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Received 17 June 2004; received in revised form 4 October 2004; accepted 4 October 2004
Abstract
Methods of predicting effective mechanical properties of composites with an interpenetrating network structure are currently not well
understood, particularly for cases in which the constituent materials have widely differing properties. Alumina–epoxy composites with an
interpenetrating composite structure have been produced via an infiltration process and the elastic properties were measured via the impulse
excitation technique. A strong dependence of properties on composition and processing was observed. Properties were compared with several
mixing law predictions made using compositional data obtained from microstructural analysis. The effective medium approximation (EMA)
was shown to predict properties adequately, whilst others models proved inappropriate.
© 2004 Elsevier B.V. All rights reserved.
Keywords: Interpenetrating network composite; Effective properties; Impulse excitation technique; Effective medium approximation
0921-5093/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2004.10.004
M.T. Tilbrook et al. / Materials Science and Engineering A 393 (2005) 170–178 171
Fig. 1. Microstructural images of alumina epoxy composite samples. Interpenetrating network structures: (A) 5% epoxy; (B) 15% epoxy; (C) 30% epoxy; (D)
45% epoxy. Alumina appears as the light phase, epoxy is the grey phase and the darker spots are pores. Powder composites: (E) 75% epoxy and (F) 90% epoxy.
Alumina appears as the grey phase, epoxy is the light phase and the darker spots are pores.
interpenetrating microstructures cannot be observed in two- structured composites. For samples containing pores, mea-
dimensional micrographs. Fig. 1(a–d) show the interpene- surement of porosity volume fraction was incorporated into
trating network microstructures with the differences between the compositional analysis, by a second thresholding pro-
(a–b) and (c–d) attributable to the buckling of foam ligaments cess. Although a small amount of porosity was observed in
during compression which resulted in increasing microstruc- most samples, this was generally <2% and at most 5%. Error
tural irregularity for higher foam compression ratios in the margins for composition measurements were estimated via
resultant alumina phases (light regions). Fig. 1(e–f) shows perturbation during the thresholding step and from variation
a different morphology with some alumina particle contact in compositions observed across single samples.
(dark regions). After cutting and polishing, the densities were determined
Fig. 2 displays an original greyscale microscope image from mass and dimensional measurements. Composite densi-
and the corresponding black and white image obtained via ties were compared with those predicted using compositions
a digital thresholding process, which was used for volume obtained from image analysis and measured densities of con-
fraction estimation. The samples tested varied in composi- stituent phases, as shown in Fig. 3. The observed disparity
tion across the range 5–50% epoxy for the interpenetrating between the two density measurements, particularly for more
M.T. Tilbrook et al. / Materials Science and Engineering A 393 (2005) 170–178 173
Fig. 2. Microstructural image for 20% epoxy sample: (A) grey-scale image and (B) black and white image after thresholding.
Fig. 5. Young’s modulus values. Experimental results for interpenetrating- Fig. 6. Young’s modulus values. Experimental results for interpenetrating-
network composite () and powder composite (䊉) samples, and theoretical network composite () and powder composite (䊉) samples, computational
predictions: isostress (A); isostrain (B); Hashin–Shtrikman upper (C) and predictions () from Wegner and Gibson [8], and theoretical predictions:
lower (D) bounds. Tuchinskii unit-cell model upper and lower bounds, and effective medium
approximation with ψ = 1 and 6.
where L is the specimen length, b the width, t the thickness,
m the mass and T1 the geometry constant determined from b
and t [27]. Similarly, the relationship used to calculate shear
modulus, G, from the torsional frequency, ftors , was:
Lm B
G=4 f2 (4)
bt 1 + A tors
where A and B are geometry constants determined from L, b
and t [27]. Poisson’s ratio was subsequently calculated as:
E
ν= −1 (5)
2G
Error margins in modulus values were estimated from er-
rors in dimensional measurements and resonant frequency
readings. Errors in Poisson’s ratio results were relatively high
due to build-up of errors from Young’s modulus and shear
modulus calculations. Fig. 7. Shear modulus values. Experimental results for interpenetrating-
network composite samples, and EMA predictions (ψ = 6).
Table 1
Experimentally obtained properties for alumina and epoxy
Property Alumina Epoxy
E (GPa) 390 3.4
Poisson’s ratio, 0.2 0.35
K (GPa) 280 3.8
Fig. 8. Poisson’s ratio values. Experimental results for interpenetrating-
G (GPa) 155 1.3
network composite samples, and EMA predictions (ψ = 6).
M.T. Tilbrook et al. / Materials Science and Engineering A 393 (2005) 170–178 175
Fig. 10. Representative microstructural images, on planes parallel to the direction of foam compaction for (A) 25% epoxy sample and (B) 10% epoxy specimen.
176 M.T. Tilbrook et al. / Materials Science and Engineering A 393 (2005) 170–178
with the experimental results as shown in Fig. 6. This is good By solving these self-consistently for K* and G* using
although such a computational model is time-consuming to MathCad, E* and ν* may be determined for spherical inclu-
produce and limited in applicability. sions (ψ = 1), as shown in Fig. 6. An iterative scheme was
used to calculate composite properties for non-spherical in-
3.4. Effective medium approximation clusions (ψ
= 1).
While it is possible to define different values of ψ for each
For a material with a random grain structure or a matrix- phase, resulting in different shape tensors, this was not pur-
inclusion topology with contacting inclusions, the effective sued in the current work, due to the uncertainty in selecting
medium approximation method may be appropriate [4]. This shape factor values. Rather, a single shape factor was used
technique, based on Hill’s self-consistent model [28], treats for both phases. As seen in Fig. 6, the closest fit was ob-
the composite material as being comprised of ellipsoidal in- tained with the EMA by altering the inclusion shape param-
clusions of each phase, surrounded by an effective medium eter, ψ, to a value of 6. This is not physically unreasonable
with the same properties as the total composite [29,30]. As as microstructural images indicated a fairly irregular inter-
well as composite elastic properties, this concept has been ap- nal geometry, particularly for the epoxy phase. Also, from
plied to effective electrical [31] and transport [32] properties considering the results in Fig. 5, the Poisson’s ratio of the
and to microcracked solids [33]. alumina was assumed to be 0.2, which is lower than values
The derivation, which is outlined here and given in full typically quoted in the literature [22]. This prediction is in-
by Kreher and Pompe [4], utilises the second-order tensor cluded in Figs. 6–9, and in each of these cases shows good
formulation for stress and strain. These are related by the agreement with measured results.
fourth-order compliance tensor: The success of the EMA in simulating elastic proper-
ties for this type of composite structure may be attributed
σ- = C- ε- (6) to its lack of inherent assumption regarding internal geom-
etry. Rather, inclusions are assumed to be surrounded by an
Tensors are denoted by an underline. Considering a single el-
effective medium. In the composites investigated, any partic-
lipsoidal inclusion with compliance, C- , in surrounding mate-
ular microstructural element of alumina or epoxy would be
rial with effective compliance, C- ∗ , and a prescribed far-field
in contact with both alumina and epoxy though not in any
strain, the local strain field is determined via the results of
regular configuration, and thus, is most accurately modelled
Eshelby [34].
via the effective medium concept. This is in agreement with
Applying this self-consistently to each phase of the com-
the conclusions of Christensen [35] and Munro [36].
posite results in a weighted mean for the effective compliance
It is possible that observed deviations from the predictions
tensor, C- ∗ , involving the compliance, C- (n) , and the inclusion
of the EMA could be explained by the observed variation in
shape-dependent strain relation tensor, T- (n) , for each phase:
microstructural morphology across the composition range.
(C- (n) − C- ∗ )T- (n) = 0 (7) Incorporating such effects into a model would be difficult,
however, and of questionable benefit, given the reasonably
where denotes the mean over all phases. This expands to good fit obtained using the EMA in the formulation presented.
yield expressions that implicitly define the effective bulk and
shear moduli, K* and G* :
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