Effect of Ti content on preparation and properties of TiB<sub>2</sub>-SiC-Ti materials

He Xiao-Xun; Li Bing-Sheng; Liu Rui; Zhang Tong-Min; Cao Xing-Zhong; Chen Li-Ming; Xu Shuai

doi:10.7498/aps.71.20220530

Abstract

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:

Authors and contacts

1.
State Key Laboratory of Environment-Friendly Energy Materials, Southwest University of Science and Technology, Mianyang 621010, China
2.
Institute of Solid State Physics, Chinese Academy of Sciences, Hefei 230000, China
3.
Institute of Modern Physics, Chinese Academy of Sciences, Lanzhou 730000, China
4.
Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China
5.
School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, China

Corresponding author: Li Bing-Sheng, libingshengmvp@163.com

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 12075194).

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References

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Cited By

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

Figure 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

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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

Figure 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).

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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

Figure 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 ℃.

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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

Figure 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%).

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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

Figure 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 × 10¹⁷ions/cm² irradiation at room temperature followed by annealing at 1500 ℃

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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%)

Figure 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.

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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%)

Figure 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%).

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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%)

Figure 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%).

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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%)

Figure 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%).

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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%)

Figure 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%).

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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%)

Figure 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%).

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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
TiB₂-SiC-Ti (Ti的质量分数为3%)	辐照后1500 ℃退火	190919	442
TiB₂-SiC-Ti (Ti的质量分数为6%)	1500 ℃热处理	48570	131
TiB₂-SiC-Ti (Ti的质量分数为6%)	辐照后1500 ℃退火	112214	131

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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
TiB₂-SiC-Ti (Ti的质量分数为3%)	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
TiB₂-SiC-Ti (Ti的质量分数为6%)	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	6.9
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	9.2

DownLoad: CSV

map

[1]	Stacey Jr W M, Abdou M A, Bertoncini P J, Bolta C C, Brooks J N, Evans K, Fasolo J A, Jung J C, Kustom R L, Maroni A, Mattas R F, Monich J S, Moretti A, Mills F E, Misra B, Norem J H, Patten J S, Praeg W F, Smelser P, Smith D L, Stevens H C, Turner L, Wang S T, Youngdahl C K 1976 Proceedings of the Second Topical Meeting on “The Technology of Controlled Nuclear Fusion” Richland, 1976 p21
[2]	Kaminsky M 1976 Proceedings of the Second Topical Meeting on “The Technology of Controlled Nuclear Fusion” Richland, 1976 p169
[3]	Rossing T D, Das S K, Kaminsky M 1977 J. Vac. Sci. Technol. 14 550 Google Scholar
[4]	Mattox D M 1978 First Wall Coating Workshop Report Sandia Laboratories, Albuquerque, 1978 p1
[5]	Boutard J L, Alamo A, Lindau R, Rieth M 2008 CR. Phys. 9 287 Google Scholar
[6]	Zhao G L, Huang C Z, Liu H L, Zou B, Zhu H T, Wang J 2014 Mater. Sci. Eng. A 606 108 Google Scholar
[7]	Bhattacharya A, Parish C M, Koyanagi T, Petrie C M, King D, Hilmas G, Fahrenholtz W G, Zinkle S J, Katoh Y 2019 Acta Mater. 165 26 Google Scholar
[8]	Istgaldi H, Nayebi B, Ahmadi Z, Shahi P, Asl M S 2020 Ceram. Int. 46 23155 Google Scholar
[9]	Konigshofer R, Furnsinn S, Steinkellner P 2005 Int. J. Refract. Met. H. 23 350 Google Scholar
[10]	Murthy T S R C, Balasubramaniam R, Basu B, Suri A K, Mungole M N 2006 J. Eur. Ceram. Soc. 26 187 Google Scholar
[11]	Asl M S, Kakroudi M G, Kondolaji R A, Nasiri H 2015 Ceram. Int. 41 5843 Google Scholar
[12]	Germi M D, Mahaseni Z H, Ahmadi Z, Asl M S 2018 Mater. Charact. 145 225 Google Scholar
[13]	Namini A S, Motallebzadeh A, Nayebi B, Asl M S, Azadbeh M 2019 Mater. Chem. Phys. 223 789 Google Scholar
[14]	Mahaseni Z H, Germi M D, Ahmadi Z, Asl M S 2018 Ceram. Int. 44 13367 Google Scholar
[15]	Nguyen V H, Asl M S, Mahaseni Z H, Germi M D, Delbari S A, Le Q V, Ahmadi Z, Shokouhimehr M, Namini A S, Mohammadi M 2020 Ceram. Int. 46 25341 Google Scholar
[16]	Ahmadi Z, Nayebi B, Asl M S, Farahbakhsh I, Balak Z 2018 Ceram. Int. 44 11431 Google Scholar
[17]	Zou B, Huang C Z, Song J P, Liu Z Y, Liu L, Zhao Y 2012 Mater. Sci. Eng. A 540 235 Google Scholar
[18]	Song J P, Huang C Z, Lv M, Zou B, Wang S Y, Wang J, An J 2014 Mater. Sci. Eng. A 605 137 Google Scholar
[19]	Chlup Z, Baca L, Halasova M, Neubauer E, Hadraba H, Stelzer N, Roupcova P 2015 J. Eur. Ceram. Soc. 35 2745 Google Scholar
[20]	Zhang Z H, Shen X B, Wang F C, Lee S K, Fan Q B, Cao M S 2012 Scripta Mater. 66 167 Google Scholar
[21]	Mukhopadhyay A, Raju G B, Basu B, Suri A K 2009 J. Eur. Ceram. Soc. 29 505 Google Scholar
[22]	Asl M S, Namini A S, Kakroudi M G 2016 Ceram. Int. 42 5375 Google Scholar
[23]	Murthy T S R C, Subramanian C, Fotedar R K, Gonal M R, Sengupta P, Kumar S, Suri A K 2009 Int. J. Refract. Met. H. 27 629 Google Scholar
[24]	Li M, Zhou X B, Yang H, Du S Y, Huang Q 2018 Scripta Mater. 143 149 Google Scholar
[25]	He Q L, Tian S, Xie J J, Xiang C L, Wang H, Wang W M, Fu Z Y 2020 J. Eur. Ceram. Soc. 40 2862 Google Scholar
[26]	Kovalcikova A, Tatarko P, Sedlak R, Medved D, Chlup Z, Mudra E, Dusza J 2020 J. Eur. Ceram. Soc. 40 4860 Google Scholar
[27]	Singlard M, Tessier-Doyen N, Chevallier G, Oriol S, Fiore G, Vieille B, Estournes C, Vardelle M, Rossignol S 2018 Ceram. Int. 44 22357 Google Scholar
[28]	Zou B, Ji W B, Huang C Z, Xu K T, Li S S 2014 Int. J. Refract. Met. H. 47 1 Google Scholar
[29]	Cai X Q, Wang D P, Wang Y, Yang Z W 2021 J. Manuf. Processes 64 1349 Google Scholar
[30]	Wang Y, Liu Q, Zhang B, Zhang H Q, Jin Y C, Zhong Z X, Ye J, Ren Y H, Ye F, Wang W 2021 Ceram. Int. 47 10665 Google Scholar
[31]	Song B, Yang W, Liu X M, Chen H Y, Akhlaghi M 2021 Ceram. Int. 47 29174 Google Scholar
[32]	Zhao B, Zhao Y Q, Hou Z M, Luo Y Y, Zhang W, Zhang P X, Wu J P 2018 Fusion Eng. Des. 137 405 Google Scholar
[33]	Vajdi M, Moghanlou F S, Ahmadi Z, Motallebzadeh A, Asl M S 2019 Ceram. Int. 45 8333 Google Scholar
[34]	Tatarko P, Grasso S, Kovalcikova A, Medved D, Dlouhy I, Reece M J 2020 J. Eur. Ceram. Soc. 40 1111 Google Scholar
[35]	Iltis X, Lefebvre F, Lemaignan C 1995 J. Nucl. Mater. 224 109 Google Scholar
[36]	Garner A, Baxter F, Frankel P, Topping M, Harte A, Slater T, Tejland P, Romero J, Darby E, Cole-Baker A, Gass M, Preuss M 2018 Zirconium in the Nuclear Industry: 18 th International Symposium West Conshohocken, 2018 p491
[37]	Wang J, Ren D L, Chen L L, Man G A, Zhang H Y, Zhang H P, Luo L H, Li W P, Pan Y B, Gao P F, Zhu Y B, Wang Z G 2020 J. Nucl. Mater. 539 152275 Google Scholar
[38]	Bhattacharya A, Parish C M, Koyanagi T, Petrie C M, King D, Hilmas G, Fahrenholtz W G, Zinkle S J, Katoh Y 2019 Acta Materialia 165 26
[39]	Golanski G, Purzynska H 2022 Int. J. Pres. Ves. Pip. 195 104574 Google Scholar
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Effect of Ti content on preparation and properties of TiB₂-SiC-Ti materials

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Effect of Ti content on preparation and properties of TiB2-SiC-Ti materials

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Effect of Ti content on preparation and properties of TiB₂-SiC-Ti materials