Thermal and Mechanical Properties of Silane- Grafted

Water Crosslinked Polyethylene

Hsu-Chiang Kuan,1 Jenn-Fong Kuan,1,2 Chen-Chi M. Ma,1 Jaine-Ming Huang3

1
Department of Chemical Engineering, National Tsing Hua University, 300, Hsin-Chu, Taiwan
2
R&D Department, Plastics Industry Development Center, 407 Tai-chung, Taiwan
3
Department of Chemical Engineering, Hsiuping Institute of Technology, 412 Tai-Chung, Taiwan

Received 8 March 2004; accepted 4 October 2004

DOI 10.1002/app.21694
Published online in Wiley InterScience (www.interscience.wiley.com).

ABSTRACT: The effects of linear low density polyeth- ethylenes were able to crosslink utilizing water as the
ylene (LLDPE) grafting with vinyltrimethoxysilane by dif- crosslinking agent. The effects of varied crosslinking time
ferent types and contents of peroxide were studied. When on the mechanical properties of the crosslinked polyeth-
grafting silane onto LLDPE, with 0.10 phr of Dicumyl ylenes were studied. It was found that the HDPE and
peroxide (DCP) or 0.05 phr content of 2,5-Dimethyl-2,5-di LLDPE were apt to crosslink during the grafting process
(tert-butyl-peroxy)-hexane (DHBP), it was found that the and thus decreased the grafting ratio. Multiple melting
grafting effect was improved; however, as Di(2-tert-bu- behavior was observed for crosslinked LDPE and LLDPE.
tylperoxypropyl -(2))-benzene (DIPP) or excess DHBP Mechanical and thermal properties of the crosslinked PE
was used, LLDPE was supposed to cause self-crosslink- are much better than that of uncrosslinked PE. © 2005
ing, which reduced the grafting effect of silane and was Wiley Periodicals, Inc. J Appl Polym Sci 96: 2383–2391, 2005
invalid in the processing of extrusion. In this study,
vinyl trimethoxysilane (VTMS) was grafted onto various
polyethylenes (HDPE, LLDPE, and LDPE) using DCP as Key words: water-crosslinking; peroxide; polyethylene; me-
an initiator in a twin screw extruder. The grafted poly- chanical property

INTRODUCTION Crosslinked PE is superior to uncrosslinked PE in

many aspects, such as excellent electrical properties,
Scott et al first proposed water crosslinking of PE in
good abrasion resistance, and improved heat per-
1972.1 The advantages of this process are energy sav-
formance and chemical resistance. It is widely used
ing, low cost, and higher productivity. Crosslinked
in the applications of primary wire and cable insu-
polyethylene possesses better physical properties than
general polyethylene, and also has become widely lation, tubes and pipes, and cable jackets. There are
adapted for a number of industrial applications. Cur- three methods for preparing crosslinked PE indus-
rently, there are three main approaches to crosslink trially: crosslinking with radiation, crosslinking
polyethylene: (1) using high-energy radiation (gamma with peroxide, and crosslinking with water.5– 8
or UV) or electrons, (2) utilizing a thermochemical Crosslinking with radiation is only suitable for thin
method (e.g., heating in the presence of peroxides), wall parts and is limited by its high-energy cost and
and (3) using water to crosslink certain polyethylene safety. Peroxide induced crosslinking has to be op-
that has been “grafted” with reactive groups.2– 4 erated at high vacuum, and it is difficult to control
the thickness of the products. Crosslinking with
water is achieved by grafting with silane, followed
Correspondence to: C.-C. M. Ma (ccma@che.nthu.edu.tw).
by hydrolysis to Si-OHgroups and subsequently
Journal of Applied Polymer Science, Vol. 96, 2383–2391 (2005) condensation to form Si-O-Si bonds.9 –15 The mech-
© 2005 Wiley Periodicals, Inc. anism is believed to be as follows8,16:
2384 KUAN ET AL.

(1)

(2)

(3)

(4)

(5)

(6)

The grafting of vinyltrimethoxysilane onto the poly- 1. (a) Linear Low Density Polyethylene (LLDPE):
ethylene polymer chain is becoming more popular due No. LL120 with a melt index of 2.0, produced
to the low investment cost and high production rate of by Taiwan Polymer Corporation, Taiwan. (b)
such a process. This process is through free radical ini- High density polyethylene (HDPE) : No.
tiators and can subsequently condense through water, LH901, with a melt index of 0.95, and (c) Low
leading to the formation of crosslinking. density polyethylene (LDPE) : No. F2201 with a
The first part of the present work is to investigate the melt index of 2.0, were purchased from Asia
effects of silane grafting onto LLDPE. Three types of Polymer Corporation.
peroxide (DCP, DHBP, and DIPP) and various peroxide 2. Vinyltrimethoxysilane (VTMS), No. Q9-6300,
contents are added. In these systems, the self-crosslink- was supplied by Dow Corning Co., USA.
ing reaction competed with the water-crosslinking reac-
3. Dicumyl Peroxide (DCP), No. PEROXIMON DC,
tion. In the second part, vinyl trimethoxysilane (VTMS)
was produced by ELF ATOCHOEM, France.
was grafted onto various polyethylenes (HDPE, LLDPE,
4. 2,5-Dimethyl-2,5-di(tert-butyl-peroxy)-hexane
and LDPE), and the effects of varied crosslinking time on
(DHBP), No. LUPEROX 101, was produced by
the mechanical properties of the crosslinked polyethyl-
ene are discussed. ELF ATOCHOEM, France.
5. Di(2-tert-butylperoxypropyl-(2))-benzene
EXPERIMENTAL (DIPP), No. PEROXIMON F40, was produced by
ELF ATOCHOEM, France.
Material 6. Di-n-butyltin dilaurate (DBTDL), No. T12, was
The materials used were: supplied by AIR PRODUCTS, USA.
SILANE-GRAFTED WATER-CROSSLINKED POLYETHYLENE 2385

TABLE I isothermal water bath at 85°C for 4 h to proceed to the

Recipes for Sample Preparation in This Study water-crosslinking reaction.
Peroxide type* Various PE pellets (HDPE, LDPE, and LDPE)
Sample LLDPE DCP DHBP DIPP Silane were premixed with silane and DCP and then fed to
code (parts) (phr) (phr) (phr) (phr) a twin screw extruder with barrel temperature rang-
ing from 110 to 180°C. The amounts of DCP and
A 100 0.05 — — —
silane were 0.1 phr and 1 phr, respectively. The
B 100 — 0.05 — —
C 100 — — 0.05 — compounded pellets were injection molded to stan-
D 100 0.1 — — — dard testing specimens. Some of the specimens were
E 100 — 0.1 — — subsequently subjected to water-crosslinking with
E 100 — 0.1 — — different crosslinking time.
G 100 0.05 — — 1.50
H 100 — 0.05 — 1.50
I 100 — — 0.05 1.50
J 100 0.1 — — 1.50 Properties tests
K 100 — 0.1 — 1.50
L 100 — — 0.1 1.50 Processability measurement was tested using a rhe-
* Chemical Structure of Peroxides: ometer (PLASTI-CORDER PL 2000, Brabender Co.)
to observe the chemical reaction and process ability
1. Dicumyl Peroxide (DCP)
of the polymer melt, and the rotor speed was 50rpm.
The mechanical properties of dumbbell shaped
specimens were measured on an Instron Model 4468
machine. Tensile test procedures followed the
ASTM D638-82 method with a crosshead speed of 20
2. 2,5-Dimethyl-2,5-di(tert-butyl-peroxy)-hexane(DHBP)
mm/min. The dimensions of the samples were 25.0
⫻ 10.0 ⫻ 1.4 mm (length ⫻ width ⫻ thickness). Six
specimens were tested in each case. Flexural tests
followed the ASTM D790 method with a span-to-
depth ratio of 40 and crosshead speed of 1.0 mm/
min. Notched impact strength was tested according
to ASTM D256, and a TMI Testing Machine (TMI
3. Di(2-tert-butylperoxypropyl-(2))-benzene(DIPP)
Co. U.S.A.) was used (the dimensions of these sam-
ples were 63.0 ⫻ 12.7 ⫻ 3.2 mm (length ⫻ width
⫻ thickness)). All tests were performed at ambient
temperature of 25 ⫾ 2°C. The differential scanning
calorimeter (DSC) analysis of the samples was car-
ried out under aN2 atmosphere with a Perkin–Elmer
DSC Pyris 1. These amorphous samples were then
7. Anti-oxidant agent, No. 1010, was produced by heated again to 100°C at a heating rate of 10°C/min.
Ciba Geigy Corp., Switzerland. Heat deflection temperature (HDT) was measured
by a TOYOSEIKI S-6M HDT tester, and followed the
ASTM D648 method. The loading pressure was 4.6
Sample preparation kgf/cm2, and the heating rate was 120°C/h.
Sample preparation was conducted according to the
recipes listed in Table I (three types of peroxide and
various peroxide contents). Samples were com- RESULTS AND DISCUSSION
pounded by single screw extruders. Processing tem-
peratures were selected from 140°C to 160°C (samples Effects of peroxide concentration on moisture-
crosslinking of LLDPE
A–F). The silane grafting reaction was performed at a
fixed silane content (1.50 phr part per hundred parts of Figure 1a shows that with LLDPE with 0.05 phr DCP
resin) and the grafted master batches were prepared and with silane (curves A–G), the torque value ap-
(samples G–L). The master batches with catalyst were proaches that of pristine LLDPE, it represents that the
prepared from LLDPE and DBTDL catalysts and anti- effect of self-crosslinking and silane grafting on LLDPE
oxidant agents (for the samples with silane treatment, is insignificant. However, when 0.1 phr DCP is added
and the content is 5 phr). All testing specimens were (curve D), the torque value increased slightly. If the
injection molded following the ASTM method. The silane content increases, torque value increased obvi-
specimens with silane treatment were placed in an ously (curve J), showing that free radicals are released by
2386 KUAN ET AL.

Figure 1 The Brabender Plot (the relationships between Torque Value and Reaction Time, t) of silane-grafted water-
crosslinked LLDPE with (a) different DCP contents, (b) different DHBP contents, and (c) different DIPP contents.

peroxide and induce the slight self-crosslinking. Conse- increases slightly (curve B), and it increases more if
quently, silane grafting reacts with LLDPE. silane is added (curve H), indicating that 0.05 phr
The peroxide used in Figure 1b is DHBP. When 0.05 DHBP content can induce slight self-crosslinking and
phr DHBP is added into LLDPE, the torque value silane was grafted to LLDPE. When 0.10 phr DHBP is

TABLE II
Tensile Strength of Silane-Grafted Water-Crosslinked LLDPE When Three Types and Various
Contents Peroxides Are Added
Tensile strength Increased
Peroxide Silane after water- percentage after
content content Tensile strength crosslinking water-crosslinking
Sample codes (phr) (phr) (Kgf/cm2) 4hr(Kgf/cm2) (%)

LLDPE — — 148.4 — —
A DCP 0.05 — 161.8 — —
G DCP 0.05 1.5 160.4 166.8 4.0
B DHBP 0.05 — 164.0 — —
H DHBP 0.05 1.5 180.8 198.5 9.8
C DIPP 0.05 — 162.0 — —
I DIPP 0.05 1.5 168.3 173.8 3.3
D DCP 1.0 — 166.0 — —
J DCP 1.0 1.5 164.1 193.2 17.7
E DHBP1.0 — 170.4 — —
K DHBP 1.0 1.5 198.0 204.8 3.4
F DIPP1.0 — 183.0 — —
L DIPP 1.0 1.5 189.7 192.6 1.5
SILANE-GRAFTED WATER-CROSSLINKED POLYETHYLENE 2387

TABLE III
Tensile Elongation of Silane-Grafted Water- Crosslinked LLDPE When Three Types and Various
Contents Peroxides Are Added
Increased
Peroxide Silane Elongation after percentage after
content content Elongation water-crosslinking water-crosslinking
Sample codes (phr) (phr) (%) 4hr(%) (%)

LLDPE — — 448.8 — —
A DCP 0.05 — 407.9 — —
G DCP 0.05 1.5 108.3 107.3 ⫺0.9
B DHBP 0.05 — 262.3 — —
H DHBP 0.05 1.5 82.9 74.5 ⫺10.1
C DIPP 0.05 — 367.5 — —
I DIPP 0.05 1.5 106.3 101.5 ⫺4.5
D DCP1.0 — 122.9 — —
J DCP1.0 1.5 105.5 63.0 ⫺40.2
E DHBP1.0 — 109.5 — —
K DHBP1.0 1.5 79.2 74.9 ⫺5.4
F DIPP1.0 — 106.7 — —
L DIPP1.0 1.5 88.1 86.6 ⫺5.1

TABLE IV
Flexural Strength of Silane-Grafted Water-Crosslinked LLDPE When Three Types and Various
Contents Peroxides Are Added
Flexural strength Increased
Peroxide Silane Flexural after water- percentage after
content content strength crosslinking 4hr water-crosslinking
Sample code (phr) (phr) (Kgf/cm2) (Kgf/cm2) (%)

LLDPE — — 109.7 — —
A DCP 0.05 — 111.5 — —
G DCP 0.05 1.5 118.7 125.9 6.1
B DHBP 0.05 — 112.8 — —
H DHBP 0.05 1.5 119.9 131.8 9.9
C DIPP 0.05 — 110.5 — —
I DIPP 0.05 1.5 121.4 126.5 4.2
D DCP1.0 — 115.9 — —
J DCP 1.0 1.5 120.5 135.3 10.9
E DHBP 1.0 — 121.8 — —
K DHBP 1.0 1.5 130.3 134.7 3.4
F DIPP1.0 — 121.9 — —
L DIPP 1.0 1.5 130.4 132.2 1.4

TABLE V
Impact Strength of Silane-Grafted Water-Crosslinked LLDPE When Three Types and Various
Contents Peroxides Are Added
Impact strength Increased
Peroxide Silane Impact after water- percentage after
content content strength crosslinking water-crosslinking
Sample code (phr) (phr) (J/M) 4hr(J/M) (%)

LLDPE — — 433.3 — —
A DCP 0.05 — 447.1 — —
G DCP 0.05 1.5 453.2 484.0 6.8
B DHBP 0.05 — 456.7 — —
H DHBP 0.05 1.5 463.5 533.0 15.0
C DIPP 0.05 — 446.4 — —
I DIPP 0.05 1.5 472.7 507.2 7.3
D DCP 1.0 — 454.3 — —
J DCP1.0 1.5 461.5 541.5 17.3
E DHBP 1.0 — 481.8 — —
K DHBP 1.0 1.5 490.6 523.0 6.6
F DIPP 1.0 — 482.9 — —
L DIPP1.0 1.5 503.3 522.5 3.8
2388 KUAN ET AL.

TABLE VI
The Characteristics of Pure HDPE and Silane-Grafted Water Crosslinked With Varying Crosslinking Time
Time of exposure HDPE-g-VTMS
Test item HDPE 0 hr 0.5 hr 1 hr 3 hr 6 hr

Tensile strength (Kgf/cm2) 247.9 326.3 344.4 346.1 346.3 348.0

Elongation (%) 239.7 48.4 46.9 39.2 35.9 35.1
Flexural strength (Kgf/cm2) 310.2 357.1 382.0 382.7 391.0 391.7
Flexural modulus (Kgf/cm2) 9240 9512 10170 10613 10893 10975
Notched Izod impact strength (J/M) 783.2 404.8 388.3 371.5 364.3 310.8
HDT (°C) 78.1 84.1 96.1 97.3 100.7 101.2

added, the torque value is higher than that of pristine bender plot are increased (Figs. 1a and b), which is
LLDPE (curve E). The self-crosslinking reaction of LL- caused by the self-crosslinking reaction of LLDPE, not
DPE occurs significantly when 0.10 phr DHBP is from the silane grafting reaction. The effective degree
added, and the processability was deducted. When of grafting in the same time was reduced.
silane is added, the torque value increases even higher From Table III, the tensile elongation of LLDPE is
(curve K). The effects of the DIPP series of peroxide on 448%. When three types of 0.05 phr peroxides are
processability are shown in Figure 1c. These results added (samples A, B, and C), the tensile elongations
are similar to that of DHBP peroxide. When 0.10 phr are still acceptable (260 – 400%), indicating the degree
DIPP is added to the system (curve L), the torque of crosslinking is small as 0.05 phr peroxide content is
value is higher than that of DHBP peroxide (curve K), added. When silane is added, the tensile elongation
indicating that the silane grafting effect of DIPP per- decreases obviously (samples G, H, and I), represent-
oxide on LLDPE is higher than that of DHBP peroxide; ing that peroxide can promote the self-crosslinking
however, its processability becomes worse. reaction of LLDPE. The tensile elongation of sample J
From the changes of mechanical properties, one decreases 40% after water-crosslinking, caused by the
may realize the effect of peroxide on the self-crosslink- effect of silane grafting and the water-crosslinking
ing reaction of LLDPE and the effective degree of reaction of LLDPE.
silane grafting. From Table II, one can find the tensile Table IV summarizes the results of flexural
strength of neat LLDPE is 148.8 kgf/cm2. Tensile strength testing. Table V summarizes the results of
strength increases as peroxides and silane are added, impact strength. The trends are similar to the results
especially when DHBP and DIPP peroxide content are of tensile property. From these mechanical proper-
more than 0.1 phr (samples E, K, F, and L). But the ties tests, it can be concluded that the better degree
tensile strength only increases 3.4% after water- of water-crosslinking can be achieved with 0.10 phr
crosslinking for 4 h. From these results, one can find DCP content than with 0.05phr DCP content (sam-
that the torque values of curves K and L in a Bra- ples J and G). LLDPE utilizing 0.1 phr DHBP pos-
sesses a higher degree of water-crosslinking than

Figure 3 Effect of various water-crosslinking time on heat

Figure 2 Effect of various water-crosslinking time on ten- deflection temperature of pristine and silane-grafted poly-
sile strength of pristine and silane-grafted polyolefin. olefin.
SILANE-GRAFTED WATER-CROSSLINKED POLYETHYLENE 2389

TABLE VII
The Characteristics of Pure LLDPE and Silane-Grafted Water Crosslinked With Varying Crosslinking Time
Time of exposure LLDPE-g-VTMS
Test item LLDPE 0 hr 0.5 hr 1 hr 3 hr 6 hr

Tensile strength (Kgf/cm2) 140.0 162.2 163.8 164.1 165.0 167.8

Elongation (%) 403.5 57.5 57.2 56.3 55.7 54.9
Flexural strength (Kgf/cm2) 104.3 132.3 134.8 135.2 135.6 137.1
Flexural modulus (Kgf/cm2) 2367 2513 2514 2588 2594 2632
Notched Izod impact strength (J/M) 453.0 553.5 544.3 533.8 532.5 522.6
HDT (°C) 57.7 58.1 58.7 59.1 59.6 60.2

that of 0.01 phr DHBP content (samples H and K). is a polymer with a high degree of crystallinity, and its
Results show that LLDPE possesses a higher degree physical properties are deeply affected by the degree
of silane grafting when peroxide contents are 0.10 of crystallinity. As can be seen from Table 6, the im-
phr DCP and 0.05 phr DHBP. The using of DIPP pact strength of the silane grafted water crosslinked
peroxide obtains a less degree of water-crosslinking HDPE was decreased, which was probably caused by
when the peroxide content is the same, and the the decreasing of the degree of crystallinity of HDPE.
processability is also worse. The HDT of the crosslinked HDPE is increased with
increasing crosslinking time. After being crosslinked
for 6 h, the HDT can be increased from 78.1°C to
Thermal and mechanical properties of silane-
grafted moisture-crosslinked polyethylene 101.2°C (greater than that of LDPE and LLDPE, as
shown in Fig. 3).
Table VI shows the characteristics of pristine HDPE
and silane grafted water crosslinked with varying
crosslinking time. It is found that the tensile strength
of the silane grafted HDPE increases 31.6%, compared
to pristine HDPE (increasing percentage is greater
than LLDPE and LDPE, as shown in Fig. 2). After
water-crosslinking for 4 h at 85°C, the tensile strength
increased only 5.5 to 6.7%, compared to the silane
grafted HDPE. This implies that the increase of the
tensile strength of the silane grafted HDPE is due to
the crosslinking of HDPE during the grafting process.
The elongation of the crosslinked HDPE is decreased
because the crystallinity of HDPE is destroyed. HDPE

Figure 5 Differential thermal analysis traces for LLDPE

and crosslinked LLDPE.

Figure 4 Effect of various water-crosslinking time on flex- Figure 6 Differential thermal analysis traces for HDPE and
ural strength of pristine and silane-grafted polyolefin. crosslinked HDPE.
2390 KUAN ET AL.

TABLE VIII
The Characteristics of Pure LDPE and Silane-Grafted Water Crosslinked With Varying Crosslinking Time
Time of exposure LDPE-g-VTMS
Test item LDPE 0 hr 0.5 hr 1 hr 3 hr 6 hr

Tensile strength (Kgf/cm2) 133.8 135.6 138.8 139.5 141.6 143.4

Elongation (%) 119.5 114.8 110.6 107.9 101.9 100.6
Flexural strength (Kgf/cm2) 92.5 111.3 114.6 115.9 119.8 120.2
Flexural modulus (Kgf/cm2) 1589 1988 1912 1947 2044 2105
Notched Izod impact strength (J/M) 523.3 511.9 505.5 470.5 483.8 445.0
HDT (°C) 54.1 55.8 60.2 61.5 62.8 63.1

Table VII lists the mechanical properties of pure VIII. Contrary to silane grafted HDPE and LLDPE, the
LLDPE and silane grafted water crosslinked LLDPE tensile strength and elongation of the silane grafted
subjected to different curing times. The tensile LDPE are not affected, implying that the crosslinking
strength, flexural strength, and impact strength are all of LDPE is not favored during the silane grafting
increased (the percentage of increasing of flexural process. The nature of the long chain branch of LDPE
strength is greater than that of HDPE and LDPE, as is responsible for the more effective silane grafting.
shown in Fig. 4), while the elongation is decreased. Upon crosslinking, the tensile strength, flexural
From these data it is also found that crosslinking of strength, and flexural modulus were increased with
LLDPE during silane grafting shows more significant increasing crosslinking time (percentage of increasing
effects on the increase of mechanical properties than of flexural modulus is greater than that of HDPE and
that of water induced crosslinking. Unlike HDPE, the LLDPE, as shown in Fig. 7). The reasons causing the
impact strength of crosslinked LLDPE is increased increase of these properties resemble those of LDPE.
with increasing crosslinking time. The reason could be Multiple melting behaviors were observed for
due to the crystallinity of LLDPE, which is much crosslinked LDPE, as well in Figure 8.
lower than that of HDPE, and therefore upon
crosslinking, the degree of crystallinity was not de-
creased as drastically as HDPE. In addition, from the CONCLUSIONS
DSC data in Figure 5, multiple melting behaviors were
observed for the cross-linked LLDPE (it cannot be seen
1. Suitable peroxide and the optimal peroxide con-
in the system of HDPE, as shown in Fig. 6). It is the
tent can enhance effective silane grafting on LL-
result of the phase separation of the two different
DPE, and the mechanical properties can be in-
crystallines, the PE crystalline and the newly formed
creased after water- crosslinking.
Si-O-Si crystalline.
2. Silane can prompt the peroxide to proceed to the
The mechanical properties of pure LDPE and silane
self-crosslinking reaction of LLDPE.
grafted water crosslinked LDPE are presented in Table
3. The effective silane grafting on LLDPE decreases
when the self-crosslinking reaction of LLDPE oc-
curs, and the processability might be reduced.

Figure 7 Effect of various water-crosslinking time on flex- Figure 8 Differential thermal analysis traces for LDPE and
ural modulus of pristine and silane-grafted polyolefin. crosslinked LDPE.
SILANE-GRAFTED WATER-CROSSLINKED POLYETHYLENE 2391

4. During the silane grafting process using DCP References

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