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TiB2材料由于高熔点和低原子序数成为新一代核反应堆等离子体壁材料的候选者之一. 然而, 单一TiB2材料难以制备和加工, 因此在TiB2中加入助烧剂来优化其性能具有重要的应用价值. 本论文利用放电等离子体烧结得到Ti质量分数分别为3%和6%的两种TiB2-SiC-Ti材料. 材料在室温条件下进行能量60 keV, 离子注量为2 × 1017 ions/cm2的He+辐照, 辐照前后材料都进行1500 ℃热处理. 利用能量色散光谱、拉曼光谱、掠角X射线衍射光谱、维氏硬度、划痕深度和宽度分布、扫描电子显微镜等手段表征材料在制备态、辐照后和退火下的微观结构及宏观性能. 结果显示, TiB2-SiC-Ti(Ti的质量分数为3%)材料本身致密性低、耐磨性差、硬度低且抗氧化性弱. 但与TiB2-SiC-Ti(Ti的质量分数为6%)材料相比, TiB2-SiC-Ti(Ti的质量分数为3%)材料更抗辐照; 论文对该实验结果进行讨论, 认为在3%—6%质量分数范围内, 增加Ti含量有助于提升TiB2-SiC-Ti材料致密性和力学性能.
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关键词:
- TiB2-SiC-Ti材料 /
- 离子辐照 /
- 高温氧化 /
- 力学性能
Since the 21st century, low atomic number material coating has been considered as one of methods for treating the first wall of controllable thermonuclear fusion device . The TiB2 material with high melting point, high hardness, low coefficient of thermal expansion, excellent wear resistance and low atomic number has entered into people’s field of vision. Single TiB2 is difficult to sinter and process into other products. Therefore, adding ceramic and metal additives to TiB2 matrix material to effectively improve the mechanical properties and processability of the material has become a research hotspot. On the basis of the existing researches of TiB2-SiC, in the present work the metal Ti powder is added as the second additive to improve the properties of TiB2 composite. The TiB2 and SiC are mixed at a mass ratio of 2 to 3, then two kinds of TiB2-SiC-Ti materials with different amounts of Ti content are prepared by spark plasma sintering (SPS) technology. The materials are irradiated by a He+ beam with energy of 60 keV and ion fluence of 2 × 1017 ions/cm2 at room temperature. The material is heat-treated at 1500 ℃ before and also after irradiation. The performances of prepared samples, the effect of irradiation on materials and the results of high temperature heat treatment are characterized by energy dispersive spectroscopy, Raman spectrum, grazing angle x-ray diffraction spectrum, Vickers hardness, wear resistance test, and scanning electron microscope. The results show that the surface morphology and toughness of TiB2-SiC-Ti material with 3% Ti mass fraction are poor as shown in SEM images. The wear resistance test indicates that the material surface is seriously worn and the wear resistance is poor. The X-ray diffraction spectrum and Raman spectra show that the material is oxidized seriously at 1500 ℃, which is likely to be the cause of the poor compactness of materials. Raman spectra, Grazing angle X-ray diffraction spectrum and some Vickers hardness data before and after irradiation indicate that the material with low Ti content possess better crystal structure and weaker irradiation hardening. In conclusion, the TiB2-SiC-Ti material with 3% Ti mass fraction exhibits lower density, poorer wear resistance and lower hardness, while the material with lower Ti mass fraction is more resistant to irradiation than the material with 6% Ti mass fraction at room temperature.-
Keywords:
- TiB2-SiC-Ti materials /
- ion irradiation /
- high-temperature oxidation /
- mechanical character
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图 1 SRIM 模拟60 keV, 2 × 1017 ions/cm2 He+ 辐照TiB2-SiC-Ti复合材料得到的损伤深度分布及He原子浓度深度分布图
Fig. 1. The depth distribution of damage and concentration of He atoms calculated with SRIM for TiB2-SiC-Ti irradiated with 60 keV He+ ions to a fluence of 2 × 1017 ions/cm2
图 2 (a) TiB2-SiC-Ti(Ti的质量分数为3%)样品和 (b) TiB2-SiC-Ti(Ti的质量分数为6%)样品的能量色散X射线光谱图
Fig. 2. Energy dispersion X-ray spectroscopy of TiB2-SiC-Ti ((the mass fraction of Ti is 3%)) samples (a) and TiB2-SiC-Ti (the mass fraction of Ti is 6%) samples (b).
图 3 制备态、辐照前1500 ℃热处理、室温下氦离子辐照和辐照后1500 ℃退火4种条件下TiB2-SiC-Ti(Ti的质量分数为3%)样品(a)和TiB2-SiC-Ti(Ti的质量分数为6%)样品(b)的拉曼光谱
Fig. 3. Raman spectra of TiB2-SiC-Ti (the mass fraction of Ti is 3%) (a) and TiB2-SiC-Ti (the mass fraction of Ti is 6%) (b) under four conditions: Original state, heat treatment at 1500 ℃ before irradiation, irradiation with 60 keV to a fluence of 2 × 1017 ions/cm2 at room temperature followed by annealing at 1500 ℃.
图 4 TiB2-SiC-Ti(Ti的质量分数为3%)和TiB2-SiC-Ti(Ti的质量分数为6%)烧结样品的X射线衍射图谱
Fig. 4. X-ray diffraction patterns of TiB2-SiC-Ti (the mass fraction of Ti is 3%) and TiB2-SiC-Ti (the mass fraction of Ti is 6%).
图 5 0.5°入射角下TiB2-SiC-Ti(Ti的质量分数为3%) (a) 和TiB2-SiC-Ti(Ti的质量分数为6%) (b) 样品的X射线衍射图谱, 包括原始状态、室温下60 keV, 2 × 1017 ions/cm2 He+ 辐照以及辐照后1500 ℃退火3种条件
Fig. 5. Grazing angle X-ray diffraction patterns of TiB2-SiC-Ti (the mass fraction of Ti is 3%) (a) and TiB2-SiC-Ti (the mass fraction of Ti is 6%) (b) at 0.5° incident angle, including the as-grown, 60 keV, 2 × 1017 ions/cm2 irradiation at room temperature followed by annealing at 1500 ℃
图 6 维氏硬度测试的实测硬度图 (a) TiB2-SiC-Ti(Ti的质量分数为3%); (b) 2 × 1017 ions/cm2 He+室温辐照的TiB2-SiC-Ti(Ti的质量分数为3%); (c) TiB2-SiC-Ti(Ti的质量分数为6%); (d) 2 × 1017 ions/cm2 He+ 室温辐照的TiB2-SiC-Ti(Ti的质量分数为6%)
Fig. 6. Measured hardness diagram of Vickers hardness test: (a) TiB2-SiC-Ti(the mass fraction of Ti is 3%); (b) TiB2-SiC-Ti(the mass fraction of Ti is 3%) irradiated with He+ to a fluence of 2 × 1017 ions/cm2 at room temperature; (c) TiB2-SiC-Ti (the mass fraction of Ti is 6%); (d) TiB2-SiC-Ti (the mass fraction of Ti is 6%) irradiated with He+ to a fluence of 2 × 1017 ions/cm2 at room temperature.
图 7 原始样品的SEM图像 (a) TiB2-SiC-Ti (Ti的质量分数为3%); (b) TiB2-SiC-Ti (Ti的质量分数为6%)
Fig. 7. Scanning electron microscope images of original sample: (a) TiB2-SiC-Ti (the mass fraction of Ti is 3%); (b) TiB2-SiC-Ti (the mass fraction of Ti is 6%).
图 8 维氏硬度测试后压痕处的SEM图像 (a), (c), (e) TiB2-SiC-Ti(Ti的质量分数为3%); (b), (d), (f) TiB2-SiC-Ti(Ti的质量分数为6%)
Fig. 8. Scanning electron microscope image of indentation after Vickers hardness test: (a), (c), (e) TiB2-SiC-Ti (the mass fraction of Ti is 3%); (b), (d), (f) TiB2-SiC-Ti (the mass fraction of Ti is 6%).
图 9 样品的摩擦系数-时间曲线 (a) TiB2-SiC-Ti(Ti的质量分数为3%); (b) TiB2-SiC-Ti(Ti的质量分数为6%)
Fig. 9. The friction coefficient-time curves of the samples: (a) TiB2-SiC-%Ti (the mass fraction of Ti is 3%); (b) TiB2- SiC-Ti (the mass fraction of Ti is 6%).
图 10 样品的磨损位置二维特征线轮廓 (a) TiB2-SiC-Ti(Ti的质量分数为3%); (b) TiB2-SiC-Ti(Ti的质量分数为6%)
Fig. 10. Two-dimensional characteristic line profiles of wear locations of samples: (a) TiB2-SiC-%Ti (the mass fraction of Ti is 3%); (b) TiB2-SiC-Ti (the mass fraction of Ti is 6%).
图 11 样品的磨损位置三维形貌 (a) TiB2-SiC-Ti(Ti的质量分数为3%); (b) TiB2-SiC-Ti(Ti的质量分数为6%)
Fig. 11. Three-dimensional morphologies of wear position of samples: (a) TiB2-SiC-Ti (the mass fraction of Ti is 3%); (b) TiB2- SiC-Ti (the mass fraction of Ti is 6%).
表 1 TiB2-SiC-Ti复合材料中各物质的拉曼峰
Table 1. Raman peaks of various substances in TiB2-SiC-Ti composites.
物质 峰的位置/cm–1 振动模式 TiB2 275, 418 声子振动 TiO2 227 二阶散射峰 446 平面外振动 610 Ti-O拉伸振动 SiO2 708 Si-O拉伸振动 SiC 794, 958 Si-C伸缩振动 C 1345, 1590 面内伸缩振动 
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表 2 TiO2位于610 cm–1处的峰的有效面积
Table 2. The effective area of TiO2 peak at 610 cm–1.
材料 条件 有效
面积面积增
加率/%TiB2-SiC-Ti
(Ti的质量分数为3%)1500 ℃热处理 35209 442 辐照后1500 ℃退火 190919 TiB2-SiC-Ti
(Ti的质量分数为6%)1500 ℃热处理 48570 131 辐照后1500 ℃退火 112214
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表 3 两种Ti含量、相同TiB2晶面指数处的峰强和半高宽
Table 3. Peak intensity and FWHM of samples at the same TiB2 crystal plane index.
晶面指数 (001) (100) (101) (002) (201) (112) TiB2-SiC-Ti
(Ti的质量分数为3%)峰高 696 1624 2708 244 280 240 半高宽 0.163 0.244 0.211 0.287 0.332 0.342 TiB2-SiC-Ti
(Ti的质量分数为6%)峰高 715 1623 2870 295 290 266 半高宽 0.159 0.210 0.211 0.251 0.315 0.334
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表 4 1 kgf载荷下的维氏硬度值
Table 4. Vickers hardness value under 1 kgf load.
样品 HV 误差 硬度变化/% TiB2-SiC-Ti
(Ti的质量分数为3%)290.104 ± 0.03 6.9 TiB2-SiC-Ti
(Ti的质量分数为3%) (辐照)311.489 ± 1.22 TiB2-SiC-Ti
(Ti的质量分数为6%)344.824 ± 17.80 9.2 TiB2-SiC-Ti
(Ti的质量分数为6%) (辐照)379.775 ± 0.62
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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