Ceramics International xxx (xxxx) xxx–xxx

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Effects of SiC content on mechanical, thermal and ablative properties of

carbon/phenolic composites
Shuang Wanga, Haiming Huanga,∗, Ye Tianb, Jie Huangc
a
Institute of Engineering Mechanics, Beijing Jiaotong University, Beijing, 100044, China
b
The 210th Institute of the China Aerospace Science and Industry Corporation Sixth Academy, Xi'an, 710065, China
c
School of Computer and Information Technology, Beijing Jiaotong University, Beijing, 100044, China

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

Keywords: Silicon carbide (SiC) particles were utilized to improve the mechanical, thermal and anti-ablative properties of
Composites carbon/phenolic (C/Ph) composites. SiC–C/Ph composites were fabricated with different weight percentage of
Thermal properties SiC by vacuum impregnation method. The mechanical and thermal properties were characterized by compres-
SiO2 sion tests, thermal conductivity tests, and thermogravimetric analysis; meanwhile, ablation resistance was in-
vestigated using plasma wind tunnel tests and scanning electron microscopy. Experimental results showed that
5 wt% SiC modified C/Ph composites owned the optimum properties. Moreover, introducing SiC particles could
result in an obvious decrease of compression strength, but an increase of thermal stability, thermal conductivity
and anti-ablative performance. Notably, the ablation rate reached its the lowest point at 5% the SiC content in
resin matrix composites.

1. Introduction (simulating temperature [14]), which are convenient for testing but
cannot simulate the external flight environment of the spacecraft like
Carbon/phenolic (C/Ph) composites are classical materials as wind tunnel tests (providing high enthalpy value, nitrogen and oxygen
thermal protection systems (TPS) owing to the extraordinary mechan- environment and plasma flow, etc. [15]). Meanwhile, the effects of SiC
ical and anti-ablative properties [1]. However, ablation resistance of C/ content on the properties of C/Ph materials are unclear. Therefore, it is
Ph composites needs to be further improved in order to meet the re- necessary to study the effect of SiC as a single filler on ablative prop-
quirement for a new generation of spacecraft operating in the external erties of C/Ph composites during plasma wind tunnel test, and the
environment with high speed and high heat flux [2,3]. optimal content of SiC to improve properties is worth exploring.
In recent years, many kinds of ceramic particles such as zirconium On this basis, C/Ph composites modifying SiC particles are fabri-
carbide, zirconium silicide, zirconium diboride, silicon carbide (SiC) cated by the vacuum-impregnation method, and effects of SiC content
and silica (SiO2) have been studied to improve anti-ablation perfor- in matrix on mechanical, thermal and ablative properties of C/Ph
mance of C/Ph composites [4–10]. Among them, SiC particles were composites are investigated; meanwhile, the mechanism of SiC oper-
generally used along with other ceramic particles. Subha et al. [7] in- ating during ablation is discussed in detail.
vestigated ablative properties of ZrO2/SiC modified C/Ph composites by
oxyacetylene flame test, and reported that zirconium carbide ceramic 2. Experimental
phase and SiO2 protected composites from ablation. Ghelich et al. [8]
proved that zirconium boride and SiC as fillers could form a dense 2.1. Materials
zirconia and SiO2 layer on the ablated surface of C/Ph composites, and
the layer as a protective barrier greatly decreased linear ablation rate. Boron modified phenolic resin THC-400 (Shaanxi Taihang
SiC can be oxidized at high temperatures and form both a liquid Impedefire Polymer Co., Ltd, China) was chosen as the matrix. Needled
phase oxide SiO2 and a volatile sub-oxide SiO, being dependent on the carbon fiber felt with a density of 0.145 g/cm3 (Tianniao High
environment and silicon content [11]. The frequently-used ablative Technology Co., Ltd, Jiangsu, China) served as the preform for C/Ph
tests are oxyacetylene test (mainly carbon dioxide and water, simu- composites. The polyacrylonitrile based carbon fibers (T700SC-12000-
lating heat flow and temperature [12,13]) and laser ablative test 50C, from Japan) were provided as the precursor of the materials. SiC

∗
Corresponding author.
E-mail address: huanghaiming@tsinghua.org.cn (H. Huang).

https://doi.org/10.1016/j.ceramint.2020.03.170
Received 11 March 2020; Received in revised form 17 March 2020; Accepted 17 March 2020
0272-8842/ © 2020 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Shuang Wang, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2020.03.170
S. Wang, et al. Ceramics International xxx (xxxx) xxx–xxx

particles (particle size distribution of 1–2 μm, purity > 99%) were Table 1
purchased from Tonghua Hongxin Abrasion Material Co., Ltd, Jilin, Density of C/Ph composites.
China. Samples SiC content (wt%) Density (g/cm3) Increase in density

blank-C/Ph 0 0.322 –
2.2. Preparation
3-C/Ph 3 0.346 0.075
5-C/Ph 5 0.373 0.158
2.2.1. Pretreatment for needled carbon fiber felt 7-C/Ph 7 0.396 0.230
In order to desize carbon fibers, needle-punched carbon fiber felt 9-C/Ph 9 0.404 0.255
was treated with analytical grade acetone and concentrated nitric acid 11-C/Ph 11 0.409 0.270

for 24 h and 2 h at room temperature. After each reagent treatment, the

felt was washed, and then dried in the oven.
in ablative surface and back-face were recorded by using infrared py-
rometer and K-type thermocouple, respectively. Simultaneously, the
2.2.2. Dispersion of SiC particles into phenolic resin changes in shape were registered by the camera. Linear ablation rate
Phenolic ethanol solution was retained constant at 25 wt%. In order was calculated using the following formula:
to investigate the effects of SiC content on mechanical, thermal, and
ablative properties, five composites containing SiC loadings which were R= (L0-La)/t (1)
3, 5, 7, 9, and 11 wt%, respectively, were prepared. Meanwhile, C/Ph -1
where R, L and t were linear ablation rate (mm·s ), thickness of the
composites without SiC particles were also fabricated as pristine sam-
samples (mm) and the ablation time (s), respectively; subscript 0 and a
ples (blank-C/Ph). The selected amount of SiC and silane coupling
represent before and after ablation test respectively.
agent (KH-550, as dispersant which was 2 wt% of SiC) were added into
The micrographs of materials were observed by scanning electron
phenolic ethanol solution. The mixture was stirred by mechanical agi-
microscope (SEM, Tescan Vega II, Tescan SRO Co., Czech Republic).
tation to disperse SiC in the mixed solution.
The fracture surface of samples was gilded before SEM observation.

2.2.3. Fabrication of SiC–C/Ph composites

Needle carbon fiber felt after pretreatment was put in the vacuum 3. Results and discussion
oven and impregnated with the mixture at room temperature. After
fully macerating under vacuum condition, the carbon felt was dried at 3.1. Density and compression strength
80 °C for 12 h and then at room temperature for 24 h, so that ethanol
was volatilized completely. The double-stage method was adopted The effect of SiC content on density of C/Ph composites is presented
which was cured at 120 °C for 1 h and 170 °C for 1 h at the heating rate in Table 1. As shown in Table 1, density of composites increases with
of 1 °C·min-1 [16,17]. Fig. 1 illustrates the fabrication process. the increase of SiC content. The composites achieve the maximum
density of 0.409 g/cm3 at the SiC content of 11 wt%. The density
change is caused by the increase of SiC content in the resin matrix.
2.3. Characterization
Fig. 2 illustrates the compression strength curves of C/Ph compo-
sites with different SiC contents. As can be seen in Fig. 2, the presence
To study the mechanical properties, compression strength was
of SiC would lead to a significant decrease in compression strength, but
tested on the samples by the universal testing machine (WDW-100D)
the effect of SiC content on reduction of compression strength is not
according to the GB/T 1448-2005 standard. The ultimate results were
obvious. Weak adhesion between SiC and phenolic resin is the main
taken from the average data of five individual tests.
reason for reducing compression strength; meanwhile, the addition of
Specimens of 100 mm × 100 mm × 25 mm were machined out and
SiC affects the formation of a continuous network structure during the
thermal conductivity was measured in the through-thickness direction
phenolic curing process, thus resulting in the reduction in compression
under steady-state conditions as per GB/T 10295-2008.
strength [18].
Thermogravimetric analysis was performed using thermal gravi-
metric analyzer instrument Q5000 (TA Instruments, USA). The sample
weighed inside the alumina crucible was put in a tube attachment, and 3.2. Thermal conductivity
heated up to 900 °C at a rate of 20 °C per minute in N2 atmosphere.
The ablation resistance of composites was evaluated in plasma wind The effect of SiC content on thermal conductivity at room tem-
tunnel at a surface pressure of 1.6 kPa, an enthalpy of 21.84 MJ kg-1, perature is exhibited in Fig. 3. As is shown, thermal conductivity of C/
and a heat flux of 1.6 MW m-2 for 50 s. The size of the test samples was Ph composites increases with the increase of SiC content. The maximum
Φ 30 mm × 25 mm. The sample was held by a graphite holder, and the thermal conductivity is obtained when SiC content is 11 wt%, which is
distance from the nozzle exit to the sample was 50 mm. Temperatures 27% higher than that of blank-C/Ph composites (0.129 W/(m·K)). On

Fig. 1. Fabrication process of the SiC modified C/Ph composites.

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Fig. 2. Compression strength of C/Ph composites with different SiC contents.

Fig. 4. TG curves of C/Ph composites with different SiC contents.

distinct trends after the second stage. It stems from the fact that SiC
reacts in the oxidation environment (composed of CO, CO2, and H2O,
mainly), and the reaction is weight gain reaction. Therefore, the re-
sidual weight of the materials with fillers is heavier than that of blank-
C/Ph composites; meanwhile, there is an inapparent difference in the
effect of content on residual weight when SiC content exceeds 5 wt%.

3.4. Ablation properties

3.4.1. Linear ablation rate

Linear ablation rates of C/Ph composites are displayed in Fig. 5. The
curve of linear ablation rate decreases first, and then increases with the
increase of SiC content, and the turning point is 5 wt%. The linear
ablation rate of 11-C/Ph samples is only 0.004 mm/s lower than that of
blank-C/Ph samples, and the reduction is only 5%. Therefore, the in-
troduction of SiC particles within the content range studied in this
paper could lower linear ablation rate of materials, and the effect is
Fig. 3. Thermal conductivity of C/Ph composites with different SiC contents. closely linked to the content of SiC.
There are molecular oxygen and atomic oxygen (excitation of mo-
the basis of the data provided by the manufacturer, thermal con- lecular oxygen) in plasma wind tunnel test [25]. The following oxida-
ductivity of SiC particles at room temperature is 83.6 W/(m·K). The tion reactions of SiC may take place in the test:
introduction of SiC could form a local high thermal conductivity region SiC+3/2O2=SiO2+CO (2)
inside the material. Furthermore, the area with high thermal con-
ductivity increases with increase of SiC, which leads to the enhance-
ment of thermal conductivity of composites.

3.3. Thermal stability

TG tests were carried out on C/Ph composites with different con-

tents of SiC. TG curves show three steps thermal degradation process in
Fig. 4. Several papers have given the explanations of the mechanisms of
phenolic pyrolysis. The first stage occurs when the temperature is below
300 °C. At this temperature range, the mass loss is primarily caused by
the small molecular substances released by the curing of phenolic resin
[19,20]. The second stage (300–700 °C) begins the pyrolysis of the
resin. Because of the fracture of crosslinked bonds, a variety of gas, such
as CO, CO2, H2O, and CH4, is released during the pyrolysis of resin
[21,22]. The primary product released in the third stage (550–900 °C) is
H2, by reason of the connection among the aromatic rings forming the
carbonaceous tridimensional structure [23,24].
TG curves of C/Ph composites with different SiC contents exhibit
the similar steps, suggesting that thermal degradation mechanism is Fig. 5. Linear ablation rate of C/Ph composites containing different contents of
independent of the presence of fillers. The pyrolysis curves show SiC particles.

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Fig. 6. Surface microstructures of ablative samples with different SiC contents: (a) blank; (b) 3; (c) 5; (d) 7; (e) 9; (f) 11.

in the ablation process does not increase. Following consideration of the

environment and surface temperature in plasma wind tunnel tests, the
formed SiO2 can react with the atomic oxygen forming SiO, which re-
sults in the evaporation of oxidation products [28]. The evaporation of
SiO2 may experience the following reactions [26]:

2SiO2+2O=Si2O3+O2 (6)

Si2O3=SiO+SiO2 (7)

The above reactions could accelerate the consumption of SiO2.

Furthermore, when SiC content in the materials increases gradually, the
oxidation process of SiC changes from passive oxidation to active oxi-
dation, and the product changes from SiO2 to SiO [29].
When the content of SiC is less than 5 wt%, passive oxidations of SiC
occupy the dominant position. The generation of SiO2 could form a
liquid film on the surface of carbon fiber and pyrolysis carbon, so as to
decrease linear ablation rate. When the content of SiC is 5–11 wt%,
active oxidation reactions occupy more proportion, and then the gen-
Fig. 7. The ablative surface temperature curves of C/Ph composites with dif- eration of SiO increases (Reactions 4, 5, 6 and 7), so as to accelerat the
ferent SiC contents. consumption of SiO2 and increase linear ablation rate.

3.4.2. Ablative surface temperature

SiC+3O=SiO2+CO (3)
Temperature trend on the ablative surface temperature during
SiC+O2=SiO+CO (4) plasma wind tunnel tests is reported in Fig. 7. The addition of SiC could
decrease ablative surface temperature, and the effect of SiC content on
SiC+2O=SiO+CO (5)
ablative surface temperature is not obvious. 5-C/Ph composites have
Reactions (2) and (3) are the passive oxidation reaction equations of the lowest surface temperature of 1956 °C, 154 °C lower than that of
SiC in the environment of molecular oxygen and atomic oxygen re- blank-C/Ph composites.
spectively, while reactions (4) and (5) are the active oxidation reaction Reactions 2–7 are exothermic reactions. The introduction of SiC into
equations. In the light of the literatures [26,27], the oxidation of SiC by C/Ph composites would lead to the increase of heat flux density and
the atomic oxygen Reactions (3) and (5) is the dominant process during ablative surface temperature. However, the formation of SiO2 with
ablation test. Fig. 6 shows the typical microstructures of ablated sam- higher thermal emissivity and the volatile heat absorption of SiO could
ples with different SiC contents in the ablative surface. It can be seen decrease surface temperature of composites. Therefore, the heat gen-
that there are a lot of carbon fibers and hardly no matrix in Fig. 6a. erated by exothermic reactions is much less than that generated by the
Nevertheless, the matrix including SiO2 exists on the ablative surface of radiation of SiO2 at high temperature in 3-C/Ph composites. The pas-
SiC–C/Ph samples (Fig. 6b–f). It indicates that the passive oxidation of sive oxidation of SiC is dominant, and the rates of reactions 6 and 7 are
SiC by atomic oxygen (Reaction 3) forming SiO2 should be the domi- slow. As SiC content increases gradually (3–5 wt%), active oxidation of
nant process during ablation. The formed amorphous SiO2 could keep SiC is intensified, and the heat released by reactions 6 and 7 increased.
materials away from the erosion of the plasma freestream in plasma The formation of SiO2 on the ablative surface does not increase sig-
wind tunnel, thereby reducing linear ablation rate and improving ab- nificantly, so ablative surface temperature of 5-C/Ph samples is slightly
lation resistance. higher than that of 3-C/Ph samples. When SiC content continues to
The difference of the residual matrix on the ablative surface in increase (5–11 wt%), the exothermic and endothermic reactions are
Fig. 6b to f is not significant, indicating that the SiO2 content generated further intensified, but SiO2 on the ablative surface does not increase
substantially. Therefore, the maximum surface temperature remains

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interests or personal relationships that could have appeared to influ-

ence the work reported in this paper.

Acknowledgements

This work was supported by the National Natural Science

Foundation of China (11772042 and 11472037).

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