Influence of Polyhedral Oligomeric Silsesquioxanes (POSS)on Thermal and Mechanical Properties of Polydimethylsiloxane(PDMS) Composites Filled with Fumed Silica

Dongzhi Chen • Yan Liu • Hongwei Zhang •

Yingshan Zhou • Chi Huang • Chuanxi Xiong

Received: 22 June 2013 / Accepted: 25 August 2013 / Published online: 4 September 2013

� Springer Science+Business Media New York 2013

Abstract A series of novel PDMS composites filled with

a given amount of fumed silica were first prepared using

divinyl-hexa[(trimethoxysilyl)ethyl]-POSS as cross-linker

by hydrolytic condensation in the presence of organotin

catalyst. The crosslinking reaction, the morphology, ther-

mal behaviors and mechanical properties of the novel

PDMS composites were characterized by attenuated total

reflection infrared spectroscopy, scanning electron micro-

scope, thermogravimetric analysis and universal tensile

testing machine, respectively. It was found that the resis-

tances to thermal degradation, thermo-oxidative decom-

position of the novel PDMS composites were greatly

improved by incorporation of POSS cross-linker, compared

with that of the reference material (MT-1). Meanwhile, we

also found that their thermal properties and mechanical

properties were gradually enhanced with the further

increment in loading amount of POSS cross-linker. The

pronounced enhancements in thermal properties and

mechanical properties of novel PDMS composites were

likely attributed to the increasing interaction of PDMS

chains and aggregated particles from synergistic effect

between POSS and fumed silica.

Keywords PDMS composites � POSS � Fumed

silica � Thermal properties � Mechanical properties

1 Introduction

Till now, PDMS polymer has been intensively studied for

their unique properties, such as excellent thermal stability,

low glass transition temperature, good electrical properties,

good weather resistance, low surface free energy, low

toxicity and low chemical reactivity [1–15]. The chemical

inertness of PDMS makes it useful in a variety of appli-

cations in automotive fields, microelectronic areas, aero-

space and construction industries [10, 15]. A large number

of commercial PDMS products, such as sealants, adhe-

sives, membrane and elastomers have been found in

everywhere. In these products, silica has been broadly used

as reinforcing agent to improve mechanical properties of

PDMS matrix due to its inherent weak intermolecular

force. But filled PDMS composites usually show a weak

thermal stability due to silanol groups from surface of

silica, which is unable to meet the practical requirements of

special fields.

An alternative approach is to modify fumed silica with

silane coupling agent, this method can improve thermal

stabilities of PDMS composites, but it is sacrificing their

mechanical properties. To overcome this defect, consider-

able efforts have been undertaken to further improve their

properties. A promising approach is to incorporate POSS

into the PDMS matrix [13, 14, 16–22]. POSS as a new

class of lightweight and high performance hybrid materials

can impart excellent comprehensive properties of com-

posites [23–38], such as mechanical properties, thermal

properties, flammability resistance and so on.

D. Chen (&) � H. Zhang � Y. Zhou � C. Xiong

School of Materials Science and Engineering, Wuhan Textile

University, Wuhan 430200, People’s Republic of China

e-mail: chdozh_2008@163.com

Y. Liu

Wuxue High School, Wuxue 435400, People’s Republic of

China

C. Huang

College of Chemistry and Molecular Sciences, Wuhan

University, Wuhan 430072, People’s Republic of China

123

J Inorg Organomet Polym (2013) 23:1375–1382

DOI 10.1007/s10904-013-9939-1

However, the previous reports mostly focus on

mechanical properties of PDMS composites. Moreover,

these PDMS composites are relatively simple systems

consisting of PDMS polymer and POSS, which are not

involved in hybrid systems, namely, fumed silica and

POSS. In our recent work, we firstly found synergistic

effect between POSS and fumed silica on thermal and

mechanical properties of PDMS composites, and mainly

investigated the influence of fumed silica on thermal and

mechanical properties of PDMS composites filled with a

given amount of POSS cross-linker [39], but relative

research on effect of POSS on thermal and mechanical

properties of PDMS composites filled with a given amount

of fumed silica is very rare. Therefore, in this work, POSS

was attempted to introduce into the system consisting of

PDMS polymer and fumed silica by chemical cross-link,

and a series of novel PDMS composites with POSS and

fumed silica were prepared, and the effect of POSS on the

thermal properties and mechanical properties of PDMS

composites filled with a given amount of fumed silica was

mainly investigated.

2 Experimental

2.1 Materials

The cross-linker divinyl-hexa[(trimethoxysilyl)ethyl]-

POSS (DVPS) was prepared according to previous litera-

tures [20, 21], and its ideal structure was shown in Fig. 1.

The Cabot-O-Sil fumed silica (LM-150) obtained from

Cabot Corporation (USA), which was used after drying at

120 �C for 24 h. Methyltrimethoxysilane (MTMOS) was

supplied by Wuhan University Silicone New Material Co.,

Ltd. Hydroxyl-terminated polydimethylsiloxane (HPDMS)

(viscosity, 5,000 cSt, 49,000 g/mol), methyl silicone oil

(viscosity, 500 cSt, 19,000 g/mol) and curing catalyst

(mixture of dibutyltin diacetate and stannous 2-ethyl hex-

anoate) were provided by Hubei Wuhan University Pho-

tons Technology Co., Ltd. Ethyl ether was purchased from

Tianjin BoDi Chemical Reagent Co., Ltd, which was used

after dehydration according to classic literature procedure.

2.2 Preparation of PDMS Composites

HPDMS polymer was charged into the kneading chamber

of the kneader (IKA HKD-T0, 6), and kneaded to move

volatile components at 130 �C for 2 h under vacuum. A

given amount of fumed silica was added into the kneading

chamber when the HPDMS polymer was cooled to RT

under vacuum. The mixture was continued to knead at RT

under vacuum until it became light blue (for about 15 min),

and then 1 g/mL ethyl ether solution of DVPS and curing

catalyst was added into the kneading chamber, and the new

mixture was obtained after kneading for 15 min, then

volatile components were removed under vacuum for

around 15 min. This new mixture was rapidly transferred

into a packing rubber tube, and then this packing rubber

tube was sealed with a piston. Subsequently, the mixture

could be squeezed out by caulking gun, and cured for about

2 days at room temperature to give a PDMS composite.

To make a good comparison, the reference PDMS

composite (MT-1) filled with a given amount of fumed

silica was also prepared using the commercial cross-linker

(MTMOS) according to the same approach. The curing

formulations for all PDMS composites were designed as

follows: HPDMS polymer, methyl silicone oil, cured cat-

alyst and fumed silica were 100, 10, 0.15 and 15, respec-

tively. Only the amount of POSS cross-linker relative to

amount of HPDMS used was changed. And the PDMS

composite formulations with various weight percent of

DVPS were listed in Table 1. According to calculation, the

relative number of reactive SiOCH3 groups per 100 g of

HPDMS in DVPS-1, DVPS-2, DVPS-3 and DVPS-4 is 6.6,

13.2, 19.8 and 26.4 mmol/g, respectively. However, the

reference material MT-1 has about 44.0 mmol of SiOCH3

groups per gram of HPDMS used. This means that MT-1

has the highest crosslinking density among the novel

PDMS composites after curing.

2.3 Characterizations of Samples

Fourier Transform infrared spectroscopy (FTIR) spectra of

the samples were measured using KBr pellet technique

with a Nicolet AVATAR 360FT infrared analyzer. Infrared

spectra of PDMS composites were obtained from a Nicolet

NEXUS 670 Spectrometer by attenuated total reflection

infrared spectroscopy (ATR-IR). Morphological analysis

was performed on an FEI Quanta 200 scanning electron

microscope (SEM) at a voltage of 30 kV. The cured sam-

ples were placed into liquid nitrogen for 5 min, and then

fractured into two pieces to create fresh surfaces. The fresh

cross-sections of samples were observed by scanning

electron microscope after they were coated with platinum.

Thermogravimetric analysis (TGA) was performed on

SETSYS-1750 (SETARAM Instruments). About 10 mg of

Si O Si

Si O SiSi O Si

OOO

Si O Si

OO O

O

O(H3CO)3Si

Si(OCH3)3

Si(OCH3)3

(H3CO)3Si

(H3CO)3Si

Si(OCH3)3

Fig. 1 The ideal structure of DVPS cross-linker

1376 J Inorg Organomet Polym (2013) 23:1375–1382

123

sample cut as small pieces was heated in an Al2O3 crucible

in air atmosphere from ambient temperature to 600 �C at a

heating rate of 10 �C/min, and in nitrogen atmosphere from

ambient temperature to 800 �C at a constant rise of tem-

perature (10 �C/min). Mechanical tensile tests were per-

formed on a universal testing machine (Instron 8871, UK,

capacity 25 kN) at 25 �C. The tensile strength, elongation

at break and modulus were measured according to ASTM

C1184-2000a, and an average of at least three effective

measurements for each sample was recorded. The shore A

Hardness is the relative hardness of elastic materials can be

determined with an instrument called a Shore A durometer

(LX-A) according to ASTM D1415-88 (1999).

3 Results and Discussion

3.1 FTIR Characterization of Novel PDMS

Composites

The FTIR spectra of the virgin polymer (HPDMS), fumed

silica and the representative sample DVPS-4 are provided

in Fig. 2. In Fig. 2a, b, a broad peak at 3,465 cm-1 and a

weak peak at 1,630 cm-1 are respectively assigned to

stretching and deformation vibration of the H-bonded sil-

anol (Si–OH) group from HPDMS and fumed silica.

Meanwhile, the sharp bands at 2,960 and 2,903 cm-1 for

asymmetric and symmetric C–H stretching vibrations of

Si–CH3, 1,411 and 1,260 cm-1 owing to asymmetric and

symmetric C–H deformation vibrations of Si-CH3 from the

HPDMS, are clearly observed respectively. However, after

HPDMS was cured, the H-bonded silanol groups from

HPDMS and fumed silica disappeared completely, as

shown in Fig. 2c. The hump peak at 1,604 cm-1 in the

magnified segment is assigned to C=C stretching vibration,

which is originated from the DVPS cross-linker. The dis-

appeared absorption band of the H-bonded silanol groups

from HPDMS and fumed silica indicated that most silanol

groups from HPDMS and fumed silica might be participate

in chemical bonding during cross-linking process. And the

peak for Si–O–Si asymmetric stretching vibration shifted

from around 1,108 cm-1 for HPDMS to 1,080 cm-1 for

the DVPS-4 sample and became broader, and the peak for

the Si–O–Si asymmetric deformation vibration also shifted

from about 1,025 cm-1 for HPDMS to 1,006 cm-1 for the

representative sample DVPS-4 and became somewhat

sharp, as shown in Fig. 2. These shifts in the absorption for

Si–O–Si vibrations provided an indication of the presence

of a strong interaction between PDMS chains and aggre-

gated particles due to chemical cross-link [10, 40]. The

similar shifting trends had also been reported in previous

literatures [40, 41].

3.2 Morphology of the Novel PDMS Composites: SEM

Study

For the distribution of POSS moieties in polymer matrices

have a great effect on both thermal and mechanical prop-

erties of resultant composite systems [42], it is necessary to

know the dispersions of DVPS cross-linker and fumed

silica in these PDMS composites. The representative SEM

image of the novel PDMS composites was provided in

Fig. 3. Many small spherical particles (bright parts) were

well dispersed, a few aggregated particles being of large

size and good adhesion between PDMS matrix (gray parts)

Table 1 The formulation and residual yields of the novel PDMS composites

Sample Relative weight ratio of

DVPS to HPDMS (wt%)

Theoretical mass

fraction of SiO2 (%)

Residual yield at 800 �C

(%) in nitrogen

Residual yield at

600 �C (%) in air

DVPS-1 5 12.88 21.48 48.64

DVPS -2 10 13.70 31.61 50.30

DVPS -3 15 14.47 43.72 52.52

DVPS -4 20 15.18 54.50 54.91

MT-1 20 10.33 14.36 45.16

Fig. 2 FTIR spectra of samples: a fumed silica, b HPDMS and c the

representative PDMS composite DVPS-4

J Inorg Organomet Polym (2013) 23:1375–1382 1377

123

and particles were also observed, as shown in Fig. 3. These

aggregated particles, including small particles and a few

aggregated particles, were likely the formations of POSS

and fumed silica ascribed to synergistically chemical cross-

link during the curing process. Between POSS cross-linker

and fumed silica, the silanol groups distributed on the

surface of fumed silica might easily adsorb POSS cross-

linker, and the crosslinking formations of POSS and fumed

silica were not difficult to produce during curing process.

3.3 Thermal Degradation of the Novel PDMS

Composites

The resistances to thermal degradation of the novel PDMS

composites were evaluated by TGA in nitrogen. The deg-

radative curves of these PDMS composites under nitrogen

were depicted in Fig. 4. We easily found that the charac-

teristic temperatures of the novel PDMS composites with a

given amount of fumed silica using DVPS as cross-linker

were higher than that of the reference sample (MT-1) when

they lost the same weight percent of their initial mass,

which indicated that adding POSS was good to improve the

resistance to thermal degradation of the novel PDMS

composites. And the important characteristic data of all

sample degradation were graphed in Fig. 5. For example,

the initial decomposition temperatures of 5 % weight loss

increased from 448.3 �C for DVPS-1 to 477.4 �C for

DVPS-4 with the increasing amount of the cross-linker

DVPS, which fluctuated around 458.9 �C for MT-1. It was

clearly seen that the characteristic temperatures of 10 %

weight loss of these novel filled PDMS composites

increased from 485.1 �C for DVPS-1 to 523.8 �C for

DVPS-4 with the content of loading POSS, which were far

higher than that of the reference PDMS composite

(475.8 �C for MT-1). When all of these PDMS composites

continued to lose 30 % weight of their initial mass, the

trend of their characteristic temperatures was similar to that

of 10 % weight loss. Meanwhile, the residual yields at

800 �C for these novel PDMS composites were represented

in Table 1. We clearly found that the residual yields were

improved from 21.48 % for DVPS-1 to 54.50 % for DVPS-

4 with the increasing amount of POSS, which were higher

than that of the reference material (14.36 % for MT-1).

From the discussion above, it was concluded that as com-

pared with the MT-1 reference material, adding DVPS

cross-linker was favorable to improve resistances to ther-

mal decomposition of PDMS composites filled with fumed

silica, and their resistances to thermal decomposition

gradually increased with the increment of the loading

amount of DVPS. These pronounced improvements in

resistances to thermal decomposition were likely attributed

to the uniform distributions of the increasing cross-linked

three-dimensional networks resulting from synergistic

effect between the increasing amount of POSS cross-linker

and a given amount of fumed silica.

After degradation, the black solid residues of DVPS

samples were obtained, which likely indicated charring

action of cross-linked networks at high temperature due to

vinyl groups from DVPS. In fact, three aspects should be

mainly taken into account for the improvement in resistance

to thermal decomposition of the novel PDMS composites.

On the one hand, the uniform distribution of the increasing

cross-linked three-dimensional networks resulting from

synergistic effect between the POSS cross-linker and fumed

silica can further increase the interaction between the PDMS

chains and the aggregated particles, which improve the

Fig. 3 The representative SEM image of the novel PDMS compos-

ites: DVPS-4

Fig. 4 TGA curves for the PDMS composites obtained in nitrogen

atmosphere

1378 J Inorg Organomet Polym (2013) 23:1375–1382

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resistances to thermal decomposition of the novel PDMS

composites [39]. On the other hand, the charring action

resulting from vinyl groups in cross-linked networks could

improve the resistances to thermal decomposition of the

novel PDMS composites [20, 21]. Meanwhile, a trace

amount of silanol groups from fumed silica might low the

resistances to thermal decomposition of the filled PDMS

composites. With the increase in loading amount of DVPS,

the amount of silanol groups might decrease, therefore, the

increasing cross-linked three-dimensional networks and the

charring action predominated in nitrogen atmosphere during

thermal degradation. As a result, the resistances to thermal

decomposition of the novel PDMS composites were greatly

improved.

3.4 Thermo-oxidative Behaviors of the Novel PDMS

Composites

The TGA curves for the thermal oxidative degradation of

these PDMS composites in air atmosphere were repre-

sented in Fig. 6. It was obviously found the resistances to

thermo-oxidative stabilities of these DVPS samples were

better than that of the MT-1 reference material, even

though the DVPS samples had lower initial decomposing

temperature as compared with the MT-1 reference sample.

The characteristic decomposition temperatures were

graphed in Fig. 7. For example, the initial characteristic

degraded temperatures of 5 % weight loss of the DVPS

samples decreased from 391.3 �C for DVPS-1 to 374.3 �C

for DVPS-4 with the increment of amount of POSS, which

were lower than that of reference sample MT-1 (392.4 �C).

In this case, the dropping trend of characteristic tempera-

tures was mainly ascribed to the oxygen catalysis. The

initial decomposing temperature of MT-1 was higher than

those of the others, which could be due to its high cross-

linking density. With loading amount of POSS increasing,

the vinyl groups content of the novel DVPS samples

increased, which likely accelerated the decomposition of

the novel PDMS composites by resultant radical in the

presence of oxygen catalysis at low temperature. With the

increase in loading amount of POSS, therefore, lower

characteristic decomposing temperatures were observed.

But, at high temperature, charring action of cross-linked

networks could become obvious, which also improved the

novel PDMS composites. And the characteristic tempera-

tures for 10 % weight loss of the DVPS sample increased

from 427.3 �C for DVPS-1 to 446.6 �C for DVPS-4, which

fluctuated around 438.6 �C for MT-1. Meanwhile, the

characteristic temperatures for 30 % weight loss of the

DVPS samples were delayed from 479.7 to 521.9 �C with

the loading amount of POSS, which were far higher than

467.6 �C for MT-1. Additionally, with the increment in

amount of POSS, the residual yields of these PDMS

composites obtained at 600 �C in air were improved from

48.64 % for DVPS-1 and 54.91 % for DVPS-4, which

higher than that of MT-1(45.16 %), as shown in Table 1.

According to theoretical calculation, POSS cage (Si8O12)

weight fractions of DVPS in DVPS-1, DVPS-2, DVPS-3

and DVPS-4 were 1.17 % (3.84 %* 30.5 %), 2.26, 3.26

and 4.20 %, respectively. If POSS cages in all of PDMS

composites were completely transformed into silica under

air without considering residue from PDMS, the total

residual yields of DVPS-1, DVPS-2, DVPS-3 and DVPS-4

should be 12.88, 13.70, 14.47 and 15.18 %, respectively,

which were far lower than the actual obtained, as shown in

Table 1. From the above data, high decomposing temper-

atures and high residual yields obtained in air suggested

that the thermo-oxidative properties of the novel PDMS

Fig. 5 The characteristic temperatures of the PDMS composites after

thermal degradation in N2 (the reference material MT-1 was defined

as zero point) Fig. 6 TGA curves for the PDMS composites obtained in air

atmosphere

J Inorg Organomet Polym (2013) 23:1375–1382 1379

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composites were gradually improved by adding an

increasing amount of POSS.

These pronounced improvements in thermo-oxidative

properties of the novel PDMS composites were likely

attributed to the competitive results of oxygen catalysis,

charring action and the uniform distributions of the

increasing cross-linked three-dimensional networks result-

ing from synergistic effect between the increasing amount

of POSS cross-linker and a given amount of fumed silica.

3.5 Mechanical Properties of the Novel PDMS

Composites

To investigate influence of POSS cross-linker on

mechanical properties of novel PDMS composites with a

given amount of fumed silica, the tensile properties of the

novel PDMS composites were evaluated by universal ten-

sile testing machine.

During the tensile testing, we found that the reference

material MT-1 had poor elongation at break (about

26.6 %), which was likely attributed to weak adhesion

between glass and aluminum sheets. Therefore, modulus at

40 % elongation of the reference material MT-1 couldn’t

be provided in the following discussion. The values of

tensile strength, elongation at break and modulus at 40 %

elongation were summarized in Table 2. The tensile

strength values of these novel PDMS composites increased

from 0.54 MPa for DVPS-1 to 0.84 MPa for DVPS-4 with

the increment of the loading amount of POSS, which were

higher than 0.58 MPa for reference material (MT-1) except

that of sample DVPS-1. Meanwhile, the modulus at 40 %

elongation of these novel PDMS composites was gradually

improved from 0.34 MPa for DVPS-1 to 0.51 MPa for

DVPS-4 with the increase in the loading amount of POSS,

which demonstrated a similar trend observed in their ten-

sile strength. The upturns in the tensile strength and

modulus at 40 % elongation of the novel PDMS compos-

ites indicated that adding the increasing amount of POSS

cross-linker was favorable to improve mechanical proper-

ties of PDMS matrix containing a given amount of fumed

silica. However, their values of elongations at break

decreased to 106.2 % for DVPS-4 from 212.0 % for

DVPS-1 with the increase in the loading amount of POSS,

which much higher than that of reference sample MT-1, as

listed in Table 2. And shore hardness of these PDMS

composites was also improved from 19 A for DVPS-1 to 34

A for DVPS-4 by adding an increasing amount of fumed

silica. As the loading amount of POSS increased, the above

reinforcing tensile strength, enhancing modulus, decreasing

elongations at break and ascending shore hardness dis-

played that POSS could be used as reinforcing filler in the

PDMS matrix containing fumed silica. The improvement in

mechanical properties of the novel PDMS composites was

likely due to synergistic effect between fumed silica and

POSS.

In fact, the improved mechanical properties of these

novel PDMS composites depend on the two opposing

factors: the increasing interaction between PDMS chains

and aggregated particles and decreasing uniform distribu-

tion of the cross-linked three dimensional networks. With

increase in the loading amount of POSS, the interaction

between PDMS chains and particulates increased, which

resulted in improvement in the modulus and the tensile

strength of the novel PDMS composites. When the cross-

linked three dimensional networks dispersed well, the

interaction between PDMS chains and aggregated particles

was strengthened, which also led to the enhancements of

Fig. 7 The characteristic temperatures of the PDMS composites after

thermo-oxidative decompositions in air (the reference material MT-1

was defined as zero point)

Table 2 Mechanical properties

of the novel PDMS compositesSample Tensile

strength (MPa)

Elongation

at break (%)

Modulus at 40 %

elongation (MPa)

Shore

hardness (A)

MT-1 0.58 26.6 – 20

DVPS-1 0.54 212.0 0.34 19

DVPS-2 0.63 168.3 0.37 23

DVPS-3 0.75 124.6 0.41 32

DVPS-4 0.84 106.2 0.51 34

1380 J Inorg Organomet Polym (2013) 23:1375–1382

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the modulus and the tensile strength of the novel PDMS

composites. Meanwhile, the number of the big-sized

aggregations in this system became more with increasing

amount of POSS, which likely led to an increase in bad

dispersions of the cross-linked three dimensional networks

and strong interaction between aggregated particles and

particles. Hence the interaction between PDMS chains and

aggregated particles was weakened relatively as compared

to the particles with good dispersion. And the distance

among the PDMS chains could be lengthened by the

H-bond from silanol groups on surface of big-sized parti-

cles, which resulted in a decrease in the value of the

elongation at break of the novel PDMS composites.

Meanwhile, the increasing crosslinking density of novel

PDMS composites with POSS loading could also lead to a

decrease in the value of the elongation at break of the novel

PDMS composites.

4 Conclusions

In this work, the novel PDMS composites with a given

amount of fumed silica were prepared using DVPS as cross-

linker. The increasing interaction between PDMS chains and

aggregated particles was found by FTIR, and the dispersion

of aggregated particles resulting from chemical cross-link of

POSS and fumed silica in these novel PDMS composites had

been observed by means of SEM. The resistances to thermal

degradation and thermo-oxidative decomposition of the

novel PDMS composites were evaluated both in nitrogen and

in air by means of TGA. It was found that the incorporation of

POSS into PDMS system filled a given amount of fumed

silica greatly improved the resistances to thermal degrada-

tion and thermo-oxidative decomposition of the novel

PDMS composites, and their resistances to thermal degra-

dation and thermo-oxidative decomposition gradually

increased with loadings of POSS cross-linker. The striking

improvements in thermal properties of novel PDMS com-

posites were likely attributable to the charring action and an

increasing interaction between PDMS chains and aggregated

particles from synergistic effect between POSS and fumed

silica. Meanwhile, it was also found that the mechanical

properties of novel PDMS composites with a given amount

of fumed silica were reinforced by incorporation of POSS.

The reinforcement in mechanical properties of novel PDMS

composites was likely ascribed to the increasing interaction

between PDMS chains and aggregated particles from syn-

ergistic effect between POSS and fumed silica.

Acknowledgments This research has received financial supports

from both the Foundation of Wuhan Textile University (No. 115027)

and the National Natural Science Foundation of China No. 51203123.

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