International Communications in Heat and Mass Transfer 37 (2010) 10361043

Contents lists available at ScienceDirect

International Communications in Heat and Mass Transfer

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / i c h m t

Effect of organoclay on the mechanical/thermal properties of microcellular injection

molded PBTclay nanocomposites
Shyh-shin Hwang a,, Sung-po Liu a, Peming P. Hsu b, Jui-ming Yeh c, Kung-chin Chang d, Ying-zhong Lai a
a

Department of Mechanical Engineering, Ching-Yun University, Chung-Li, 32097, Taiwan, ROC

Department of Computer Application Engineering, Far-East University, Tainan, 74420, Taiwan, ROC
Department of Chemistry, Chung-Yuan Christian University, Chung-Li, 32023, Taiwan, ROC
d
Taiwan Textile Research Institute, Tucheng, 23674, Taiwan, ROC
b
c

a r t i c l e

i n f o

Available online 9 July 2010

Keywords:
Compound
Organoclay
Nanocomposites
Microcellular
Twin-screw extruder
PBT

a b s t r a c t
An organically modied montmorillonite (MMT) was compounded with polybutylene terephthalate (PBT) in a
twin-screw extruder. The organoclay PBT nanocomposites were then injection molded by conventional and
microcellular methods. Nitrogen was used as the blowing agent. The effect of organoclay content, organoclay size (8
and 35 m), and speed of the screw (80 and 100 rpm) on the mechanical and thermal properties were investigated.
The results showed that when the MMT content was 1.0 wt.%, the nanocomposites have maximum tensile
strength, wear resistance, and cell density. Moreover, the larger the particle size, the greater the tensile strength.
The screw speed during compounding also affected the mechanical strength. The higher speed of the screw
increased the tensile strength of the nanocomposites. The addition of MMT also helped the thermal stability of the
PBT/clay nanocomposites. The WXRD results showed that when MMT loading is 1.0 wt.%, the nanocomposites
have maximum d-spacing structure. TEM results showed that MMT is well dispersed on the nanocomposites at a
MMT loading of 1.0 wt.%.
2010 Elsevier Ltd. All rights reserved.

1. Introduction
Polybutylene terephthalate (PBT) is commonly used as an engineering plastic. It has many advantageous properties, including good ow
properties, excellent thermal stability, and good chemical resistance.
However, PBT has a low heat distortion temperature and poor
mechanical properties. Many attempts have been made to improve
these properties of PBT by blending it with different llers. These
composites are mostly polymer clay nanocomposites (PCN). Adding a
small amount of clay to the polymer gives PCN enhanced physical and
mechanical properties in aspects such as Young's modulus, tensile
strength [1], and ame retardancy [2], by comparison with neat
polymers. For example, Zhou et al. [3] studied the effect of the epoxy
on the mechanical properties and melt viscoelastic behavior of PBT/
MMT nanocomposites. The results showed that with epoxy as the
compatibilizer, the clay is easily intercalated and dispersed well on the
PBT matrix. Therefore, the PCN demonstrated better tensile and impact
properties than neat PBT. However, the excess epoxy reduced the
material performance. Amendola et al. [4] employed two commercial
organoclays melt compounded with PBT with different clay loadings
and screw speeds. It was found that PCN exhibiting mixed intercalated/

Communicated by W.J. Minkowycz.

Corresponding author.
E-mail address: stanhwang@cyu.edu.tw (S. Hwang).
0735-1933/$ see front matter 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.icheatmasstransfer.2010.06.010

exfoliated clay layer structure and the extent of exfoliation increased

with extrusion rate for low amounts of clay. Chow [5] studied the
mechanical/thermal properties of cyclic extrusion PBT/MMT nanocomposites followed by injection molding with 3 wt.% clay loading. He found
that organoclay improved the crystallinity of PBT. The melting
temperature, crystallization temperature, and degree of crystallinity of
PCN extruded once were comparable with that extruded twice. This
revealed that PBT/MMT intercalated nanocomposites exhibited good
retention of mechanical/thermal properties after being extruded twice
followed by injection molding.
Wu. et al. [6] investigated the immiscible morphology of PBT/PE
blend nanocomposites by melt compounding. They concluded that PE
domain size was reduced when the PBT phase was continuous (PBT/
PE = 60/40). The clay prevented the agglomeration of the PE particles.
Chang and Mun [7] used PBT/MMT nanocomposite ber to investigate
the thermal/mechanical properties of the nanocomposite. Fiber was
spun for different draw ratios. The tensile properties of the nanocomposite bers increased with increasing organoclay contents at draw
ratio = 1. But the tensile properties of the bers decreased with
increasing draw ratio.
Several methods for the preparation of the PCNs have been
developed, including in-situ polymerization, melt compounding, and
template synthesis [8]. Many papers have reported the preparation of
polymer nanocomposites by in-situ polymerization [911]. This
technique gives the PCN a good degree of exfoliation, which cannot
be achieved by melt compounding of polymer and clay. A more

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1037

Table 1
Effects of organoclay content, clay size, and screw speed on the tensile strength of the
PBT/MMT nanocomposites.
Organoclay
content (wt.%)

Screw speed 100,

Clay size 8 m
Solid/foamed
(kgf/mm2)

Screw speed 100,

Clay size 35 m
Solid/foamed
(kgf/mm2)

Screw speed 80,

Clay size 35 m
Solid/foamed
(kgf/mm2)

Neat PBT
0.5 wt.%
1.0 wt.%
2.0 wt.%
3.0 wt.%
4.0 wt.%

4.908/3.195
4.967/3.391
5.082/3.405
5.056/3.387
4.935/3.198

4.908/3.195
5.166/3.395
5.222/3.651
5.123/2.917
4.718/2.303
4.372/1.780

4.908/3.195
5.012/
5.143/3.219
4.986/1.189
4.745/0.982
4.65/1.297

Table 2
Effects of organoclay content, clay size, and screw speed on the size of the PBT/MMT
foams.
Organoclay
content (wt.%)

Screw speed 100,

Clay size 8 m
(m)

Screw speed 100,

Clay size 35 m
(m)

Screw speed 80,

Clay size 35 m
(m)

Fig. 2. Wide-angle XRD patterns of solid MMT/PBT nanocomposites at 1.0 wt.% clay
loading with 35 m clay size at different screw speeds.

Neat PBT
0.5 wt.%
1.0 wt.%
2.0 wt.%
3.0 wt.%
4.0 wt.%

164
157
105
200
219

164
134
78
90.4
106
273

164

93
159
210
220

2. Materials and experimental

economic method that uses conventional polymer processing is melt

compounding of the polymer with the organoclay [12,13].
PCN is also applied during the foaming process where the clay
serves as the nucleation agent, leading to a small cell size [14] that is
useful in acoustic and thermal insulator applications [8]. Microcellular
foaming blends polymer and supercritical uid, creating millions of
microcells whose size is less than 100 m [15], improving the part's
dimensional stability [16]. However, few reports associated with PBT
clay on the microcellular foaming have been published. In this paper,
we investigate the effect of the organoclay content, size and screw
speed of the melt compounding on the mechanical/thermal properties of the microcellular injection molded PBT/MMT nanocomposites,
based on the studies of thermogravimetric analysis (TGA), differential
scanning calorimetry (DSC), tensile test, wear resistance, and SEM,
respectively.

Fig. 1. Wide-angle XRD patterns of solid MMT/PBT nanocomposites with 8 m clay size.

MMT with a cation-exchange capacity of 90 mequiv/100 g was used

as the clay, while stearylbenzyldime-ammonium chloride (STAC),
supplied by Sd-Chemie (Germany), was used as an organic modier
of MMT. Two different organoclay sizes, Nanol 9 and 919 (8 m and
35 m), were used in this study to investigate the effect of clay size on
the mechanical/thermal properties of the PCN. Pure PBT, DHK220, was
supplied by Shin-Kong Co. Ltd. and PBT/MMT nanocomposites were
prepared by twin-screw extruder (KTX-30, Cobel Co., Japan). To study
the effect of screw speed on the properties of the PBT/MMT
nanocomposites, two different speeds, 80 and 100 rpm, were used in
this study. The mixing ratios of MMT/PBT were 0 wt.%, 0.5 wt.%, 1 wt.%,
2 wt.%, and 3 wt.% respectively.

Fig. 3. TEM image of solid 1 wt.% MMT/PBT nanocomposites with 8 m clay size.

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S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

Fig. 6. DSC curves of the melting temperature in solid MMT/PBT nanocomposites for
clay size 35 m and screw speed 100 rpm.

Fig. 4. TEM image of solid 3 wt.% MMT/PBT nanocomposites with 8 m clay size.

2.1. Injection molding machine

The injection-molding machine used was the Arburg 420C Allrounder 1000-350, equipped with Mucell capability. Nitrogen was used as
the gas source. In this study, process conditions were kept constant in
order to examine the effect of the organoclay contents, organoclay sizes
on the mechanical and thermal properties. A mold of ASTM standard
tensile and impact sample was used in this study.
2.2. Instrumentations
An SEM was used to observe the morphology of the cell structure in the
foamed polymerclay nanocomposites material. The SEM image of the cell
structure was taken on a JEOL JSM6360. Specimens were cut into smaller
pieces and gold was sputtered onto the surface. They were then inspected
using the SEM. The samples for TEM study were prepared by placing the

Fig. 5. TGA curves of solid MMT/PBT nanocomposites for clay size 35 m and screw
speed 100 rpm.

bulk of the PCN materials into epoxy resin capsules, followed by curing the
epoxy resin at 100 C for 24 h in a vacuum oven. The cured epoxy resin
containing PCN materials was microtomed with a Reichert-Jumg UltracutE into slices 6090 nm thick. Subsequently, one layer of carbon, about
10 nm thick, was deposited on these slices on 300-mesh copper nets for
TEM observations on a JEOL JEM-2010 with an acceleration voltage of
200 kV. Wide-angle X-ray diffraction study of the samples was performed
on a Panalytical X'Pert Pro X-ray diffractometer with copper target and Ni
lter at a scanning rate of 2/min. A DuPont thermal analysis system
equipped with model TA DSC-Q10 and TA TGA-Q50 was used for the
thermal analyses under N2 and air ow. The tensile test of the ASTM
standard sample was carried out using a tensile test analyzer, an HT9102 M, manufactured by Hong-Da Company.
A ball-on-plane Schwingung Reibung Verschkiss (SRV) oscillation
friction wear tester was used to carry out the wear measurement. The
diameter of the steel ball was 10 mm and the hardness of the steel ball
was 62 2 HRc. The applied load was 60 N.
3. Results and discussion
The effects of organoclay content, clay size, and screw speed on the
tensile strength and cell size of the PBTclay nanocomposite materials

Fig. 7. Loaddisplacement curves of solid MMT/PBT nanocomposites with 8 m clay

size at 100 rpm screw speed.

S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

1039

Fig. 8. Loaddisplacement curves of foamed MMT/PBT nanocomposites with 8 m clay

size at 100 rpm screw speed.

Fig. 10. Tensile strength comparison of solid PCN at clay loading of 1.0 wt.% with
differing clay sizes and screw speeds.

varied from 0 to 4 wt.% of organoclay with respect to the PBT, as

summarized in Tables 1 and 2 respectively.

around 23, implying that the clay has an intercalated layer structure,
as shown in Figs. 3 and 4. For the morphological image study (Fig. 3), the
TEM micrograph of the PCN material with clay size 8 m at MMT 1 wt.%
content shows the dispersion of intercalated MMT within the PBT
matrix. In the micrographs, the bright eld shows the PBT matrix, while
the dark lines show the transverse section of the MMT layers. Some of
the clay layers slightly aggregate when the MMT content is 3 wt.%, as
shown in Fig. 4.

3.1. Characterization
Fig. 1 shows the wide-angle powder XRD patterns for a series of
solid PCN materials with the clay size of 8 m at the screw speed of
100 rpm. The diffraction peaks of the PCN materials at the [001]
direction for clay loadings of 0.5 wt.%, 1 wt.%, 2 wt.% and 3 wt.% were
found to be 2 = 2.49, 2.36, 2.45, and 2.64 respectively, corresponding
to a d-spacing of 3.35 nm, 3.74 nm, 3.61 nm and 3.55, respectively.
Generally, the d-spacing of the organoclay is around 1.89 and
2.03 nm for clay sizes of 8 and 35 m, respectively. However, slight
aggregation of the clay occurred at clay loadings of 2 wt.% and 3 wt.%,
which caused d-spacing narrowing. Fig. 2 shows the wide-angle powder
XRD patterns for the solid PCN materials with a clay size of 35 m at clay
loading of 1.0 wt.% at different screw speeds (80 and 100 rpm). It is
observed that the PCN at high speed suffered high shear rates, which
made the clay layer more dispersed. Moreover, the larger clay size
results in longer d-spacing layers than the smaller clay size. For the two
different clay sizes used, it is seen that the diffraction peaks appear

Fig. 9. Tensile strength comparison of solid PCN at differing clay loadings, clay sizes, and
screw speeds.

3.2. Thermal stability

Fig. 5 shows the TGA curves of the MMT/PBT nanocomposites for
the clay size 35 m and a screw speed of 100 rpm, as well as the neat
PBT, under atmosphere. In general, one major stage of weight loss
appears, starting from 390 C, and ending at 430 C. This corresponds
to the structural decomposition of the polymer. For PCN materials,
clay has been found to enhance the thermal stability of the polymer
[17,18]. We found that the beginning of thermal decomposition in
these nanocomposites shifted slightly, to a higher temperature, than
that of neat PBT. DSC measurements showed that the addition of the
organoclay results in an increase in the melting temperature, relative
to neat PBT, as shown in Fig. 6.

Fig. 11. Wear resistance comparison of solid PCN with differing organoclay contents,
sizes, and screw speeds.

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S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

3.3. Mechanical properties

ASTM standards D 638-99 and D 256-99 were used as the tensile
and impact tests, respectively. To investigate the effect of clay size and
screw speed of twin-screw extruder on the tensile strength of solid
molding, two different clay sizes and screw speeds were used in this
study. The clay sizes were 8 m (Nanol 9) and 35 m (Nanol 919)
and screw speeds of the twin-extruder were 80 rpm and 100 rpm. The
relationship between the mechanical properties and the clay content

of solid and foamed PCN with 8 m clay (Nanol 9) at 100 rpm screw
speed is shown in Figs. 78 respectively. Neat PBT is a very ductile
material. Adding a small amount of MMT can increase its tensile
strength but decreases its ductility. The tensile strength reaches its
maximum at a clay loading of 1 wt.% and then levels off at loadings of
2 wt.% and 3 wt.%. Foamed PBT/MMT nanocomposites have similar
trends in tensile strength as the clay loading increases, as observed in
solid molding, but the elongation of the foamed PCN is worse than
that of the solid PCN.

Fig. 12. SEM of worn surfaces of solid PCN with differing organoclay contents, sizes, and screw speeds.

S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

Fig. 9 shows the tensile strength comparison of solid PCN at

different screw speeds (100 and 80 rpm) and clay sizes (8 and 35 m).
It is observed that neat PCN material at high shear rate (high screw
speed) has high tensile strength. The high shear rate made the dspacing of the layer clay widen (Fig. 2), increasing the tensile strength.
Furthermore, PCN with large clay size (35 m) has greater tensile
strength than that of the small clay size (8 m). While one research

1041

group reported that particle size has a major effect on the wear rate,
with larger sizes resulting in poorer wear resistance, there does not
appear to be a signicant effect on the friction coefcient [17].
Among the three PCNs, the maximum tensile strength is attained
at the clay loading of 1.0 wt.% no matter what the clay sizes and screw
speeds are. Fig. 10 shows the load displacement curves of the three
PCNs with 1.0 wt.% clay loading. PCN with large clay size has larger

Fig. 13. Cell structure of PBT/MMT nanocomposite foams with differing organoclay contents, sizes, and screw speeds.

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S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

tensile strength but is more brittle than PCN with small clay size.
Furthermore, PCN at the same clay size extruded at high speed has a
greater tensile strength than that extruded at low speed. PCN
extruded at high speed suffers higher shear rates during processing,
which creates a more dispersed clay layer and enhances the tensile
properties of the PCN [4].

Where f is the foam density and p is the density of solid polymer.

The void fraction () or weight reduction of polymer foams can be
calculated from Eq. (2) [20].
= 11 = VER

The foam cell density (Nf) can be calculated from Eq. (3) [21].
3.4. Wear resistance
3=2

A ball-on-plane Schwingung Reibung Verschkiss (SRV) oscillation

friction wear tester was used to carry out the wear measurement. The
diameter of the steel ball was 10 mm and the hardness of the steel ball
was 62 2 HRc. The applied load was 90 N. It is well known that wear
resistance is proportional to the tensile strength, meaning that
material with high tensile strength also has high hardness and wear
resistance. Fig. 11 shows the wear resistance comparison of solid PCN
with differing organoclay contents, sizes and screw speeds. As clay
loading of the PCN increases, weight loss decreases (high wear
resistance) due to the strength enhancement. As the clay loading
increases up to 1 wt.%, weight loss decreases, and then levels off due
to the strength decay of the PCN. Among the three materials, PCN with
35 m clay size and a screw speed of 100 rpm has the maximum
tensile strength and wear resistance.
Fig. 12 shows an SEM image of the worn surfaces of the solid PCNs
at differing organoclay contents, sizes and screw speeds. We can see
that as the strength of the PCN increases (Fig. 12a), the material is
more rigid and its worn surfaces are smoother than those of the high
loading clay PCN (Fig. 12d). The worn surfaces in Fig. 12d, e, and f are
rough, showing obvious signs of abrasive and adhesive wear. By
contrast, a relatively smooth and uniform worn surface is formed on
the PCN (Fig. 12a, b, and c). This is consistent with previous friction
and wear studies on PA6/SiO2 nanocomposites [19].
3.5. Effect of clay content, clay size and screw speed on PBT
nanocomposites foams
Cell size, volume expansion ratio (VER), and cell density, are the
three main parameters for judging a foam structure [20]. VER can be
calculated from Eq. (1) [15].
VER = p = f

Nf = n =A

VER

where n is the number of cells and A is the area taken from the SEM
picture. Table 2 shows the cell size of the microcellular injection molded
MMT/PBT nanocomposites at different organoclay contents, sizes and
screw speeds. The neat PBT and PCN materials were microcellular
injection foamed with 0.8 wt.% N2. Evidently, as the content of MMT
increases, the cell size decreases, leveling off when clay content exceeds
1.0 wt.% no matter what the clay sizes and screw speeds. Further, in the
PCNs, when the clay size increases, the cell size decreases. This is in
agreement with most previous foaming results [14,21], where well
dispersed clay particles in polymer nanocomposites were shown to
have smaller cell sizes than in neat polymer. This can also be explained
from the tensile strength of the foamed MMT/PBT nanocomposites. The
foamed PCN has the maximum tensile strength at an organoclay loading
of 1.0 wt.%, a clay size of 35 m, and a screw speed of 100 rpm. In turn,
foamed PCNs has the smallest cell size at the clay loading of 1.0 wt.%, a
clay size of 35 m, and a screw speed of 100 rpm. Fig. 13 shows the cell
structure of foamed MMT/PBT nanocomposites with different organoclay contents, sizes and screw speeds.
Pure PBT foam had the largest cell size of the 3 batch foams studied
here, on the order of 164 m, as shown in Table 2. Foamed cell size
was approximately 105, 78 and 93 m for the PBT nanocomposite
foam with 1.0 wt.% organoclay under identical process conditions for
clay size/screw speeds equaling 80 m/100 rpm, 35 m/100 rpm, and
35 m/80 rpm respectively. As the organoclay content in the PBT
nanocomposites increased, the cell size in the nanocomposite foams
decreased. The cell size levels off when the clay content exceeds 1 wt.
%. This is caused by the clay layer aggregation, as shown in Fig. 4.
Fig. 14 also demonstrates the foam cell density changes with pure
PBT and its nanocomposites of clay size 35 m and screw speed 100 rpm
at different organoclay contents. The foaming process decreases the cell
size and increases the cell density. In general, microcellular nanocomposite foams have higher tensile strength but lower impact strength

Fig. 14. Cell size and cell density vs. clay content in nanocomposite foams of clay size 35 m and screw speed 100 rpm.

S. Hwang et al. / International Communications in Heat and Mass Transfer 37 (2010) 10361043

than their neat resin counterparts. The effect of the nano-clays on the
mechanical properties is also related to the weight reduction [22]. The
addition of clay to polymer can create more nucleation sites for foaming
and can produce smaller cell sizes by comparison with neat polymer. In
turn, a foamed polymer with smaller cell sizes has less weight reduction,
which enhances the tensile strength [23]. In addition, the foamed
polymer with large cell sizes has a thinner cell wall thickness and hence
tends to have lower tensile strength.
4. Conclusions
In this study, a series of PCN materials consisting of commercial PBT
and organoclay were successfully prepared using melt compounding.
The as-prepared PCN materials were then subjected to microcellular and
conventional injection molding. The samples were characterized by XRD
and TEM. We found that addition of organoclay to the PBT resulted in an
increase in mechanical strength and an increase in thermal stability,
based on analysis by tensile, TGA, and DSC tests. Furthermore, the
incorporation of organoclay into the PBT matrix showed a decrease in
the cell size based on the cell morphology measurement. The organoclay
size and screw speed during melt compounding affected the tensile
strength of the PCN as well.
Acknowledgment
This work was supported by the National Science Council grant
NSC 96-2221-E-231-011.
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