
52.95
54.18
44.73
37.96
31.17
1.04
0.88
0.68
0.66
0.63
0.63
78.61
56.61
43.63
27.67
25.59
22.51
2.82
2.31
2.07
1.81
2.06
1.99
0.83
0.95
1.20
1.16
0.94
0.71
2.91
5.14
6.86
9.18
8.85
7.02
10%
20%
30%
40%
50%
K46
K46
K46
K46
K46
43.29
32.87
26.21
23.25
23.23
2.82
3.12
3.29
3.41
3.78
84.61
80.64
76.63
NA
NA
0.95
1.14
1.14
NA
NA
53.32
36.04
31.38
33.39
33.99
2.97
3.13
3.22
3.58
3.86
1.17
1.39
1.27
0.95
NA
4.87
6.07
8.44
10.21
10.02
10%
20%
30%
40%
50%
BJO
BJO
BJO
BJO
BJO
40.84
32.16
25.75
22.29
15.50
2.39
1.88
1.58
1.33
1.17
62.87
51.08
38.11
31.39
25.95
0.80
0.71
0.63
0.57
0.53
60.47
46.70
38.91
31.52
27.22
2.14
1.90
1.52
1.25
1.09
0.87
0.99
1.15
0.92
0.66
3.95
3.69
8.76
8.61
8.03
R S2
;
6d
S3m
;
4Wt3
t > 2:5
K Ic
ry
Void
(%)
2
;
1844
experiences catastrophic failure across a plane perpendicular to the tensile axis. Table 2 presents mechanical
properties and void content of the dierent compositions studied. The trends in the tensile strength, rt, with
increasing microsphere content are rather similar for the
three types of microspheres, except for 50 vol% phenolic
microspheres. Luxmoore and Owen [14] concluded that
a crack will initiate from an oversized void when a composite is subjected to tensile loading. Indeed, numerous
specimens fractured at a cross-section containing a void.
The specic tensile strength, rt/q, for various compositions of syntactic foam are shown in Fig. 3(a). Fig. 3(a)
shows that rt/q increases upon inclusion of a small
amount of microspheres when compared to neat epoxy
resin. The presented data for neat epoxy are obtained
experimentally. However, beyond 10 vol%, a decreasing
trend in rt/q is observed for all types of microspheres.
The decreasing trend in rt/q with increasing ller content indicates that the relative reduction in strength is
larger than the relative reduction in density. Indeed, a
decrease in rt with increasing ller content is observed,
see Table 2. The comparable trends and values suggest
that rt/q is independent of the microsphere type and
size, but only varies with the microsphere volume fraction. The following curve-tting relation between the
rt/q and the volume fraction of microspheres, x, has
been derived for 0.1 < x < 0.5:
rt =q 2157x4 2712x3 1050x2 93x 40:768:
50
40
30
20
10
0
0
(a)
-1
9
Nevertheless, clear advantages regarding other
mechanical properties arise upon introduction of hollow
microsphere as shown in the discussion that follows.
Luxmoore and Owen suggested [14] that the failure of
the foam is attributed to the failure of the resin matrix.
The non-linearity in rt/q is caused by the reduction
in the area of the epoxy matrix in a cross-sectional area.
10
20
30
vol % microspheres
40
50
0
0
(b)
10
20
30
40
50
vol % microspheres
Fig. 3. Specic tensile properties of syntactic foam containing (j) K15, (m) K46 and (d) phenolic microspheres: (a) specic tensile strength; (b)
specic Youngs modulus.
1845
160
140
120
100
III
80
60
II
40
20
0
-20
-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
1846
(a)
1.50
-1
100
-1
80
60
40
20
0
0
10
20
30
40
vol% microspheres
50
60
(b)
1.25
1.00
0.75
0.50
0.25
0.00
0
10
20
30
40
50
60
vol% microspheres
Fig. 6. Specic compressive properties of syntactic foam containing (j) K15, (m) K46 and (d) phenolic microspheres: (a) specic compressive yield
strength; (b) specic compressive modulus. Due to the short of supply for K46 microspheres, compression tests for K46 specimens were conducted
from 0 to 30 vol% microspheres only.
80
80
60
60
Stress (MPa)
Stress (MPa)
40
20
1847
40
20
Increasing volume fraction
0
0.00
(a)
0.01
0.02
0.03
0.04
0.05
0.06
Strain (mm/mm)
0.00
(b)
0.01
0.02
0.03
0.04
0.05
0.06
Strain (mm/mm)
Fig. 7. Flexure stress strain curves of syntactic foam containing various amounts of (a) K46 and (b) phenolic microspheres. The arrow indicates the
direction of increasing ller content.
1848
70
60
50
40
30
20
10
0
(a)
-1
80
10
20
30
40
50
vol % microspheres
10
20
30
40
50
vol % microspheres
(b)
Fig. 9. Specic exural properties of syntactic foam containing (j) K15, (m) K46 and (d) phenolic microspheres: (a) specic exure strength;
(b) specic exure modulus.
Fig. 10. SEM micrograph of the fracture surface of syntactic foam containing 10 vol% K15 microspheres under (a) tension, and (b) compression.
The black arrows denote the direction of crack propagation.
0.5
-1
1.0
0.5
0.0
0
10
20
30
40
50
vol % microspheres
Fig. 11. Specic fracture toughness vs. ller content for syntactic foam
containing (j) K15, (m) K46 and (d) phenolic microspheres. Due to
the short of supply for K46 microspheres, fracture toughnesses for K46
specimens were assessed from 0 to 40 vol% microspheres only.
1849
Fig. 12. SEM micrographs of the fractured surface of SENB specimens of syntactic foam containing 10 vol% microspheres: (a) K15 microspheres;
(b) hollow phenolic microspheres.
We believe that the type of major toughening mechanism has changed at the transition point of 30 vol% of
microsphere content. The toughening from 0 to
30 vol% microspheres is inuenced by a combination
of the ller stiening eect and crack bowing mechanisms in the presence of round-shaped llers. The
change in toughening mechanism is conjectured to be
caused by the inter-particle spacing theory as discussed
by Lee and Yee [13] for glass bead/epoxy composites.
Increase in microsphere content will decrease interparticle separation between microspheres. The increase
of microsphere content beyond the complete wetting
ability of epoxy also introduces inter-sphere sliding
and stress concentration. Higher volume fractions of
microspheres allow more microspheres to debond from
the matrix. Debonding is accompanied by premature
cracks. If the direction of these cracks is parallel to the
crack growth direction, the subcritical cracks act as precursors and facilitate crack propagation.
SEM was used to elucidate the toughening mechanisms in the various microstructures of syntactic foam,
see Figs. 12 and 13. Fig. 12 shows the fracture surface
of syntactic foams containing low volume fractions of
Fig. 13. SEM micrograph of the fractured surface of SENB specimens of syntactic foam containing large amounts of microspheres: (a) 40 vol% K46
microspheres; (b) 50 vol% hollow phenolic microspheres.
1850
with K46 microspheres outperforming K15 microspheres, it is surmised that the thickness-to-radius ratio
and the wall material of the microsphere aect the size
of the step structure and thus K1c/q.
Figs. 13(a) and (b) show the microstructures of syntactic foam containing 40 vol% K46 and 50 vol% hollow
phenolic microspheres, respectively. Compared to Fig.
12, step structures are absent in Fig. 13. Instead, the
dominant fracture mechanism that is observed is debonding of microspheres. The existence of excessive debonding introduces stress concentration and premature
cracks leading to reduced fracture toughness.
4. Conclusions
From the results presented in this paper, it can be
concluded that the specic properties of syntactic foam
depend on the types and volume fractions of microspheres utilized in the syntactic foam. Increase in microsphere density (K46 vs. K15) and the thickness-to-radius
ratio led to an increase in specic tensile stiness. The results for the tensile and exural tests were comparable
due to the fact that both types of tests exhibited the
same failure mode. Both tests elicited a decreasing trend
in specic strength with increasing ller content. A distinct trend in compressive behavior was noted in contrast to the tensile failure. The compression tests
revealed the excellent compressive properties of syntactic foam and in particular the superior performance of
K46 microspheres, giving rise to higher compressive
yield strengths and moduli compared to K15 and phenolic microspheres.
From the fracture toughness tests, it was concluded
that all types of studied microspheres show a similar
trend in the specic fracture toughness with increasing
ller content. For lower ller content an increase in
the specic fracture toughness was observed. The increase reached a maximum after which a decrease in
the specic fracture toughness was seen. The change in
behavior was attributed to a change in the dominant
toughening mechanisms from ller stiening, crack
front bowing to excessive debonding of microspheres
in reduced matrix volume. This work, however, demonstrated the usefulness of a combination of desired properties for syntactic foam such as light-weight high
stiness, high compression and high toughness.
Acknowledgments
The authors thank Nanyang Technological University and DSO National Laboratories Singapore for the
support of this work. One of us (SCW) acknowledges
the support of NSF Grant# CMS 0335390 administered
by the Mechanics and Materials Program.
References
[1] Gupta N, Kishore, Woldesenbet E, Sankaran S. Studies on
compressive failure features in syntactic foam material. J Mater
Sci 2001;36(18):448591.
[2] Gupta N, Woldesenbet E, Kishore. Compressive fracture features
of syntactic foams microscopic examination. J Mater Sci
2002;37(15):3199209.
[3] Kim HS, Oh HH. Manufacturing and impact behavior of
syntactic foam. J Appl Polym Sci 2000;76(8):13248.
[4] Gupta N, Woldesenbet E, Mensah P. Compression properties of
syntactic foams: eect of cenosphere radius ratio and specimen
aspect ratio. Compos Part A 2004;35A(1):10311.
[5] Bunn P, Mottram JT. Manufacture and compression properties
of syntactic foams. Composites 1993;24(7):56571.
[6] Shutov FA. Syntactic polymer foams. In: Klempner D, Frisch
KC, editors. Handbook of polymeric foams and foam technology. Hanser Publishers; 1991. p. 35574.
[7] Rothon RN. Particulate-lled polymer composites. New
York: Longman, Scientic and Technical; 1995.
[8] Anon. Standard test methods for void content of reinforced
plastics. ASTM D 2734-94. New York: ASTM; 1994.
[9] Andrews EW, Gioux G, Onck P, Gibson LJ. Size eects in ductile
cellular solids. Part 2: Experimental results. Int J Mech Sci
2001;43:70113.
[10] Anon. Standard test method for atwise compressive properties
of sandwich cores. ASTM C 365-00. New York: ASTM; 2000.
[11] Anon. Standard test method for exural properties of unreinforced and reinforced plastics and electrical insulating materials.
ASTM D 790-00. New York: ASTM; 2000.
[12] Hertzberg RW. Deformation and fracture mechanics of engineering materials. New York: Wiley; 1996.
[13] Lee J, Yee AF. Fracture of glass bead/epoxy composites: on
micro-mechanical deformations. Polymer 2000;41(23):836373.
[14] Luxmoore AR, Owen DRJ. The mechanics of syntactic foams. In:
Hillyard NC, editor. The mechanics of cellular plastics. Barking: Applied Science Publishers; 1980. p. 35991.
[15] Krstic VD, Erickson WH. A model for the porosity dependence of
Youngs modulus in brittle solids based on crack opening
displacement. J Mater Sci 1987;22(8):28816.
[16] El-Hadek MA, Tippur HV. Simulation of porosity by microballoon dispersion in epoxy and urethane: mechanical measurements
and models. J Mater Sci 2002;37:164960.
[17] Bardella L, Genna F. On the elastic behavior of syntactic foams.
Int J Solids Struct 2001;38(4041):723560.
[18] Fine T, Sautereau H, Sauvant-Moynot V. Innovative processing
and mechanical properties of high temperature syntactic foams
based on a thermoplastic/thermoset matrix. J Mater Sci
2003;38(12):270916.
[19] Pawlak A, Galeski A. Determination of stresses around beads in
stressed epoxy resin by photoelasticity. J Appl Polym Sci
2002;86(6):143644.
[20] Gupta N, Li G, Jerro D, Woldesenbet E, Pang S-S. Eect of
nano-size clay particles on the exural properties of syntactic
foams. In: Proceedings of the 62nd annual technical conference of
the society of plastics engineers, ANTEC 2004, USA, Society of
Plastics Engineers, p. 132024.
[21] Wouterson EM, Boey FYC, Hu X, Wong S-C. A study on
fracture toughness of syntactic foam. In: International conference
on materials for advanced technologies (ICMAT) proceedings,
MRS Singapore; 2003.
[22] Kawaguchi T, Pearson RA. The eect of particlematrix adhesion
on the mechanical behavior of glass lled epoxies. Part 2. A study
on fracture toughness. Polymer 2003;44(15):423947.
[23] Lange FF. The interaction of a crack front with a second-phase
dispersion. Philos Mag 1970;22(179):98392.