Toughening and Reinforcement of Rigid PVC

with Silicone Rubber/Nano-CaCO3 Shell-Core

Structured Fillers

Ling Yang,1 Yuan Hu,1 Hong Guo,1 Lei Song,1,2 Zuyao Chen,2 Weicheng Fan1
1
State Key Laboratory of Fire Science, University of Science and Technology of China, 230026 Anhui,
People’s Republic of China
2
Department of Chemistry, University of Science and Technology of China, 230026 Anhui, People’s Republic of China

Received 1 September 2005; accepted 28 February 2006

DOI 10.1002/app.24685
Published online in Wiley InterScience (www.interscience.wiley.com).

ABSTRACT: To improve the mechanical properties and composites of PVC/SR/nano-CaCO3 were studied. The
structure of poly(vinyl chloride) (PVC)/nano-CaCO3 nano- results indicate that KH560 has the optimal interfacial
composite, a core (nano-CaCO3)/shell (SR) structured fil- modificatory effect. The environmental scanning electron
ler (40–60 nm) was successfully prepared by refluxing microscope (ESEM) study testified that PVC/SR/nano-
methyl vinyl silicone rubber (SR) and nano-CaCO3 par- CaCO3 nanocomposites had a typical rubber–plastics-
ticles (coupling agent KH550, KH560, or NDZ-101 as toughening mechanism. Ó 2006 Wiley Periodicals, Inc. J Appl
interfacial modifier) in toluene with vigorous stirring, Polym Sci 102: 2560–2567, 2006
according to an encapsulation model. It is effective in
rigid PVC composite’s toughness and reinforcement. The Key words: poly(vinyl chloride); nanocomposites; core-
interfacial modifier’s structure and interaction of nano- shell polymers; morphology; mechanical properties

INTRODUCTION PVC materials.3–6 But one of the most promising means

in preparing inorganic–organic nanocomposite via
Polymer blends are of significant importance because
melt blending, such as PVC–clay nanocomposites,7–9
blending could provide a means for improving me-
were reported successively. Other nanoparticles such
chanical properties as well as processability. On the
as nanometric CaCO3, SiO2, TiO2, and ZnO particles
other hand, incorporation of rubbery polymers low-
have been used to prepare nanocomposites.10–13 And
ers the tensile strength,1 resistance to heat, and pro-
nano-CaCO3 has been one of the most commonly used
cessing behavior of plastics,2 and so it is highly im-
inorganic fillers for PVC.14–16 Wu et al. studied the me-
portant for theory and practice to look for better
chanical properties, morphology, and rheology of the
methods of plastics toughening.
system chlorinated polyethylene (CPE)/nano-CaCO3
In the study of the toughening of common plastics,
master batch as reinforcement filler in PVC; CPE as an
poly(vinyl chloride) (PVC) toughening has attracted
interfacial modifier were studied.15 Although CPE/
great interest owing to its low price and good resist-
nano-CaCO3 master batch has a high toughening effect
ance to aging and corrosion. In the recent decade,
for PVC, using CPE increases the content of halogen in
scientists have already studied elastomer as filler in
material and limits material’s using area.
PVC matrix to improve the processing properties of
The goal of the present study was to investigate the
PVC and achieve rubber–plastics-toughening of rigid
probability of toughening of PVC filled with nano-
CaCO3 particles. To eliminate incompatibility be-
Correspondence to: Y. Hu ([email protected]). tween inorganic–organic interfaces, silicone rubber
Contract grant sponsor: China NKBRSF Project; contract (SR) was used as an interfacial modifier. For this pur-
grant number: 2001CB409600. pose, a kind of master batch of SR/nano-CaCO3 par-
Contract grant sponsor: National Natural Science Founda-
tion of China; contract grant number: 50476026. ticles was prepared via refluxing nano-CaCO3 in tolu-
Contract grant sponsor: Specialized Research Fund for the ene solution of SR. The master batch was employed as
Doctoral Program of Higher Education; contract grant num- filler to prepare nanocomposites with PVC via a melt
ber: 20040358056. mixing; the mechanical properties and morphology
Contract grant sponsor: Program for New Century Excel- were investigated. The correlation between the me-
lent Talents in University.
chanical properties and morphology of nanocompo-
Journal of Applied Polymer Science, Vol. 102, 2560–2567 (2006) sites was established. The toughening mechanisms
V
C 2006 Wiley Periodicals, Inc. were also proposed.
NANO-CaCO3/SR PARTICLE WITH CORE/SHELL STRUCTURE 2561

TABLE I 908C with vigorous stirring, after that the product was
Organo-Functional Coupling Agent Structure dried at 758C for 16 h, then the MVMQ coating nano-
KH550 CaCO3 particles were homogenized by grinding in an
agate mortar and ready for using in PVC formulations.
KH560
NDZ-201
Preparation of PVC nanocomposites
The rigid PVC formulations were mixed on the two-
roll mill at 160–1658C for 10 min, then the resulting
EXPERIMENTAL mixtures were cooled to room temperature for upper
testing. Table II shows the PVC formulations.
Materials
A suspension PVC (S1000, MW: 62,500) employed in
this study was purchased from Qilu Petrochemical, ANALYSES AND CHARACTERIZATION
Shandong Province, China. Methyl vinyl silicone rub- The morphology of MVMQ coating nano-CaCO3 par-
ber (MVMQ, 110-2), with a vinyl content of 0.17%, was ticles was evaluated using bright field transmission
commercially obtained from Dongjue Fine Chemicals electron microscopy (TEM). All of the particles of
(Nanjing). Nano-CaCO3 fillers with an average particle nano-CaCO3 and SR/nano-CaCO3 master batch were
diameter of 40 nm were supplied by Nano-Tech Sci- dispersed in ethanol in an ultrasonic bath for 10 min.
ence and Technology Company, Beijing, China. The fil- TEM images were obtained on a JEOL JEM-100SX
ler was surface treated with coupling agent (Table I) of microscope with an acceleration voltage of 80 kV.
silane coupling agent KH550 and KH560, titanate cou- The morphology of PVC sample’s tensile fractured
pling agent NDZ-101 by the manufacturer from Nanj- surface tore in tensile testing and fractured surface
ing ShuGuang Chemical General Company. The treat- obtained in Notched Izod impact test were studied by
ment method is described as follows: the required vol- environmental scanning electron microscope (ESEM)
ume of the coupling agent was diluted with an equal examination: all the tensile fractured surfaces were
amount of toluene, and a 1:1 solution was formed. The coated with gold–palladium film. The center of the
diluted solution was slowly sprayed, for 10-min peri- fractured surface for each sample was examined on
ods, on the nano-CaCO3 filler contained in a rotating PHILIPS XL 30 ESEM-TMP.
mixer of the Sigma type. The rotation direction of the The tensile tests were carried out using a Universal
mixer was changed every 5 min to ensure distribution Testing Machine DCS-5000 (Shimadzu, Japan) at a
of the coupling agents in the nano-CaCO3 filler. The head speed of 200 mm/min according to ASTM D-
additives, such as a lead complex thermal stabilizer, 638. All measurements were repeated five times and
calcium stearate, and external wax, were provided by the values averaged.
Haolong Chemical, Tianjin, China. The shore A hardness was obtained from LX-A Rub-
ber–Plastics Shore A Sclerometer (Mingzhu Instru-
ments, Jiangdu) according to GB T 531 92.
SAMPLE PREPARATION Notched Izod impact strength was measured with a
SUMITOMO impact tester according to the standard of
Preparation of SR/nano-CaCO3 master batch
ASTM D256 at room temperature. The thickness of the
A given weight of MVMQ (4 g) was dispersed in Izod impact specimens was 1/8 in., and the impact
180 mL toluene and stirred at 908C till MVMQ swelled energy was 4 J.
in toluene completely; nano-CaCO3 (15 g) was scattered The Fourier transform infrared (FTIR) spectra were
into a small amount of toluene before dispersing in recorded using a Nicolet MAGNA-IR 750 spectrome-
MVMQ. The mixture was heated and refluxed for 2 h at ter using a thin film.

TABLE II
Summary of Rigid PVC Compounds
Sample code PVC (g) DOTP (g) TBLS (g) St (g) BPA (g) Packed nano-CaCO3 (g)
EPVC0 100 40 4 0 0.5 None
EPVC1 100 40 4 0.3 0.5 15 (melt blending directly, without modification)
EPVC2 100 40 4 0.3 0.5 15 (coated, without modification)
EPVC3 100 40 4 0.3 0.5 15 (coated, modified by KH550 coupling agent)
EPVC4 100 40 4 0.3 0.5 15 (coated, modified by KH560 coupling agent)
EPVC5 100 40 4 0.3 0.5 15 (coated, modified by NDZ-101 coupling agent)

St, Styrene; BPA, Bisphenol-A.

2562 YANG ET AL.

A differential scanning calorimeter (PerkinElmer 250 nm. But Figure 1(b–e) shows that the coating of
Diamond DSC) was used to examine the thermal prop- SR prevents nano-CaCO3 particles’ aggregation, and
erties of the rigid PVC/SR/nano-CaCO3 nanocompo- so the particles of master batch are symmetrical and
sites at a heating rate of 208C/min under a nitrogen the sizes are about 20–60 nm; the SR shell prevents the
flow. The sample was two-stage-heated. First, the sam- aggregation of nano-CaCO3 particles effectively. A
ple was heated from 30 to 808C and then cooled to reason for this may be the low surface energy of this
room temperature to release the internal stress of the kind of SR and its high molar mass, which causes it to
sample. Second, the sample was reheated from 35 to cover other particles easily and prevents nano-CaCO3
1208C at a heating rate of 208C/min. The Tg of the rigid particles’ aggregation.17
PVC/SR/nano-CaCO3 nanocomposite was recorded
and analyzed.
Mechanical properties
Impact strength is one of the most important mechani-
RESULTS AND DISCUSSIONS
cal properties of plastic–rubber blends since it deter-
Figure 1(a) testifies that nano-CaCO3 particles are easy mines the utility of these materials. It is generally
to aggregate and result in asymmetric sizes from 40 to believed that the interfacial adhesion between the dis-

Figure 1 TEM micrographs of (a) nano-CaCO3 particles and (b)–(e) SR/nano-CaCO3 master batch.
NANO-CaCO3/SR PARTICLE WITH CORE/SHELL STRUCTURE 2563

ESEM morphological analysis

For further study of the mechanisms of reinforcement
effect of SR/nano-CaCO3 for PVC, electromicroscopy
was employed. Figures 4 and 5 give the morphology of
PVC samples’ divulsive surface torn in tensile testing
at different amplifier. From the comparison of Figure
4(b–f) with Figure 4(a) and Figure 1, it can be obtained
that the usage of SR (including melt blending directly),
although does not prevent completely the particles
from aggregation, can effectively reduce nano-CaCO3
particles’ size to improve particles’ dispersion in PVC
matrix. There are many ‘‘filaments’’ in tensile fractured
surface except sample EPVC0 [Fig. 4(a)]. But there are
regular tropism structure be similar to fascicules in
Figure 2 Notched Izod impact strength and Shore A EPVC4 [Fig. 4(e)].
hardness of PVC/nano-CaCO3 nanocomposites versus dif-
ferent coupling agent. Figure 5 shows the morphology at high amplifier.
Figure 5(a) is the morphology of sample EPVC0’s ten-
sile fractured surface, it is obvious that there is sub-
stantial debonding of two phases before yielding in
persed rubber particles and the matrix plays an im-
the composites, and the surface of CaCO3 particles
portant role in the toughening of polymers. Figure 2
are perfectly clean. It can be concluded that there is
presents the notched Izod impact strength and Shore
almost no adhesion between CaCO3 particles and
A hardness of PVC/nano-CaCO3 nanocomposites
PVC matrix, so EPVC0 has the worst mechanical
using different coupling agent, which indicated that
properties. On the other hand, Figure 5(b–f) testify
the nano-CaCO3 particles had a remarkable toughen-
that PVC compounds reinforced by SR/nano-CaCO3
ing effect on PVC. The impact strength of pure PVC
master batch have different morphology. Apart from
(sample EPVC0) was 46.2 kJ/m2, and it increased
some agglomerated particles, a relatively good disper-
slightly to 64.9 kJ/m2 for the PVC/SR/nano-CaCO3
sion is clearly seen. And there are many ‘‘filaments,’’
melt blending directly (sample EPVC1), but increased
shown in Figure 5(b–d) and Figure 5(f), the ‘‘fila-
acutely for PVC/master batch nanocomposites; the
ments’’ are mainly occurring between SR/nano-
impact strength of EPVC4 is high up to 87.5 kJ/m2.
CaCO3 particles, this phenomenon shows that the
Shore A hardness are all increased compared with
‘‘filaments’’ are the coating of SR formed during the
that of EPVC0. It is obvious that the toughening effi-
tensile process. In Figure 5(e), because of better misci-
ciency of SR/nano-CaCO3 master batch on PVC is
bility of PVC and SR/nano-CaCO3 master batch for
much higher than that of normal nano-CaCO3 fillers.
effect of KH560 coupling agent, the ‘‘filaments’’ con-
The strength and elongation at break of PVC/
sists not only of SR but also part of PVC matrix, so the
nano-CaCO3 nanocomposites and PVC/SR/nano-
‘‘filaments’’ is tangled up on the surface of the PVC/
CaCO3 nanocomposites are presented in Figure 3.
SR/nano-CaCO3 nanocomposites. But there is a kind
The PVC/SR/nano-CaCO3 nanocomposites melt
blending directly (sample EPVC1) exhibited a dis-
tinctly higher tensile strength than that of pure PVC,
which revealed that not only the nano-CaCO3 par-
ticles gave a strength enhancement on the PVC ma-
trix, but also SR had a lubricant effect which made
nano-CaCO3 particle have a good dispersion. How-
ever, a further increase in the tensile strength and
elongation at break of PVC sample using SR/nano-
CaCO3 master batch, especially sample EPVC4,
nano-CaCO3 particles were modified by KH560 cou-
pling agent, had the best tensile strength (24.9 MPa)
and the longest elongation at break (390.98%).
From the mechanical properties, it can be con-
cluded that the dispersion effect of the shell-core
structured SR/nano-CaCO3 master batch are better
than that of nano-CaCO3, and SR/nano-CaCO3
master batch have better reinforcing effect on PVC Figure 3 Strength and elongation at break of PVC/nano-
matrix. CaCO3 nanocomposites versus different coupling agent.
2564 YANG ET AL.

Figure 4 ESEM micrographs of tensile-fractured surfaces of PVC nanocomposites (
1000): (a) EPVC0; (b) EPVC1;
(c) EPVC2; (d) EPVC3; (e) EPVC4; (f) EPVC5.

of structure such as region marked C. Figure 6 gives shown in Figure 11. Owing to the incorporation of
the morphology of region ‘‘C’’. It is obvious that there coupling agent into the composites, the strong inter-
is an excellent adhesion between master batch par- action between the filler and polymer transformed
ticles and PVC matrix; the two phase structure disap- structurally the composite into an interpenetrating
pears and many regular and strong tropistic fascicu- polymer network, during the tensile process regular
lus slice-layered structures are formed on the tensile- tropism fasciculi are formed and arranged orderly to
fractured surfaces which apparently bond the two form slice-layered structure.
phases together (region marked A and B). The toughening of PVC by microsized CaCO3 par-
The scheme for interactions of the PVC/nano- ticles could be explained by the crack front bowing
CaCO3 composite and PVC/SR/nano-CaCO3 are mechanism.18 However, the size of nano-CaCO3 par-

Figure 5 ESEM micrographs of tensile-fractured surfaces of PVC nanocomposites (
6000): (a) EPVC0; (b) EPVC1;
(c) EPVC2; (d) EPVC3; (e) EPVC4; (f) EPVC5.
NANO-CaCO3/SR PARTICLE WITH CORE/SHELL STRUCTURE 2565

characteristics. Several long shearing bands are par-

allelized to each other and few cavitations emerge
on the fracture surface of sample EPVC4 in which
SR/nano-CaCO3 master batch were modified with
KH560 [Fig. 7(e)], indicating that the PVC/SR/nano-
CaCO3 modified with KH560 blend fractures in a
ductile mode. Meanwhile, the shearing bands
become quite short and less orientational, and a high
degree of cavitation is found on the fracture surface
of the sample EPVC3 and EPVC5 in which SR/nano-
CaCO3 master batch were modified with KH550 and
NDZ-101, respectively, [Fig. 7(d and f)]. And there
are only some ‘‘filaments’’ [Fig. 7(b and c)], that rep-
resent sample EPVC1 and EPVC2, respectively, but
in Figure 7(b) there are more cavitations than that in
Figure 6 ESEM image of the region signed as ‘‘C’’ in
Figure 5e (
6000). Figure 7(c). All these phenomena suggest that the
rigid PVC samples with SR have better compatibil-
ity, and the coupling agents lead to inseparable inter-
ticles used in this study is from several 10 nm to sev- action between PVC matrix and SR/nano-CaCO3
eral 100 nm (because of serious aggregation), and par- master batch. Along with the increasing interphase
ticle of SR/nano-CaCO3 is 40–60 nm, the applicability compatibility of the PVC matrix and SR/nano-CaCO3,
of the bowing mechanism is questionable, because the PVC/SR/nano-CaCO 3 nanocomposites have
such small-sized rigid particles may not be able to tighter and tighter microstructures with less cavi-
resist the propagation of the crack. Obviously, the tation, so these PVC nanocomposites not only have
toughening effect of SR/nano-CaCO3 master batch on better impact strength, but also have higher shore A
PVC could be contributed to a new mechanism. Such hardness (as shown in Fig. 2).
a high toughening effect for PVC/elastomer/nano-
CaCO3 nanocomposites was attributable to a typical
rubber–plastics-toughening mechanism.4,6,15
Analysis of coupling agent effect
To evaluate the toughening mechanism, we stud-
ied the fractured surfaces in Notched Izod impact The use of different kind of coupling agent produced
test. Figure 7 reveals the ESEM photographs of the different interaction between PVC matrix and SR/
fractured surfaces of PVC composites. Similar to the nano-CaCO3 master batch and lead to different me-
tensile behavior, pristine PVC exhibits brittle failure; chanical properties and ESEM morphologies of PVC/
but the nanocomposites contained SR show ductile SR/nano-CaCO3 nanocomposites, which further de-

Figure 7 ESEM photographs for the fracture surfaces of (a) EPVC0; (b) EPVC1; (c) EPVC2; (d) EPVC3; (e) EPVC4; (f)
EPVC5.
2566 YANG ET AL.

pends on the interfacial adhesion of the PVC matrix-SR

and SR-nano-CaCO3. Figure 8 compares the FTIR spec-
tra of EPVC0–EPVC5. These nanocomposites have
almost the same FTIR spectra [see Fig. 8(a)]. From Fig-
ure 8(a) it can be seen that in the spectrum of PVC
nanocomposites exist aliphatic groups of CH (2960 and
2929 cm1), CH3 (1380 cm1), and CH2 (1450 cm1).
The peaks between 3000 and 2800 cm1 indicate the
presence of CH3, CH2, and CH functional
groups, and the bands between 600 and 700 cm1 can be
attributed to CCl stretching vibrations. SiCH3
absorption appeared at 1260 cm1, the SiOSi
absorption had a peak at 1019, and 780 cm1 was the
absorption of H3CSiCH¼ ¼CH2, the bands between
1620 and 1670 cm1 are attributed to C¼ ¼C stretching
vibrations.19,20 These results show that there are no new Figure 9 Tg of rigid PVC/SR/nano-CaCO3 nanocomposites.
chemical bond between PVC matrix and SR elastomer
shell and nano-CaCO3 core. But the peaks marked as
agent KH560]. So in the process of tensile, the nano-
‘‘arrow’’ in Figure 8(b) suggest that there are new chem-
composite EPVC4 formed oriented fasciculus in the
ical bonds formed. Analyzing every component of the
tensile-fractured surface [Fig. 4(e)].
PVC nanocomposites, it can be concluded that the new Tg temperatures of PVC/SR/nano-CaCO3 nano-
chemical bonds are attributed to chemical interaction composites also probe the interactions in these materi-
of PVC and coupling agent, KH550 and KH560. The
als. Figure 9 shows the DSC curves of PVC/SR/nano-
scheme for chemical interactions of PVC matrix and
CaCO3 nanocomposites. Compared with EPVC0 (Tg
coupling agent are shown in Figure 10. Figure 10(a) is
¼ 82.388C), Tg temperatures of sample EPVC1 (Tg
the intermolecular hydrogen bond between PVC and
¼ 70.68C) and EPVC2 (Tg ¼ 79.28C) are decreased, this
KH550; Figure 10(b–d) is the intermolecular hydrogen
result testified that SR-made nano-CaCO3 particles
bonds between PVC and KH560. Obviously, (a)–(c) are
diapered in PVC matrix well and increased the degree
stable, but (d) is unstable and instantaneous. Because of molecular chain movement of PVC. Meanwhile, Tg
of these kinds of hydrogen bonds, the interaction of sample EPVC3, EPVC4, and EPVC5 are increased
between PVC and SR/nano-CaCO3 master batch are
to 88.18C, 99.88C, and 88.98C, respectively. The sample
different as shown in Figure 11). Owing to the incorpo-
EPVC4 of SR/nano-CaCO3 master batch modified
ration of intermolecular hydrogen bonds, the strong
with KH560 has the maximum Tg. The major driving
interaction between filler and polymer transformed
structurally the composite into an interpenetrating
polymer network [Fig. 11(d) PVC/SR/nano-CaCO3
master batch ternary nanocomposite with coupling

Figure 8 FTIR spectra for PVC/SR/nanoCaCO3 nanocom- Figure 10 Schematic representation for intermolecular hy-
posites (1) EPVC1; (2) EPVC2; (3) EPVC3; (4) EPVC4; drogen bonds between PVC matrix and coupling agents
(5) EPVC5. (a)–(d).
NANO-CaCO3/SR PARTICLE WITH CORE/SHELL STRUCTURE 2567

of nanocomposites could be improved remarkably by

the incorporation of SR and coupling agent. The
ESEM study indicated that the KH560-treated SR/
nano-CaCO3 particles in the PVC matrix (sample
EPVC4) were evenly distributed, and eliminated
incompatibility between inorganic–organic interfaces
effectively. The impact strength of EPVC4 containing
SR/nano-CaCO3 master batch modified with KH560
is high up to 87.5KJ/m2, tensile strength is 24.9 MPa,
and elongation at break is 390.98%. Such a high tough-
ening effect for PVC/SR/nano-CaCO3 nanocompo-
sites was attributable to a typical rubber–plastics-
toughening mechanism.

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