Study on Preparation and

Properties of Silane-
crosslinked Polyethylene/
Magnesium Hydroxide/
Montmorillonite
Nanocomposites
LEI SONG, MING LI AND YUAN HU*
State Key Laboratory of Fire Science, University of Science and Technology
of China, Hefei, Anhui 230026, PR China

HONGDIAN LU
Department of Chemical and Material Engineering, Hefei University, Hefei
Anhui 230022, PR China
(Received April 16, 2007)

ABSTRACT: Silane-crosslinked polyethylene/magnesium hydroxide/organo-

montmorillonite nanocomposite is prepared from linear low density polyethylene
(LLDPE), vinyltrimethoxysilane, magnesium hydroxide (MH), and organo-
montmorillonite (OMT). The morphology is characterized by the X-ray
diffraction and high resolution electron microscopy. It is indicated that the
intercalated morphology is formed in the polymer matrix. The mechanical
properties, thermal stability, flammability, and crystallization are investigated
by tensile, limiting oxygen index, cone calorimetry, thermogravimetry, and
differential scanning calorimetry experiments. Results indicate that the cross-
linked nanocomposite shows lower thermal-oxidative stability and fire safety
than the crosslinked LLDPE/MH composite at the same additive level,
the reason is postulated to be that the presence of MH and OMT decreases
the crosslinking degree and the crosslinking network structure prevents the
migration of OMT layers to the surface.

*Author to whom correspondence should be addressed. E-mail: yuanhu@ustc.edu.cn

JOURNAL OF FIRE SCIENCES, VOL. 26 – November 2008 493

0734-9041/08/06 0493–15 $10.00/0 DOI: 10.1177/0734904108092117
ß SAGE Publications 2008
Los Angeles, London, New Delhi and Singapore

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494 L. SONG ET AL.

KEY WORDS: polyethylene, crosslinking, magnesium hydroxide, mont-

morillonite.

INTRODUCTION

POLYETHYLENE (PE) HAS been known as an excellent dielectric and

insulating material. However, its relatively low upper use temperature
has limited its use. Crosslinking is an effective way to enhance the
thermal and mechanical properties of PE, and silane crosslinking has
got the most attention in recent years for its advantages such as being
cost-effective and easily operated [1–8]. Silane crosslinking enhances the
thermal stability; however, silane-crosslinked polyethylene (SXPE) is
still combustible. Therefore, it is strongly required to increase the flame
retardancy of SXPE. Magnesium hydroxide (MH) has been widely used
as halogen-free flame retardant for PE [9–11]. Meanwhile, the polymer/
montmorillonite nanocomposites exhibit dramatic concurrent enhance-
ments of thermal stability, flame retardancy, mechanical, and barrier
properties even when employing small loading levels of montorillonite
(510 wt%) when compared to pure polymer [12–14]. Therefore, it is
worthwhile to investigate the effect of the combination of OMT and
MH in SXPE.
In this study, flame retardant silane-crosslinked LLDPE composites
using MH and MH/OMT were prepared. Their mechanical and flame
retardant properties, thermal-oxidative stability, and nonisothermal
crystallization behaviors were investigated.

EXPERIMENTAL

Materials

Linear low density polyethylene (LLDPE, DFDA7042) was supplied

by Qilu Petrochemical Company. The initiator dicumyl peroxide (DCP)
and dibutyltin dilaurate (DBDL) were supplied by Shanghai Experiment
Reagent Company, and vinyltrimethoxysilane (VTMS) was supplied by
Hefu Chemistry Company. The maleated linear low density polyethylene
(MAPE) with approximately 1.1 wt% maleic anhydride used as compa-
tibilizer, OMT (median part size: d50 ¼ 2 mm) which has been prepared
from pristine montmorillonite by ion exchange reaction using hexade-
cyltrimethylammonium bromide, and the magnesium hydroxide (MH)

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Preparation of Silane-crosslinked Nanocomposites 495

(median part size: d50 ¼ 1 mm) were kindly provided by Keyan Chemistry
Co. All these commercial chemicals were used directly without further
purification. Before preparation, LLDPE, MH, and OMT were dried
at 1008C for 12 h.

Preparation

Samples were prepared by two-step method including grafting

and crosslinking process. The identifications and formulations of all
the samples are listed in Table 1. In the grafting process, all the
VTMS-grafted samples were prepared with a twin-roll mill (XK-160,
JiangSu, China). For PE02, LLDPE/MAPE was melted at 1308C, the
mixture of 2.0 phr (part of reagent per hundred parts of polymer) VTMS,
0.1 phr DCP, and 0.1 phr DBDL was added to melted LLDPE/MAPE and
the mixture (LLDPE/MAPEþVTMSþDCPþDBDL) was melt-blended
for about 10 min to obtain VTMS-grafted LLDPE. The same procedure
was used to prepare PE04 and PE05. For theses samples, MH or MH/
OMT was added to melted LLDPE/MAPE, and the mixture (LLDPE/
MAPEþMH or LLDPE/MAPEþMH/OMT) was melt-blended for about
5 min at 1308C; Then the mixture of 2.0 phr (part of reagent per hundred
parts of polymer) VTMS, 0.1 phr DCP, and 0.1 phr DBDL was added, and
10 min later the sample was obtained. All the grafted samples were first
compression molded at 1308C into 1 or 3 mm thick sheets under a pressure
of 9 MPa for 10 min. In the crosslinking process, the grafted samples
were immersed into hot water (808C) for 12 h to get crosslinking samples.

Characterization

X-ray diffraction (XRD) was carried out on PE05 using a Japan Rigaku
Dmax-rA X-ray diffractometer (30 kV, 10 mA) with Cu ( ¼ 0.154178 nm)

Table 1. The identifications and formulations and the values of

mechanical properties of all samples: (C) represents as
crosslinked sample.

Sample Composition(phr) Gel content EB TS

code LLDPE/MAPE/MH/OMT (%) (%) (MPa)

PE01 75/25/0/0 / 887.000 18.382

PE02 75/25/0/0(C)a 30.5 748.833 22.987
PE03 75/25/90/0 / 400.875 11.622
PE04 75/25/90/0(C)a 19.6 159.400 13.302
PE05 75/25/85/5(C)a 18.1 87.625 13.385

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496 L. SONG ET AL.

irradiation at about 2/min in the range of 1.5–10. High resolution

electron microscopy (HREM) observations were performed for PE05.
The HREM specimen was cut from an epoxy block with the embedded
PE05 film at room temperature using an ultramicrotome (Ultracut-1,
UK) with a diamond knife. HREM images were obtained with a JEOL
2010 microscope at an acceleration voltage of 200 kV.
The LOI measurements were carried out in accordance with ASTM
D2862. The specimens used for the test are of dimensions 100 
6.5  3 mm3.
The tensile tests were performed on a Universal Testing Machine
(WD-5D, Changchun, China) with a crosshead speed of 50 mm/min
according to ISO 527. Five specimens were taken to estimate the pre-
cision of the reported data.
The cone calorimeter experiments were evaluated following the
procedure defined in ISO 5660, on the 3 mm thick 100  100 mm2
plaques. The cone data obtained are reproducible to within 10% when
measured at 35 kW/m2 heat flux.
The thermogravimetric analyses (TGA) were conducted with a
Netzsch STA 409C thermoanalyzer instrument. In each case, about
10 mg specimens were heated from 258C to 7008C using a linear heating
rate of 108C/min under air flow.
The differential scanning calorimety (DSC) measurements were
performed with a Perkin–Elmer Diamond DSC differential scanning
calorimeter, using nitrogen as a purge gas. About 5–10 mg samples were
crimp-sealed in aluminum pans. The samples were first heated at
108C/min to 1808C and maintained at the temperature for 5 min, then
cooled at 108C/min to room temperature.

RESULTS AND DISCUSSION

Morphology Study

Figure 1 shows the XRD patterns of OMT and PE05 (VTMS-

crosslinked LLDPE/MH/OMT). The average basal spacing (d001) of
OMT is 2.2 nm. Figure 1 shows the average basal spacing of PE05 shifts
from 2.2 to 4.0 nm, the gallery height increases by 1.8 nm compared to
OMT. This indicates that the polymer molecular chains intercalate and
expand the gallery of OMT. An intercalated morphology, namely, a
multilayer structure consisting of alternating polymer molecular chains
stacked with the layers of the silicate layers is created in polymer matrix.
This intercalated morphology is further confirmed by HREM (Figure 2).

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Preparation of Silane-crosslinked Nanocomposites 497

Arbitrary intensity

PE05

OMT
2 4 6 8 10

2θ (degree)

Figure 1. XRD patterns of OMT- and VTMS-crosslinked LLDPE/MH/OMT nano-

composite (PE05).

Figure 2. HREM images of VTMS-crosslinked LLDPE/MH/OMT nanocomposite

(PE05).

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498 L. SONG ET AL.

The dark lines in the HREM image correspond to the OMT layers.
Figure 2 shows an intercalated morphology wherein distance between
adjacent layers was about 4 nm. So the results of XRD and HREM
confirm that the VTMS-crosslinked LLDPE/MH/OMT intercalated
nanocomposite was prepared.

Determination of Gel Content

The weighed samples of small pieces in a copper net were put into
boiling xylene for 12 h. The extracted samples were washed using
acetone and then dried to a constant weight. The gel content is
expressed as the percentage of the remaining sample weight to total
polymer weight in the sample before extracted. For MH- and OMT-
contained samples, the percentage of the MH and OMT have to be
deducted from the remaining sample. The gel contents of crosslinked
samples PE02, PE04, and PE05 are 30.5, 19.6, and 18.1%, respectively.
This indicates that the grafting and crosslinking reactions have occurred
and the addition of MH and OMT dramatically decreases the gel
content, namely, the crosslinking degree. The possible reason is
hypothesized: (1) During the grafting process, the siloxane
groups (Si(OCH3)) of a part of VTMS-grafted LLDPE interact with
the hydroxyl groups on the surface of MH and at the edge of OMT layers
to form hydrogen bonds which restrict the movement of VTMS grafted
LLDPE; (2) During the crosslinking process, macroscale MH and
nanoscale OMT layers restrict the VTMS grafted LLDPE macromole-
cular chains to move and touch via barrier effect and hydrogen bonds;
the hot water induces the hydrolyzation of the siloxane groups
(Si(OCH3)) of VTMS to silanol groups (Si(OH)), a part of silanol
groups interact with the hydroxyl group on the surface of MH and at the
edge of OMT layers to form siloxane bonds with surface of MH and OMT
through condensation [15]. So, a part of VTMS-grafted LLDPE
molecular chains are covalently bonded with the MH and OMT.
In summary, MH and OMT not only decrease the crosslinking degree
via consumption of some siloxane groups and barrier effect, but also
impair the regularity of the crosslinking network structure via barrier
effect and hydrogen bonds. These negative effects on the crosslinking
reaction, namely crosslink-inhibiting effect, results in the decreasing
gel content of PE04 and PE05. The gel content of PE05 is lower than
that of PE04. It is obviously indicated that the crosslink-inhibiting effect
of OMT is stronger than that of MH. The reason probably is that
the dispersion of nano-size layers of OMT is much better than that of
the micro-size particles of MH.

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Preparation of Silane-crosslinked Nanocomposites 499

Thermal-oxidation Stability

Figure 3 shows the TGA curves and the thermal-oxidative degradation

temperatures corresponding to a mass loss of 10% (T10%) and 50%
(T50%), which are listed in Table 2. It is indicated that the thermal
stability in terms of T10% for crosslinked LLDPE (PE02) is improved to
about 13.58C compared to PE01, whereas the improvement is only about
58C in the MH flame-retardant systems, the reason being the crosslink-
inhibiting effect of MH. For the nanocomposite PE05 in which MH was
partially replaced by OMT exhibits only slight higher of T10% than

1.0

0.8

0.6
Weight (%)

PE04
PE05
0.4

0.2 PE03

PE02

0.0 PE01

100 200 300 400 500 600 700

Temperature (°C)
Figure 3. TGA curves of the samples.

Table 2. TGA data of all the samples.

Sample code T10% (8C) T50% (8C) Residue (%)

PE01 404.2 463.5 0.01

PE02 417.7 469.0 2.3
PE03 394.8 469.6 28.5
PE04 402.3 474.6 33.2
PE05 403.5 471.0 30.5

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500 L. SONG ET AL.

that of PE04. Whereas T50% and the amount of residue of PE05 are
lower than that of PE04. It is contrary to our expectation, since the
presence of OMT is helpful to enhance the thermal stability of polymers,
the combination of OMT and metallic hydroxide has been reported to
have a synergistic effect and is often used as flame retardants for
polymers [16]. In this study, this depression may be due to the following
reasons: the crosslink-inhibiting effect of OMT decreases the cross-
linking degree of crosslinked polymer and impair the regularity of the
crosslinking network structure, and this effect is stronger than that of
MH; the 3D crosslinking network structure prevents the OMT layers
from migrating to the surface of molten polymer matrix via chemical
bonds and hydrogen bonds, although the literature reported that the
water vapor is favorable to the migration of OMT layers through the
molten matrix to accumulate on the substrate and this accumulation
is favorable for the formation of the char residue [17].

Crystallization Behavior

Differential scanning calorimetry (DSC) is a conventional method to

study the crystallization process of polymers. From DSC exotherms,
some information can be obtained, including the onset crystallization
temperature (To), which is the temperature at the crossing point of the
tangents of the baseline and the high-temperature side of the exotherm;
the peak crystallization temperature (Tp) of the exotherm and the
enthalpy of crystallization (
Hc) which is proportional to the degree of
crystallinity.
Figure 4 shows the DSC exotherms of all the samples under
nonisothermal condition. It can be seen from Table 3 that both the
To and Tp of the PE02 shift to a lower temperature in comparison
with that of PE01 and the degree of crystallinity (proportional to
Hc)
of PE02 also decrease. This is because that crosslinked LLDPE forms 3D
network structure, which makes the macromolecule chains less flexible
and restricts the movement of the macromolecule chains, causing the
crystallization temperature and degree of crystallinity to decrease.
Generally, the addition of nucleating agents in polymers could result in
an increase of To and Tp, therefore To and Tp of PE03 (in comparison to
PE01) show some increase by reason for the heterogeneous nucleation
effect of MH. Theoretically, crosslinked sample PE04 should get lower
To and Tp than PE03. In fact, both the To and Tp of PE04 shift to higher
temperature in comparison with PE03. The crosslink-inhibiting effect of
MH which decreases the crosslinking degree of crosslinked LLDPE and
impairs the regularity of crosslinking network structure is favorable of

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Preparation of Silane-crosslinked Nanocomposites 501

PE05
PE04

PE03

PE02

PE01
Endo

60 80 100 120 140

Temp (°C)

Figure 4. DSC exotherms of the samples.

Table 3. The onset crystallization temperature,

peak crystallization temperature and enthalpy
of crystallization of all samples.

Sample code To(8C) Tp(8C)
Hc(J/g)

PE01 112.33 110.24 91.2129

PE02 112.01 108.82 80.8898
PE03 114.03 110.98 42.4283
PE04 114.93 111.46 43.6754
PE05 114.63 111.42 45.0666

increasing the crystallization temperature and the crystallinity of

crosslinked LLDPE. Moreover, during grafting process, MH particles
are grafted by some VTMS-grafted LLDPE macromolecular chains via
hydrogen bonds that is favorable of increasing dispersion of MH in the
LLDPE matrix. Along with the dispersion of MH increasing, the
heterogeneous nucleation effect of MH also increases. This is also
favorable of increasing the crystallization temperature and the crystal-
linity of crosslinked LLDPE. For nanocomposite PE05, it shows no

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502 L. SONG ET AL.

obvious change in To and Tp, but the crystallinity content becomes

higher compared to PE04. This indicates that the heterogeneous
nucleation effect of OMT layers is stronger than that of MH.
Probably, the reason is also that the dispersion of nano-size layers of
OMT is much better than that of the micro-size particles of MH.

Mechanical Properties

The effect of the additives on the mechanical properties of crosslinked

LLDPE composites is shown in Table 1. It can be seen that PE02 shows
25.1% higher tensile strength (TS) and 15.7% lower elongation at break
(EB) in comparison with that of PE01. When incorporated with MH,
PE03 shows dramatic decrease in TS and EB. After crosslinking the
sample, PE04 shows only 14.5% increase of TS and 60.2% decrease of EB
compared to PE03. For the nanocomposite, TS exhibits almost the same
mechanical properties as PE04, but EB further decreases. This result
indicates that crosslinking is a useful method to enhance TS of LLDPE,
whereas the increase is impaired by the incorporation of MH and OMT.
The nanocomposite does not exhibit enhanced effect of mechanical
properties on crosslinked LLDPE.

Flammability Properties

The heat release rate (HRR), in particular peak HRR (PHRR)

measured by cone calorimeter has been found to be the most useful
parameter to evaluate fire safety and the cone calorimetry is one of the
most effective bench-scale methods for studying the flammability
properties of materials. The comparison of the HRR behavior of all
samples is presented in Figure 5. It shows that the PHRR value of PE02
is reduced by about 25% compared to PE01, this reduction may be
resulted from the crosslinking network structure which is helpful to
promote char formation and the deposition of SiO2 generated from the
oxidative degradation of VTMS, which forms a thin efficient barrier on
the substrate to oxygen permeation [18]. For the excellent flame
retardancy of MH, the PHRR of PE03 is 68% lower than PE01; however,
PHRR value of PE04 is only reduced by about 3.5% when compared to
PE03. Moreover, it is noticed that nanocomposite PE05 shows slight
increase in PHRR compared to PE04.
The CO concentration values from cone calorimeter are presented in
Figure 6 and corresponding results are listed in Table 4. When compared
to PE01, PE02 shows a significant reduction in peak CO concentration,
whereas PE03 and PE04 present no obvious change; moreover,

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Preparation of Silane-crosslinked Nanocomposites 503

800

PE01
PE02
600 PE03
PE04
PE05
HRR (kW/m2)

400

200

0
0 200 400 600 800 1000 1200
Time (s)

Figure 5. Heat release rate curves of the samples.

PE05 shows little increase, this trend is in consistent with HRR values.
On the other hand, another important parameter total heat release
(THR) of all samples is also listed in Table 4. Figure 6 shows that
the trend of THR is in according with the results of PHRR and CO too.
Table 4 shows that the limiting oxygen index (LOI) of samples increase
after silane crosslinking. But the LOI of nanocomposite is similar to
PE04. This indicates the incorporation of OMT is not helpful to improve
the LOI values.
In summary, the silane crosslinking can increase the flame retar-
dation of MH-filled LLDPE which may be due to the increase of the
thermal stability of the crosslinked LLDPE matrix. The incorporation of
the flame retardant MH can improve the flame retardation of the
silane-crosslinked LLDPE. But the crosslink-inhibiting effect of MH and
OMT weakens the positive fire safety effect caused by crosslinking
process. Incorporation of OMT is not helpful in improving the flame
retardance of MH-filled silane-crosslinked LLDPE and even decreasing
its flame retardance. The reason probably is that the crosslinking
network structure prevents the OMT layer from migrating to the
burning polymer surface and also prevents the flame-retardant effect
from taking place, which includes barrier effect and enhancement of
char formation [19,20].

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504 L. SONG ET AL.

0.0040

0.0035

0.0030

0.0025
CO

0.0020

0.0015

0.0010

0.0005

0.0000
PE01 PE02 PE03 PE04 PE05
Sample

100

80
THR

60

40

20

0
PE01 PE02 PE03 PE04 PE05
Sample

Figure 6. CO and total heat release graphs of the samples.

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Preparation of Silane-crosslinked Nanocomposites 505

Table 4. LOI and cone calorimeter data of all

the samples.

Sample LOI Peak HRR Peak THR

code (vol%) (kW m2) CO (%) (MJ/m2)

PE01 17 728.874 0.00383 107.182

PE02 18 546.423 0.00232 102.827
PE03 29.5 204.569 0.00061 37.366
PE04 32 197.327 0.00064 39.895
PE05 32.4 237.586 0.00085 46.392

CONCLUSIONS

The VTMS-crosslinked LLDPE, the MH-filled VTMS-crosslinked

LLDPE, and the MH-filled VTMS-crosslinked LLDPE/OMT nanocom-
posite have been prepared. Crosslinking process improves the fire safety,
thermal-oxidative stability, and mechanical properties of LLDPE, but
the crosslink-inhibiting effect of MH and OMT weakens this positive
effect. And the MH-filled VTMS-crosslinked LLDPE/OMT nanocompo-
site even shows a low fire safety and thermal-oxidative stability
compared to the MH-filled crosslinked LLDPE composite. Except for
the crosslink-inhibiting effect of OMT, the migration of OMT layers is
impeded by the crosslinking network structure of LLDPE matrix which
impair the barrier effect of OMT layers.

ACKNOWLEDGMENT

The work was financially supported by the National Natural Science

Foundation of China (No.50476026), Specialized Research Fund for
the Doctoral Program of Higher Education (20040358056), Program for
New Century Excellent Talents in University, and National 11th
Five-year Program (2006BAK01B03, 2006BAK06B06, 2006BAK06B07).

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BIOGRAPHY

Lei Song

Lei Song is an assistant professor of State Key Laboratory of Fire

Science in University of Science and Technology of China. He was
supervised by Professor Yuan Hu and Professor Zuyao Chen at State
Key Laboratory of Fire Science in University of Science and Technology
of China and received his PhD in inorganic chemistry in 2002. Since
1999 he has been working in areas of flame retardant polymer/clay
nanocomposites.

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