Ceramics International xxx (xxxx) xxx–xxx

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

Fabrication and ultra-high-temperature properties of lightweight carbon-

bonded carbon fiber composites
Yanfei Chena,b, Yunong Zhaoc, Debao Liua, Ran Taoa, Tianbao Chengd, Shigang Aia,
Baosheng Xua,b,*, Yazheng Yanga,b, Daining Fanga,b
a
Institute of Advanced Structure Technology, Beijing Institute of Technology, Beijing, 100081, PR China
b
Beijing Key Laboratory of Lightweight Multi-functional Composite Materials and Structures, Beijing Institute of Technology, Beijing, 100081, PR China
c
State Key Laboratory for Turbulence and Complex Systems, College of Engineering, Peking University, Beijing, 100871, China
d
Chongqing Key Laboratory of Heterogeneous Material Mechanics, College of Aerospace Engineering, Chongqing University, Chongqing, 400030, China

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

Keywords: Carbon bonded carbon fiber (CBCF) composites with different fiber volume fractions (FVFs) are prepared. This
CBCF composites paper mainly investigates the effect of FVFs and the ultra-high temperature on the mechanical and thermal
Ultra-high temperature properties of CBCF composites. Experimental results show that the microstructure of CBCF composites is ani-
Mechanical and thermal properties sotropic, random distribution in xy direction and layering in z direction. With higher FVFs, the modulus and
fracture strength are higher. The fracture strength in xy direction is greatly higher than that in z direction,
because more fibers bear the load. Elastoplastic behavior of stress-strain curves is observed in z direction, which
is attributed to the compression of porosity and gap. Especially, at ultra-high temperature, the plastic hardening
effect is remarkable. In addition, the thermal conductivities of CBCF composites with different FVFs are char-
acterized, which increase exponentially with temperature.

1. Introduction
Due to the light weight, high porosity, low thermal conductivity and
high temperature capability, carbon-bonded carbon fiber (CBCF) com-
posites have been widely used for thermal insulation applications
[1–3]. Inside the material, a carbon fiber network is bonded together at
the intersections of fibers by discrete carbon matrix [4]. Fiber network
presents a dissipative damage tolerant behavior [5]. Traditional CBCF
composites are prepared using chopped carbon fibers and phenolic
resin prepared by vacuum filtration [6] or pressure filtration [7]. To
overcome poor mechanical and thermal performance owing to the in-
homogeneous distribution of carbon fibers and phenolic resin powder,
pressure filtration technique was developed [8,9]. Above prepared
CBCF composites are of weak anti-oxidation resistance above 500 °C
under oxidative environments. Therefore, antioxidant particles or si-
lica-based glass coatings were introduced to overcome these issues
[10–13]. CBCF composites decorated with nano SiO2–Al2O3 aerogel
was prepared by sol-gel impregnation to improve their thermal in-
sulation and mechanical properties [14]. In addition, micromechanical
and finite element models are used to study the failure behaviors of
lightweight chopped fiber reinforced composites [15,16]. Although
CBCF composites are promising candidates for use in thermal insulation
systems and many improvements of properties have been made, the
high-temperature mechanical performances are rarely reported. In this
context, CBCF composites with different FVFs are prepared, and their
high-temperature properties, including thermal and mechanical prop-
erties, are investigated.
2. Experimental procedures
2.1. Material
The fabrication method of CBCF composites is referred to Ref. [2].
Firstly, the rayon-based carbon fibers with diameter of about 7.0 μm
were cut into about 1.0 mm long, and then dispersed in a slurry with
mass content of 0.6 wt% polyethyleneimine as dispersant. Secondly, the
chopped carbon fibers were added in above solution and stirred well to
make them disperse evenly. Thirdly, phenolic resin was added and
continued to stir to make the chopped carbon fibers and phenolic resin
disperse well again. Fourthly, polyacrylamide was added to make
phenolic resin be adsorbed to the surface of fibers without agglom-
eration. Fifthly, stirred above mixed slurry, quickly poured it into the
mold, filtered out the water and the green body was shaped by com-
pression moulding. Finally, the green body was kept warm for 5 h at

*
Corresponding author. Institute of Advanced Structure Technology, Beijing Institute of Technology, Beijing, 100081, PR China.
E-mail address: xubsh@bit.edu.cn (B. Xu).

https://doi.org/10.1016/j.ceramint.2019.07.250
Received 29 May 2019; Received in revised form 20 July 2019; Accepted 22 July 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Yanfei Chen, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2019.07.250
Y. Chen, et al. Ceramics International xxx (xxxx) xxx–xxx

80 °C, cured for 3 h at 150 °C and pyrolyzed under 1000 °C in vacuum

furnace. The CBCF composites with different FVFs were controlled by
applied load during compression moulding. The fabricated CBCF com-
posites were cut into specimens with a size of
10 mm × 10 mm × 12 mm for compressive test. The as-received CBCF
composites attained three FVFs of 9.6%, 13.2% and 14.5%.

2.2. Characterization

The morphology of CBCF composites were examined by a FEI

Quanta 250 scanning electron microscopy (SEM). The thermal con-
ductivity of the disk–shape specimens with diameters of 12.7 mm and
thicknesses of approximately 2.0 mm was measured by laser flash
method using a Netzsch LFA 457 apparatus based on ASTM E1461. The
compressive properties of specimens at ultra-high temperature were
performed by a self-developed ultra-high-temperature thermo-me-
chanical coupled test instrument, which has been reported in previous
investigation [17]. The tests were conducted at a constant displacement
rate of 0.5 mm/min. The force was recorded by the load cell of the test Fig. 2. Fibre orientation angle in xy direction.
machine. The compressive stress, compressive strain and elastic mod-
ulus were calculated with following equations: to the different distribution of fibers in the two directions. In xy di-
P l H ⋅ΔP rection, there are more fibers to bear the load than those in z direction.
σ= , ε= , E=
W ⋅L H W ⋅L⋅Δl (1) Therefore, the fracture strength in xy direction is greater than that in z
direction. CBCF composites exhibit elastoplastic behavior in z direction.
where P and l are the load and displacement respectively in the testing
For the material in z direction, there exists long plastic hardening
process, and L, W and H are the length, width and height of the spe-
process for low FVF specimens. The plastic hardening process was not
cimen. ΔP / Δl is the slope of the straight line in the load-displacement
only attributed to the compression of porosity, but also the bending and
curve recorded during testing.
rotation of the fibers. Similar behavior is observed for compressive
specimen with low FVF (9.6%) in xy direction. For the specimens with
3. Results and discussion
higher FVF in xy direction, larger than 13.1%, when stress reaches peak
value, it instantly falls and then decreases slowly. However, a degree of
Fig. 1 shows the as-received sample and the SEM images of CBCF
plastic hardening behavior is still observed in z direction. This is be-
composites. The chopped fibers are distributed anisotropically. The fi-
cause there exist gaps between layers, which is compressed during load,
bers in xy direction are distributed uniformly, but layering effect is
as shown in Fig. 1c. Fig. 4 shows the relationship between the tem-
observed in z direction. The fibers are bonded together by discrete re-
perature and compressive stress-strain curve of 14.5% FVF specimen.
gions of vitreous carbons. Although the SEM images shows the or-
The effect of temperature on stress-strain behavior in xy direction is not
ientation of the fibers, the extent of the orientation is not quantified.
obvious. However, as temperature rising, the plastic hardening effect is
Image analysis technique [18] is used to determine the degree of or-
obviously enhanced in z direction. The failure strength in z direction is
ientation through orientation histograms. xy plane sample with 9.6%
not tested. The modulus and strength versus temperature specimen with
FVF is analyzed. Fig. 2 illustrates the fiber orientation in xy plane. Al-
14.5% FVF are presented in Fig. 5. In xy direction, the modulus and
though some scatter of the data (about 90°) is evident, the general trend
fracture strength increase with rising temperature up to 1400 °C , and
indicates a fairly random variation of fiber number with angle. Marked
then decreases when temperature is higher than 1400 °C. However, the
anisotropy of the fiber orientations has been found in z direction [4].
relationship between modulus and temperature in z direction is oppo-
site. As shown in Fig. 4b, when temperature is higher than 800 °C,
3.1. Mechanical properties rising temperature increases the yield stress and failure strength in z
direction.
Fig. 3 shows the influence of FVF on the compressive stress-strain In the experiments at room temperature and ultra-high temperature,
curve at room temperature. Higher the FVF, the greater modulus and we find that the effect of temperature on the fracture morphologies is
strength. However, when FVF is greater than 13.1%, the influence is not similar. Fig. 6 shows the fracture morphologies in xy and z directions.
remarkable and the stress-strain curves in two directions have almost Delamination shown in Fig. 6b is a typical failure mode, which is
the same trend. The fracture strength in xy direction is almost three consistent with the experimental observation. In z direction, the
times greater than that in z direction. The differences can be attributed

Fig. 1. (a) Macroscopic image of CBCF composite; SEM images of the CBCF composite in (b) xy direction and (c) z direction.

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Fig. 3. The influence of the FVF on the compressive stress-strain at room temperature. (a) in xy direction; (b) in z direction.

material is broken into debris. Internal fiber debonded from the

bonding materials, the broken bonding material and fiber broken into
segments are almost observed in two directions.

3.2. Thermal properties

Fig. 7 shows the relation between thermal conductivity and tem-

perature. The thermal conductivity in both directions increases with
rising temperature for CBCF composites with 13.1% FVF and 14.5%
FVF, respectively, which increase exponentially with temperature. The
thermal conductivity in xy direction is higher than that in z direction,
which can be also attributed to the microstructure anisotropy in CBCF
composite. For CBCF composite with 13.1% FVF, the measured con-
ductivities of CBCF composite at room temperature are 0.076
W ⋅m−1⋅K−1 in z direction and 0.149 W ⋅m−1⋅K−1 in xy direction. With
temperature rising up to 1500 °C, corresponding thermal conductivities
Fig. 5. The modulus and strength versus temperature for the specimens with
increases to 1.069 W ⋅m−1⋅K−1 and 1.385 W ⋅m−1⋅K−1, respectively. For
14.5% FVF.
CBCF composite with 14.5% FVF, the measured conductivities of CBCF
composite at room temperature are 0.075 W ⋅m−1⋅K−1 in z direction and
0.180 W ⋅m−1⋅K−1 in xy direction. With temperature rising up to 1500 temperature and ultra-high-temperature are investigated. Three types
°C , corresponding thermal conductivities increases to 1.314 W ⋅m−1⋅K−1 of FVFs of CBCF composites are prepared by pressure filtration tech-
and 1.516 W ⋅m−1⋅K−1, respectively. The thermal conductivity is higher nique. The microstructure of CBCF composites is anisotropic, random
for CBCF composite with higher FVF, especially in z direction. distribution in xy direction and layering in z direction. Elastoplastic
behavior is observed in z direction, which is attributed to the com-
pression of porosity and gap. The fracture strength in xy direction is
4. Conclusion greatly higher than that in z direction is because more fibers bear the
load. At ultra-high temperature, the plastic hardening effect is re-
In this paper, the microstructure, the effect of FVFs on the me- markable. In addition, the thermal conductivities of CBCF composites
chanical properties and thermal properties of CBCF composites at room

Fig. 4. The influence of temperature on the compressive stress-strain for the specimens with 14.5% FVF. (a) in xy direction; (b) in z direction.

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Y. Chen, et al.
Fig. 6. The fracture morphologies of compressive specimens (a) in xy direction; (b) in z direction.
Fig. 7. The thermal conductivity of CBCF composites with 13.1% and 14.5%
FVFs.
with different FVFs are characterized, which increase exponentially
with temperature.
Acknowledgments
This work is supported by the National Natural Science Foundation
of China (Nos. 11672030 and 11602125), the China Postdoctoral
Science Foundation (Nos. 2019M650500), and Beijing Institute of
Technology Research Fund Program for Young Scholars.
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