Author’s Accepted Manuscript

Enhanced mechanical properties of SiC/Al

composites at cryogenic temperatures

Qiuyuan Liu, Feng Wang, Weiwei Wu, Di An,

Zhiyong He, Yanpeng Xue, Qifu Zhang, Zhipeng
Xie
www.elsevier.com/locate/ceri

PII: S0272-8842(18)33051-7
DOI: https://doi.org/10.1016/j.ceramint.2018.10.233
Reference: CERI19945
To appear in: Ceramics International
Received date: 8 October 2018
Revised date: 24 October 2018
Accepted date: 29 October 2018
Cite this article as: Qiuyuan Liu, Feng Wang, Weiwei Wu, Di An, Zhiyong He,
Yanpeng Xue, Qifu Zhang and Zhipeng Xie, Enhanced mechanical properties of
SiC/Al composites at cryogenic temperatures, Ceramics International,
https://doi.org/10.1016/j.ceramint.2018.10.233
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Enhanced mechanical properties of SiC/Al composites at
cryogenic temperatures

Qiuyuan Liu a,b, Feng Wang b,Weiwei Wuc, Di Ana, Zhiyong He b, Yanpeng Xued, Qifu

Zhang b, Zhipeng Xiea,*

a
State Key Laboratory of New Ceramics and Fine Processing, Tsinghua University,

Beijing 100084, China

b
China Iron & Steel Research Institute Group, Beijing 100081, China

c
Sinoma Wind Power Blade Co., Ltd, Beijing 100192, China

d
National Center for Materials Service Safety, University of Science and Technology

Beijing, 100083, Beijing, China

*
Corresponding Zhipeng Xie, Tel/Fax: +86 1062794603, xzp@mail.tsinghua.edu.cn

Abstract:

In this study, silicon carbide particulates reinforced Al matrix (SiC/Al) composites

was prepared by the pressureless infiltration technique. The phase transformation and

mechanical properties of SiC/Al compositess were observed at different cryogenic

temperatures. With the temperature decreasing, the phase composition retained the

same and no new diffraction peaks were detected. The mechanical properties of the

samples were improved at cryogenic temperatures. Upon decreasing the temperature

from 293 K to 77 K, the flexural strength increased from 289.08±21.58 MPa to

353.46±18.75 MPa, and fracture toughness went up from 7.52±0.72 MPa·m1/2 to

9.26±0.53 MPa·m1/2, respectively. The enhancement of mechanical properties was

due to the elastic modulus increasing. Possessing the excellent mechanical properties

at cryogenic temperatures, SiC/Al composites could have potential applications in

cryogenic environment.

Keywords:

SiC/Al composites; Mechanical properties; Cryogenic temperatures; Strengthening

mechanism

1. Introduction

Recently, the requirements for reducing the quality of spacecraft structures and

improving the payload capacity of spacecraft have been becoming more and more

urgent due to the development of aerospace science and engineering. In order to solve

this problem, the best way is to select the materials with specific strength, thermal

stability and better comprehensive performance for the design of spacecraft structure.

SiC/Al composites has attracted more and more attentions because of its relatively

good comprehensive properties, such as high specific modulus, hardness and

[1-3]
corrosion resistance . Many literatures have reported that SiC/Al is a potential

material which could be used for the cryogenic application[4-20]. For example, SiC/Al

composites could be used as the structure material in spacecraft for remote sensing

satellites with long duty cycles. But few researches about mechanical properties of

SiC/Al composites under cryogenic environment are reported.

 In this work, the SiC/Al composites prepared by pressureless infiltration technique

was used as the experimental material. The effects of different temperatures on the

phase evolution, flexural strength and fracture toughness of SiC/Al composites were

investigated. The strengthening mechanism was also discussed as well.

2. Experimental

2.1. Fabrication of the SiC/Al composites

α-SiC powders with diameter of 10 µm and 90 µm (purity of 99.7%, Qingzhou

micro powder Co., Ltd, Shandong province, China) and aluminum alloy (Self-made,

Al-8%Si-5%Mg) were used as starting materials to prepare SiC/Al composites. Firstly,

SiC powders were blended with the PVA (Polyvinyl alcohol with average degree of

polymerization of 1750, Sinopharm Chemical Reagent Co., Ltd., Beijing, China), then

pressed to cylindrical pellets (60 mm) at a pressure of 20 MPa. The obtained samples

were heated at 500 ºC for 2 h to burn out the binder, then sintered at 1100 ºC for 4 h to

form a SiO2 layer on the particle surfaces which was used to enhance the wetting

properties of SiC by aluminum alloy. The aluminum alloy and sintered SiC samples

were put into a graphite furnace, then sintered at 930 ºC for 2 hours in the flowing

pure nitrogen atmosphere. Finally, the SiC/Al composites was obtained when the

temperature cooled down.

2.2. Characterization

The density of the obtained samples was evaluated according to Archimedes’

method, by using deionized water as the medium. The microstructures of the samples

were determined by scanning electron microscope (SEM, Merlin Compact, Zeiss,

Germany). The phase composition of the samples at the temperature of 293 K, 195 K

and 77 K was characterized by In-situ x-ray diffraction (XRD, XRD-6000,

SHIMADZU, Japan), respectively. The cryogenic temperature was achieved by a test

chamber filled with liquid nitrogen.

The flexural strength (σf) was tested by a three-point bending method on 4 mm × 3

mm × 36 mm specimens in a universal testing machine (AG-IC, Shimadzu, Japan)

with a span of 30 mm and a crosshead speed of 0.5 mm/min. The fracture toughness

(K1C) was evaluated by a single-edge notched beam test with a span of 30 mm using 4

mm × 6 mm × 36 mm test bars and the crosshead speed of 0.05 mm/min. The test

temperature of the flexural strength and fracture toughness was 293 K, 195 K and 77

K, respectively.

The Raman spectra were measured by a Raman spectroscopic apparatus (Lab RAM

HR Evolution, HORIBA Jobin Yvon, Paris, France). Its excitation source as an

argon-ion laser that was operated at a wavelength of 473 nm and 532 nm with a power

of 300 mW at the laser head.

3. Results and discussion

The bulk density of the SiC/Al composites is 2.90 g/cm3. The morphology of the
as-prepared samples is shown in Fig. 1. It could be observed from the image that SiC
particles with diameter of 10 µm and 90 µm distributed uniformly in the SiC/Al
composites. In addition, no big pores were observed. The cross section reveals that the
interface between second-phase SiC particles and Al matrix is visible and
organizational structure is even.
 Fig. 1. SEM images of the samples (a) surface topography of and (b)
cross-section topography.

Fig. 2 displayed the XRD patterns of the samples at 77 K, 195 K and 293 K. At 293

K, the major phases of the composites were SiC and Al. Other weak diffraction peaks,

such as Mg2Si, were also detected. With the temperature decreasing, the phase

composition retained the same and only the diffraction peaks shifted towards low

theta value. The lattice constants of SiC and Al of the composites were exhibited in

Table 1. When the temperature reduced the from 293 K to 77 K, lattice constant of

SiC went down from 15.1437 Å to15.1351 Å according to the diffraction peaks of

(006) and (112). Similarly, the calculated lattice constant of Al decreased from 4.0496

Å to 4.0411 Å in view of the diffraction peaks (111) position. Moreover, the cell

volume of Al matrix reduced from 66.4104 Å3 to 65.9882 Å3. The results above

indicate that lattice of SiC/Al composites would shrink at cryogenic temperatures.

 Fig. 2. XRD patterns of the samples at different temperatures.

Table 1. Lattice constants of the SiC and Al phases

crystal lattice constant

phase
indices 293 K 77 K

SiC (006)、(112) 15.1437 Å 15.1351 Å

Al (111) 4.0496 Å 4.0411 Å

The flexural strength of the composites was tested by three-point bending method at

293 K, 195 K and 77 K, which were displayed in Fig. 3. It could be observed that the

temperature went down from 293 K to 77 K, the flexural strength increased from

289.08±21.58 MPa to 353.46±18.75 MPa.

 Fig. 3. Flexural strength of the sample at different temperatures.

Under the cryogenic environment, Griffth equation is used to describe the enhanced

strength qualitatively[21],
1
1  2 E  2
f    (1)
Y  c0 

where, Eγ, γ,c0 and Y is elastic modulus, fracture surface energy ,original crack size

and crack shape parameter, respectively. The elastic modulus E and fracture surface

energy γ will increase by reducing the temperature which can be attributed to the

stronger bonding force between atoms, while c0 and Y remain constant.

The lattice constants of SiC and Al of the composites were shrunk with the

temperature decreasing (as seen in Table 1). It was suggested that the distance

between atoms was reduced, then the bonding force was enhanced which would lead

to the elastic modulus E increasing. This is the strength improvement mechanism of

the sample at cryogenic temperature.

Fig. 4 presents the fracture toughness of the composites measured at different

temperatures. It was easily observed that the fracture toughness was 9.26±0.53

MPa·m1/2 at 77 K, increasing by 23.1% compared with that of the sample at 273 K.

[22]
According to the literature , fracture toughness KIC could be calculated by the

following equation,

K1C   2 E 
1
2
(2)

where E is the elastic modulus and γ is the fracture surface energy. According to the

analysis of the flexural strength, the elastic modulus E and fracture surface energy γ

increased with the the temperature reducing. Therefore the fracture toughness would

improve due to the enhancement of E and γ under cryogenic temperatures. Moreover,

[23-26]
according to the literature the residual stress will generate with the temperature

decreasing due to the thermal expansion mismatch of second-phase SiC particles

(αSiC=4.2×10-6 K-1) compared with Al matrix (αAl=23×10-6 K-1). The induced

residual stress could be expressed by the following formula [27],

T
 (3)
1  m  2 Em  1  2 p  E p

where σ is the residual stress, ΔT is the difference between sintering and testing

temperature, Δα is the difference in coefficients of thermal expansion, Em ( Ep) and νm

(νp) is the Young's modulus of the matrix(the particle) and the Poisson's rations of the

matrix( the particle), respectively.

 Fig. 4. Fracture toughness of the samples at different temperatures.

According to the formula, the residual stress σ is proportional to ΔT. Therefore, σ

will increase by reducing the temperature down to 77 K. Due to the smaller linear

coefficient of thermal expansion of the SiC compared to the SiC/Al matrix, free SiC

particles are subjected to a radial compression field which creates extra resistance to

the approaching crack front. For illustrating this, in-situ raman spectroscopy of SiC/Al

composites at selected temperatures was recorded (Fig.5). During cooling, the SiC

characteristic peak located at 790 cm-1 went red shift, indicating that residual stresses

increased as a result of the difference of thermal expansion coefficient with the

temperature decreasing[28]. Hence, resulting from higher residual stress, stronger

resistance to crack propagation at 77 K could augment the fracture toughness of

SiC/Al composites than that at room temperature.

 Fig. 5 In-situ Raman spectrum of the samples at various temperatures

4. Conclusions

In summary, SiC/Al composites were fabricated by the pressureless infiltration

technique. Mechanical properties of the composites at cryogenic temperatures were

investigated. At 77 K, the flexural strength and fracture toughness was 353.46±18.75

MPa and 9.26±0.53 MPa·m1/2 respectively, increasing by 22.3% and 23.1%, as

compared with that of the sample at 273 K. The mechanical properties of the samples

were enhanced with the temperature decreasing. With the temperature decreasing, the

elastic modulus was increasing due to binding energy enhancement among atoms

under cryogenic environment which was the reason for the enhancement of

mechanical properties. Moreover, under the condition of cryogenic temperatures, the

improvement of fracture toughness could be attributed to the residual stress

originating from the thermal expansion mismatch between the second-phase SiC

particles and Al matrix. Based on the favorable performances, the as-prepared SiC/Al
composites would have potential applications in cryogenic environment.

Acknowledgments
The National Science and Technology Major Project (Grant no. 2013ZX02104) and

CAS Key Laboratory of Cryogenics, TIPC (CRYO201804) were sincerely

acknowledged by the authors for the support.

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