Effects of high temperature heat treatment on the micro structure and mechanical performance of C/C-SiC composite materials
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摘要: 后高温热处理对反应熔融浸渗法(RMI)制备C/C-SiC复合材料的微观结构与性能有着至关重要的影响。为研究后高温热处理对RMI制备C/C-SiC复合材料微观结构和力学性能影响及机制，本研究通过等温化学气相渗透法(CVI)工艺，以天然气为碳源气体，氮气为载气和稀释气体，在碳纤维预制体内部沉积热解碳基体，制得密度为1.2 g/cm3的C/C多孔体，然后通过反应熔融浸渗法制备出C/C-SiC复合材料，研究了不同后高温热处理温度对C/C-SiC复合材料相组成、内应力及力学性能的影响。将制备得到的C/C-SiC复合材料分别在1300℃、1500℃和1700℃下进行后高温热处理，研究了后高温热处理对C/C-SiC复合材料密度、孔隙率、基体成分、内应力以及对弯曲性能的影响。结果表明:经1300℃、1500℃及1700℃后热处理后，C/C-SiC复合材料的密度降低，开孔率增加，SiC基体含量上升，SiC基体的分布更为广泛，同时还伴随有残余Si挥发产生的大孔，残余Si含量显著降低。在1300℃、1500℃和1700℃的后热处理导致弯曲强度先增加后减小，1500℃后处理时弯曲强度最大为296.52 MPa，随着后处理温度提高，弯曲模量降低，1700℃后热处理下降程度最大。Abstract: The microstructure and properties of C/C-SiC composites prepared by reactive melt infiltration (RMI) are significantly affected by post-heat treatment. In order to study the effect and mechanism of post-heat treatment on the microstructure and mechanical properties of C/C-SiC composites prepared by RMI, the isothermal chemical vapor infiltration (CVI) process was used to deposit pyrolytic carbon matrix in the carbon fiber preform, and C/C porous bodies with a density of 1.2 g/cm3 were prepared by using natural gas as carbon source gas and nitrogen as carrier gas and dilution gas. Then C/C-SiC composites were prepared by reactive melt infiltration method. The effects of different post-heat treatment temperatures on the phase composition, internal stress and mechanical properties of C/C-SiC composites were studied. The prepared C/C-SiC composites were treated at 1300℃, 1500℃ and 1700℃ respectively. The effects of post-high temperature heat treatment on the density, porosity, matrix composition, internal stress and bending properties of the C/C-SiC composites were investigated. The results show that after heat treatment at 1300℃, 1500℃ and 1700℃, the density of C/C-SiC composites decreases, the porosity increases, the content of SiC matrix increases, the distribution of SiC matrix becomes more extensive, and the residual Si content decreases significantly with large pores caused by residual Si volatilization. At 1300℃, 1500℃ and 1700℃, the bending strength increases first and then decreases. At 1500℃, the bending strength reaches a maximum of 296.52 MPa. With the increase of the post-treatment temperature, the bending modulus decreases, and at 1700℃, the bending strength decreases the most.
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Key words:
- C/C-SiC /
- RMI /
- High-temperature thermal treatment /
- Flexural properties /
- microscopic structure
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图 1 后热处理对复合材料密度和孔隙率的影响：(a) 密度；(b)孔隙率
Figure 1. Effect of post heat treatment on density and porosity of composite materials: (a) Density; (b) Porosity
图 2 后热处理对复合材料SiC基体含量及残余硅含量的影响：(a) SiC基体含量的变化；(b)残余Si含量的变化
Figure 2. The effect of post heat treatment on the content of SiC matrix and residual silicon in composite materials: (a) Changes in SiC matrix content;(b) Changes in residual Si content
图 3 2250-PR-1300试样的SEM图片。(a) 整体结构；(b) 0°无纬布；(c) 碳毡；(d)针刺纤维；(e) 90°无纬布；(f) 纤维与基体炭之间的结合
Figure 3. SEM images of samples 2250-PR-1300. (a) Overall structure; (b) 0°weft free fabric; (c) Carbon felt; (d) Acupuncture fibers; (e) 90°weft free fabric; (f) The bonding between fibers and matrix carbon
图 4 2250-PR-1500试样的SEM图片。(a) 整体结构；(b) 0°无纬布；(c) 碳毡；(d)针刺纤维；(e) 90°无纬布；(f) 纤维与基体炭之间的结合
Figure 4. SEM image of 2250-PR-1500 sample. (a) Overall structure; (b) 0°weft free fabric; (c) Carbon felt; (d) Acupuncture fibers; (e) 90°weft free fabric;(f) The bonding between fibers and matrix carbon
图 5 2250-PR-1700试样的SEM图片。(a) 纤维与基体炭之间的结合；(b)碳毡； (c) 0°无纬布；(d)针刺纤维； (e) 90°无纬布； (f) 整体结构
Figure 5. SEM image of 2250-PR-1700 sample. (a) Overall structure; (b) 0°weft free fabric; (c) Carbon felt; (d) Acupuncture fibers; (e) 90°weft free fabric; (f) The bonding between fibers and matrix carbon
图 6 经不同温度后热处理后C/C-SiC复合材料的XRD图谱
Figure 6. XRD patterns of C/C-SiC composites after heat treatment at different temperatures
图 7 经不同温度后热处理后C/C-SiC复合材料XRD图谱的谱峰偏移：(a) SiC (111)晶面的谱峰偏移；(b) SiC (220) 晶面的谱峰偏移； (c) SiC (311) 晶面的谱峰偏移； (d) 石墨炭(002)晶面的谱峰偏移
Figure 7. The peak shift of the XRD spectrum of C/C-SiC composite material after heat treatment at different temperatures: (a) Spectral peak shift of SiC (111) crystal plane; (b) Spectral peak shift of SiC (220) crystal plane; (c) Spectral peak shift of SiC (311) crystal plane;(d) Spectral peak shift of graphite (002) crystal surface
图 8 不同后热处理温度处理后C/C-SiC复合材料的拉曼Mapping图：(a) 2250-PR mapping图; (b) 2250-PR-1300 mapping图;(c) 2250-PR-1500 mapping图; (d) 2250-PR-1700 mapping图
Figure 8. Raman Mapping of C/C-SiC composite materials treated at different post heat treatment temperatures: (a) 2250-PR mapping diagram; (b) 2250-PR-1300 mapping diagram; (c) 2250-PR-1500 mapping diagram; (d) 2250-PR-1700 mapping diagram.
图 9 2250-PR-1300、2250-PR-1500及2250-PR-1700弯曲试样断口的SEM图。(a) 和(b) 1300℃后热处理; (c) 和(d)1500℃后热处理; (e) 和(f)1700℃后热处理
Figure 9. SEM images of the fracture surface of 2250-PR-1300、2250-PR-1500 and 2250-PR-1700 bending specimens. (a) and (b) Heat treatment after 1300℃; (c) and (d) Heat treatment after 1500℃; (e) and (f) Heat treatment after 1700℃
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