Reactive and Functional Polymers 138 (2019) 114–121

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Reactive and Functional Polymers

journal homepage: www.elsevier.com/locate/react

A novel composite silicone foam with enhanced safeguarding performance T

and self-healing property
⁎
Xiaofan Zhao, Junhua Zhang
The State Key Laboratory of Polymer Materials Engineering, Polymer Research Institute of Sichuan University, Chengdu 610065, China

A R T I C LE I N FO A B S T R A C T

Keywords: A novel hybrid silicone foam was successfully prepared by mixing shear stiffening gel (STG) with poly-
Silicone foam methylvinylsiloxane (MVQ) using expandable microsphere as a blowing agent. Storage modulus of STG/MVQ
Shear stiffening gel composite foam increased from 0.045 MPa to 0.38 MPa, when the shear frequency shifted from 0.1 Hz to 100 Hz,
Self-healing presenting a remarkable shear stiffening characteristic. The tensile result demonstrated that the elongation at
Anti-impact
break of the hybrid foam was as high as 814%. Besides, the hybrid foam gained excellent self-healing perfor-
Safeguarding
mance due to the cold-flow feature and viscous state of STG. More importantly, the drop hammer test indicated
the safeguarding performance enhanced as the STG contents increased, with the residual peak force decreasing
from 36.72 KN to 31.50 KN. In addition, a possible mechanism was proposed that it was the dynamic “BeO
bonds” that played a significant role in shear stiffening.

1. Introduction
Silicone rubber, as a typical kind of elastomer, has been widely
applied in various fields due to its excellent properties including non-
toxicity, biocompatibility, oxidation resistance and stable mechanical
performance in a wide range of temperature [1–5]. Silicone rubber
foam, endowed with the advantages of silicone rubber and foam, ex-
hibits favorable thermal insulation [6,7], light-weight performance,
superb flexibility [8] and excellent energy absorption property [9,10].
Silicone vulcanization preparation can be briefly classified into two
categories: high temperature vulcanization (HTV) and room tempera-
ture vulcanization (RTV). A peroxide-vulcanizing agent is usually used
for HTV during the curing process. In RTV system, crosslinking agents
containing functional groups on silicon atoms will react with silicone
polymers containing hydrosilanes in the presence of metal catalysts
[11]. Generally speaking, chemical and physical foaming are two
major methods to prepare silicone foam. However, there are many
drawbacks about chemical foaming. On one hand, it's difficult to
achieve uniform cell structure and obtain foams with cell size less than
50 μm. It has been reported that an ethylene propylene diene
monomer/silicone rubber foam was prepared by using azodicarbona-
mide (AC) as a chemical blowing agent. The foam possessed an average
cell size about 120 μm, with a low cell density (~4.20 × 104 cells/cm3)
and non-uniform bubble size [12]. On the other hand, the decomposed
chemical blowing agent leaves residues in products and some residues
may generate an unpleasant smell [13]. These drawbacks restrain the
application of chemical foaming to a large extent. Under these cir-
cumstances, physical foaming seems to become a better choice. Su-
percritical CO2 foaming technology has drawn much attention in recent
years. The average cell size can be controlled around 10 μm with a cell
density up to a magnitude of 1010 [14].
Herein, a physical blowing agent expandable microsphere was
adopted to fabricate the silicone foam. These microspheres contain two
parts, which have a low-boiling volatile hydrocarbon core wrapped by a
thermoplastic shell. Once heated, the liquid core starts to evaporate,
meanwhile, the thermoplastic shell swells [15]. The whole micro-
sphere can expand up to a hundred times than its pristine volume if the
foaming temperature is well controlled [16]. Thus, it has been applied
to foam various polymer composites owing to its unique structure. L.
Wang et al. investigated the compressive properties of epoxy foam
using expandable microspheres as a blowing agent. By optimizing the
foaming temperature and the precuring extent, epoxy foams with
homogeneous cells and stable compressive property could be obtained
[17]. Y. Xu et al. reported a light-weight and high-performance EMI-
shielding epoxy composite foam via impregnating epoxy/MWCNT/mi-
crosphere blends into a 3D silver coated melamine foam as conductive
framework [18]. However, to the best of our knowledge, there are few
reports about the fabrication and property of silicone foam using ex-
pandable microsphere as blowing agent. The crosslinking rate of the
rubber melt should be synchronous with the foaming rate of expandable

⁎
Corresponding author.
E-mail address: zhangjh@scu.edu.cn (J. Zhang).

https://doi.org/10.1016/j.reactfunctpolym.2019.03.004
Received 14 December 2018; Received in revised form 28 February 2019; Accepted 3 March 2019
Available online 05 March 2019
1381-5148/ © 2019 Elsevier B.V. All rights reserved.
X. Zhao and J. Zhang
microspheres [19]. If the HTV silicone rubber sheet is not crosslinked
or slightly crosslinked, it can't sustain the cells due to the weak matrix.
The cells will easily collapse and the foam's mechanical strength would
be quite low. But if the silicone rubber sheet has high degree of cross-
linking, it will be difficult for microspheres to expand [20]. The
matching of these two processes is crucial to obtain rubber foams with
excellent properties [21].
Shear stiffening gel (STG), first known as Silly Putty, is a type of
smart material whose mechanical properties enhance tremendously
with the increase of shear frequency, exhibiting a typical shear stif-
fening characteristic [22–24]. Under general conditions, STG exhibits
a soft and viscous state with reversible deformation. Once applying
high-rate external stimulation, STG will become stiff with its elastic
modulus increasing sharply. After the external loading is removed, STG
returns back to the initial viscous state. Due to its unique rate-depen-
dent feature, it has been applied in damping, piezoresistive sensor [25]
as well as impact resistance [26]. Recently, S. Wang et al. reported a
novel versatile electrical skin (e-skin) with safeguarding and multi-
sensing properties based on a hybrid structure by assembling Ag na-
nowires (AgNWs), polyester (PET) film into shear stiffening polymer/
polydimethylsiloxane(SST/PDMS) matrix [27]. Y. Wang et al. studied
the dynamic behavior of magnetically responsive shear-stiffening gel
under high strain rate [28]. It was found that the elastic modulus of the
MSTG increased with increasing strain rate and magnetic field. X.
Gong's group used a “dip and dry” method to penetrate STG into PU
sponge and developed a high performance anti-impact material [29].
However, this method is solvent-consuming and can't guarantee that
STG is homogenously dispersed in the PUS matrix, which may affect its
energy absorption ability. Due to that STG has the same SieO backbone
with silicone rubber, these two polymers could share a good compat-
ibility via direct physical mixing. In our work, we used the silicone
foam as matrix instead of PUS to fabricate a novel safeguarding foam
with quite good self-healing property. The closed cells formed by ex-
pandable microsphere and the rubber scaffold endow silicone foam
with excellent energy dissipation performance.
2. Experimental
2.1. Materials
Silicone rubber (Polymethylvinylsiloxane, MVQ, 110-2S) with a
molecular weight of 450,000–700,000 g/mol and 0.13–0.2% vinyl
group was purchased from Dongjue Silicone Group Co. Ltd., Nanjing,
China. Fumed silica with an average particle size of 40 nm was pur-
chased from Aladdin Co. Ltd., Shanghai, China. Boric acid used to
prepare shear stiffening gel (STG), as well as the curing agent benzoyl
peroxide (BPO) were all provided by Chengdu Kelong Factory of
Chemical Engineering Reagent. The expandable microsphere F-36D
(Expancel Matsumoto, Japan, particle size D = 10–20 μm) was used as
received. The hydroxyl silicone oil containing around 5% hydroxyl was
supplied by Jipeng Silicone Fluoride Materials Co. Ltd., Shenzhen,
China.
2.2. Preparation of shear stiffening gel (STG)
Certain amount of hydroxyl silicone oil was continuously stirred in a
beaker above 100 °C for preheating. Then the crosslinking agent boric
acid was successively added and the mixture kept reacting for several
hours. The schematic of preparing STG is shown in Scheme 1 [23].
2.3. Preparation of STG/MVQ composite foam
Methyl vinyl silicone rubber (MVQ), fumed silica, and hydroxyl si-
licone oil were masticated in a two-roll mill (Labtech, America) for
20 min until fumed silica was homogenously distributed in the rubber
matrix. Then the expandable microsphere, shear stiffening gel STG and
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Reactive and Functional Polymers 138 (2019) 114–121
curing agent BPO were gradually fed into the mill for further 15 min
compounding. The rubber composite was stored at room temperature
for 24 h to release the remaining stress of polymer chains after the
mixing process [30,31]. Afterwards, the rubber sheet was cast into a
mould (15 cm × 10 cm × 9 cm) and precured under 5 MPa at 120 °C for
30 min by a plate vulcanizing press. The sheet was 3 mm thick by
controlling the nip gap of the two-roll mill. Finally, the foam was
postcured at 160 °C for additional 3 h in the oven. When the mass ratio
of STG to the obtained hybrid STG/MVQ foam was W, the specimen was
named as STG-W (e.g. STG-40 means the mass ratio of STG: STG/MVQ
composite is 40: 100).
2.4. Characterization
Foam morphology was observed by scanning electron microscopy
(FEI Company, America). The samples were sprayed by gold layer after
brittle fracture using liquid nitrogen. The average cell size (D) of the
foamed sample was calculated by averaging the sizes of at least 100
cells, which was estimated by Eq. (1):
∑ di ni
D=
∑ ni (1)
where ni is the number of cells with an area-equivalent diameter of di
[32].
Rheological properties of silicone foam with various contents of
shear stiffening gel were recorded by a HAAKE RARS III rheometer. The
shear frequency swept from 0.1 to 100 Hz and the strain amplitude was
kept 1%. Tensile and compressive properties were both measured by
Instron 5567 testing machine according to ISO 3386-2-1997 and ISO
1798-2008 at room temperature. The above two experiments were re-
peated at least five times to reduce the random error.
In addition, a drop hammer test instrument was applied to in-
vestigate the safeguarding performance of the composite silicone foam
samples. During the process, the drop hammer weighed 5 kg fell from
different heights to strike the sample with different impact energy.
Then the sensor at the bottom captured the residual force and trans-
ferred into electric signals. Thus the signals went through the signal-
amplifier and were eventually recorded as residual peak force.
3. Results and discussion
3.1. Effects of the STG contents on cell morphology
Fig. 1 shows the SEM micrographs of STG/MVQ composite foam
and the corresponding cell size distribution with various STG contents.
It was found that all the samples shared an independent closed cell
structure and the average cell size was 68 μm, 65 μm, 56 μm, 58 μm and
54 μm respectively in Fig. 1(a), (b), (c), (d), (e). Overall, The cell size
distribution of foams with STG became narrower compared to the
pristine sample. Cell size reached up to 160 μm for STG-0, whereas the
maximum cell diameter for STG-20, STG-30 and STG-40 was about
120 μm. More importantly, the addition of STG seemed to make it easier
for silicone foams to obtain better cell morphology, especially for STG-
30 and STG-40. We could observe that the sample without STG ex-
hibited a relatively large non-uniformed bubble shape. What's worse,
some bubbles swelled too much when foaming, even collapsed and
coalesced. At this case, the cell wall was not sturdy enough that the
microspheres expanded excessively and squeezed each other, which led
to the irregular oval bubble shape. However, compared with pure sili-
cone foams, the well-dispersed STG polymer acted as a barrier to curb
gas diffusion when foaming. Once heated, the curing speed of rubber
matrix may not catch up with microspheres swelling. At this time, the
introduced STG polymer tended to hinder the over-growth and coa-
lescence of bubbles, leading to regular cell morphology with thick cell
walls. Above all, the results suggested that STG contents played an
X. Zhao and J. Zhang
Scheme 1. Preparation of STG polymer.
important role in building enhanced cell walls and well-organized cell
morphology.
3.2. Viscoelastic properties of STG/MVQ hybrid silicone foam
Rheological tests were carried out to investigate the frequency-de-
pendent mechanical properties of STG/MVQ samples. The storage
modulus G' (also known as elastic modulus), is a measurement of the
elasticity of the material, which also indicates the stiffness of the ma-
terial [33]. From Fig. 2(a), we can see that the initial storage modulus
G' of the pure STG at 0.1 Hz was 4.3 KPa and it increased significantly as
the external shear frequency increased. Once the shear frequency came
around 1 Hz, G' rose slowly and the maximum G'max was as high as
0.4 MPa (100 Hz). The tanδ value of pure STG (Fig. 2(c)), which is the
ratio of G" to G', was above 1 when stimulated by stress at low fre-
quency, exhibiting a typical soft viscous state. Whereas it came below 1
at high shear frequency, presenting a remarkable shear stiffening fea-
ture. However, the storage modulus (G') and loss modulus (G") (seen
Fig. 2(b)) of MVQ foams without STG seemed to exhibit no obvious
fluctuation in the whole frequency range, indicating that the rheolo-
gical properties of pure silicone foam were quite independent of ex-
ternal stimuli. When having introduced STG into MVQ foam matrix, the
storage modulus of the hybrid foam enhanced compared with the initial
MVQ foam at high frequency. As the increasing of shear frequency, G′ of
the hybrid foam strengthened steadily, exhibiting rate-dependent
rheological properties, which could be ascribed to the addition of STG.
This shear stiffening phenomenon was more obvious for composite
STG-40, which means STG-40 sample performed better than STG-20.
The loss modulus of samples mixed with STG shifted first, then reached
to peak and finally subsided with the increasing of shear frequency.
Furthermore, G" of STG/MVQ hybrid was more enhanced than that of
MVQ foam matrix in the same shear frequency, presenting an im-
provement in energy dissipation [29]. Based on the above analysis, it
was concluded that the STG/MVQ hybrid silicone foam exhibited ty-
pical shear stiffening characteristics as shear rates increased, which can
act as a novel flexible safeguarding material. Moreover, Fig. 2(d) pre-
sents the complex viscosity value under various shear frequency. It is
interesting to observe that η* of pure STG exhibited a platform at low
shear frequency and then decreased as the frequency shifted. In the
contrast, the η* of the three foam samples kept declining during the
whole frequency range.
3.3. Effects of STG contents on mechanical properties
3.3.1. Compressive properties of STG/MVQ hybrid silicone foam
The compressive stress-strain curves of silicone foams with various
STG contents are shown in Fig. 3(a) and the compression modulus was
calculated from the initial slope of the strain-stress curves [34]. These
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Reactive and Functional Polymers 138 (2019) 114–121
compressive strain-stress processes could be divided into linear elasti-
city stage, platform stage and compact stage, and these three regions
were explained by the Gibson-Ashby theory [35]. All the samples ex-
hibited typical compressive behavior of foams and the stress increased
monotonously as the strain increased. The corresponding Young's
modulus and compressive stress at 60% strain of samples against the
STG content were plotted in Fig. 3(b). The sample without STG pre-
sented the highest Young's modulus of 4.21 MPa, while the other
samples were 3.87 MPa, 3.97 MPa, 3.83 MPa and 3.84 MPa respec-
tively. Simultaneously, the stress at 60% strain declined as the increase
of STG contents. According to foam theory, the mechanical behavior of
cellular materials is not only determined by sample density but also
influenced by microstructure characteristics [36]. Although the addi-
tion of STG endowed the silicone foam with better cell distribution and
thicker walls, which could enhance the foam mechanical properties
remarkably. However, the viscous and cold-flow feature of STG wea-
kened the mechanical performance of the rubber matrix under the
compressive low loading rate. Overall, it was figured out that the sili-
cone foam without STG exhibited better compressive performance than
those with STG.
3.3.2. Tensile properties of STG/MVQ hybrid silicone foam
The typical stress–strain curves obtained from tensile test are dis-
played in Fig. 4(a) and the related tensile property values are shown in
Fig. 4(b) as well. All the samples stretched slowly as the train raised and
finally fractured in the middle position. As shown, the tensile stress and
modulus declined with the increasing of STG contents, which was ba-
sically consistent with the compressive modulus change. It was sur-
prising to notice that all the foams could be stretched to more than
400% of their original length, particularly for STG-40 sample whose
elongation at break was as high as 814%. This elongation enhancement
is probably related to the high flexibility of molecular chains in STG,
which has a great compatibility with rubber matrix. The tensile loading
rate was 50 mm/min, slow enough for the segments to relax and dis-
entangle. Therefore, the foam could be stretched extensively without
fracture. On the other hand, the increasing amounts of STG were closely
associated with well-organized cell distribution and fewer foam defects,
which also contributed to a large elongation at break.
3.4. Self-healing performance
The obtained composite foam could be bent and twisted into dif-
ferent shapes without any fracture. As shown in Fig. 5(b) and (c), the
STG polymer collapsed apparently after 1 h, exhibiting irreversible cold
flow feature. While the hybrid foam stood still and maintained its shape
with no deformation. After compounding, the silicone foam acted as a
supporting skeleton and STG polymer were well dispersed in the matrix
due to their similar molecular chains. Thus, the creep behavior of STG
X. Zhao and J. Zhang Reactive and Functional Polymers 138 (2019) 114–121

Fig. 1. Effects of STG contents on the cell morphology and distribution: (a) STG-0, (b) STG-10, (c) STG-20, (d) STG-30, and (e) STG-40.

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X. Zhao and J. Zhang Reactive and Functional Polymers 138 (2019) 114–121

Fig. 2. Storage modulus (G′) (a), loss modulus (G″) (b), loss tangent (tanδ) (c) and complex viscosity (η*) (d) of STG/MVQ hybrid foams under stimulation of different
shear rates.

could be conquered by this method. The self-healing process of STG/
MVQ foam is depicted in Fig. 5(e)-(f). The STG-40 sample was cut into 4
pieces separately and after pressing for a while, the broken pieces ad-
hered with each other. The sample after self-healing could withstand its
own weight without falling apart. However, the sample without STG
addition could not stick together at all. This specific self-healing per-
formance resulted from the cold-flow feature and viscous state of STG at
room temperature [37]. To better calculate its self-healing perfor-
mance, the tensile stress-strain curves of healed samples are presented
in Fig. 5(g). It shows that the more STG was mixed, the better adhesion
the sample exhibited. All the samples fractured in the self-healing po-
sition. STG-40 presented better adhesion ability than the others, with an
elongation at break of 34%. Meanwhile, its tensile stress at break was
around 0.05 MPa, which means its mechanical strength recovered
about 11.1% after healing compared to the pristine STG-40 foam, with
tensile stress at break of 0.45 MPa.
3.5. Drop hammer test
For better understanding the procedure of drop hammer test, the
schematic of the device is displayed in Fig. 6. The peak force refers to
the maximum residual force directly measured by the pressure sensor
placed beneath the sample after being impacted. Under the same im-
pact condition, the smaller the peak force is, the better the safeguarding
performance of the material is. As shown in Fig. 7(a), the peak force
declined steadily with the increasing STG contents, from 36.72 KN to
31.50 KN. In other words, the material performed better impact re-
sistance with more STG addition. It is also seen in Fig. 7(b) that the

Fig. 3. (a) Compressive stress-strain curve of STG/MVQ composite foams; (b) Young's modulus and stress at 60% strain with various STG contents.

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X. Zhao and J. Zhang Reactive and Functional Polymers 138 (2019) 114–121

Fig. 4. (a) Tensile stress-strain curve of STG/MVQ composite foams; (b) Young's modulus and elongation at break with various STG contents.

residual peak force curve of STG-40 was always lower than that of STG-
0, further demonstrating the STG-40 sample obtained better anti-impact
performance than that of pure silicone foam. Furthermore, when the
impact energy was low, the difference between the two curves was
quite negligible, and the protective performance of STG-40 was slightly
better compared to pure silicone foam. When subjected to larger impact
energy, the gap between the two curves shifted gradually, which in-
dicated the foam with STG presented more excellent safeguarding
performance under high-rate stimuli. This result was exactly in ac-
cordance with that of rheological test, showing the rate-dependent ef-
fect of STG inside the polymer composite. Based on the above data, we
could prove that the compounding of STG helped silicone foam possess
enhanced safeguarding performance.

3.6. Mechanisms of shear stiffening properties of STG/MVQ silicone foam

In general, the shear stiffening phenomenon of STG is greatly at-

tributed to its high strain-rate dependent property. Under heating, the
hydroxyl group of boric acid reacted with that in hydroxyl silicone oil
to form boron–oxygen (BeO) bonds. The soft and flexible silicon-
oxygen (SieO) bonds formed the backbone of STG and the B atoms
acted as crosslinking points. As mentioned by M. Goertz, the electron-
deficient p orbital of B atom could obtain electrons from O atom in the
SieO structure, forming dynamic “BeO bonds”, which is similar to
hydrogen bond [38]. When shear stress is loaded under low rate, the
molecular chains have enough time to relax, disentangle and the tran-
sient BeO bonds are easily devastated. Under this circumstance, the
Fig. 6. Schematic of the drop hammer test device.
polymer is viscous and can be molded into various shapes. However,
under high-rate mechanical stress, the “BeO bonds” could not keep up
with the changes of external stimuli, due to that the relaxation time of
the “BeO bonds” is much longer than the frequency [39]. As shown in
Fig. 8, a great number of dynamic “BeO bonds” can't have enough time
to break. Instead, they are regarded as locked and hinder the slippage of

Fig. 5. (a) STG/MVQ hybrid foam under twist; (b) pristine STG polymer(left) and STG/MVQ hybrid foam(right); (c) samples 1 h after; (d)-(f) the self-healing process
of STG-40; (g) tensile stress-strain curves of self-healed composite foams.

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X. Zhao and J. Zhang
Fig. 7. Results of drop hammer test: (a) the effects of STG contents on residual peak force under 50 J impact energy; (b) peak force values under different impact
energy for sample STG-0 and STG-40.
Fig. 8. Mechanism diagram of shear stiffening performance in STG/MVQ composite foam under high strain rate.
polymer chains in short time. Thus the polymer exhibits stiff char-
acteristic with its storage modulus increasing tremendously. During the
whole loading and unloading period, STG could absorb a lot of energy
through the fraction and disentanglement of the high weight molecular
chains [40]. Hence, it is considered to be a very promising material in
body armor.
4. Conclusions
In this work, a novel STG/MVQ hybrid foam with favorable safe-
guarding performance was successfully fabricated using expandable
microsphere as a blowing agent. The SEM results indicated that STG
endowed the foam with enhanced cell walls and well-organized cell
morphology. The rheological tests suggested the storage modulus of
STG/MVQ hybrid foam increased with the increasing of shear fre-
quency, owing to the rate-dependent effect of STG. Although samples
mixed with STG possessed poorer elastic modulus, it exhibited superior
elongation at break in tensile tests. Besides, the hybrid foam gained
excellent self-healing performance due to the cold-flow feature and
viscous state of STG. More importantly, the drop hammer test demon-
strated the safeguarding performance enhanced with the increase of
STG contents. It presented better protecting capability under high-rate
stimuli, which was consistent with the results of rheological test. A
possible mechanism was proposed to explain the shear stiffening effects
of STG. It was the dynamic “BeO bonds” that played a significant role
in shear stiffening and impact resistance. Overall, the prepared STG/
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Reactive and Functional Polymers 138 (2019) 114–121
MVQ composite foam possessed a promising future in the application of
anti-impact and energy dissipation.
Funding information
The work was supported by Lengine Defense Technology Group Co.,
Ltd.
Data availability
The raw/processed data required to reproduce these findings cannot
be shared at this time as the data also forms part of an ongoing study.
Acknowledgements
The authors want to thank Ms. Luyao Yan for determining anti-
impact test.
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