微波辅助硼热/碳热合成TiB2粉体的保温时间作用机制研究

doi:10.3969/j.issn.1001-1935.2026.01.004

耐火材料 ›› 2026, Vol. 60 ›› Issue (1): 19-24.DOI: 10.3969/j.issn.1001-1935.2026.01.004

微波辅助硼热/碳热合成TiB₂粉体的保温时间作用机制研究

长世伦, 刘振阳, 王兴国, 李欣, 张照磊, 乔佳, 陈滨

江苏大学材料科学与工程学院江苏镇江 212013

收稿日期:2025-03-24 出版日期:2026-02-15 发布日期:2026-02-26
通讯作者: 李欣,女,1991 年生,博士,讲师。E-mail:1000005148@ujs.edu.cn
作者简介:长世伦:男,2000 年生,硕士研究生。E-mail:1320597097@qq.com
基金资助:
^*热还原协同SPS烧结制备TiB₂-Al₂O₃超高温复相陶瓷(江苏大学,X2025102990301)。

Action mechanism of insulation time in microwave-assisted borothermal/carbothermal synthesis of TiB₂ powder

Chang Shilun, Liu Zhenyang, Wang Xingguo, Li Xin, Zhang Zhaolei, Qiao Jia, Chen Bin

First author’s address: School of Materials Science and Engineering,Jiangsu University,Zhenjiang 212013,Jiangsu,China

Received:2025-03-24 Online:2026-02-15 Published:2026-02-26

摘要/Abstract

摘要： 为阐明微波场中保温时间对二硼化钛(TiB₂)粉体合成过程的调控机制,以TiO₂-B₄C-C体系为研究对象,采用微波辅助硼热/碳热耦合还原工艺,在1 450 ℃下系统探究保温时间(10、20、30和40 min)对产物物相组成、显微形貌及粒度分布的演变规律,从而揭示TiB₂晶体的生长机制。结果表明:当保温时间为10 min时,体系存在TiO₂和B₄C的中间反应过程,导致存在TiC和B₂O₃副产物;保温时间延长至20 min,TiC、B₂O₃和C的反应完成,获得纯相TiB₂粉体;保温时间超过30 min后,微波非热效应显著增强,诱发晶粒异常生长及烧结颈形成。较优工艺参数为1 450 ℃保温20 min,制备了d₅₀为0.32 μm的亚微米TiB₂粉体,其晶界清晰且呈规则六方结构。

关键词: TiB₂粉体, 保温时间, 微波加热, 硼热/碳热还原法, 晶体生长

Abstract: To clarify the regulatory mechanism of the insulation time on the synthesis process of titanium diboride (TiB₂) powder in microwave fields,this study took the TiO₂-B₄C-C system as the research object and adopted a microwave-assisted borothermal/carbothermal coupled reduction process to systematically investigate the evolution of the phase composition,morphology and particle size distribution of the products with different insulation time (10,20,30,and 40 min) at 1 450 ℃,thereby revealing the crystal growth mechanism of TiB₂.The results show that:when the insulation time is 10 min,an intermediate reaction process involving TiO₂ and B₄C occurs in the system,resulting in the formation of byproducts TiC and B₂O₃;when the insulation time is extended to 20 min,the reactions of TiC,B₂O₃ and C complete,obtaining pure-phase TiB₂ powder;when the insulation time exceeds 30 min,the microwave non-thermal effect is significantly enhanced,inducing abnormal grain growth and formation of sintering necks.The optimal process parameters are insulation at 1 450 ℃ for 20 min,obtaining submicron TiB₂ powder with d₅₀ of 0.32 μm,which has clear grain boundaries and regular hexagonal structures.

Key words: TiB₂ powder, insulation time, microwave heating, borothermal/carbothermal reduction method, crystal growth

中图分类号:

TQ175

长世伦, 刘振阳, 王兴国, 李欣, 张照磊, 乔佳, 陈滨. 微波辅助硼热/碳热合成TiB₂粉体的保温时间作用机制研究[J]. 耐火材料, 2026, 60(1): 19-24.

Chang Shilun, Liu Zhenyang, Wang Xingguo, Li Xin, Zhang Zhaolei, Qiao Jia, Chen Bin. Action mechanism of insulation time in microwave-assisted borothermal/carbothermal synthesis of TiB₂ powder[J]. Refractories, 2026, 60(1): 19-24.

参考文献

[1] 张珊珊,胡成川.TiB₂基复合材料制备技术研究进展[J].内燃机与配件,2023(5):111-113.
[2] 张智敏,蒋明学,李勇,等.碳热还原法制备硼化钛热力学分析[J].轻金属,2008(11):46-49.
[3] 梁贵生,张芬萍,侯光辉,等.可润湿性硼化钛阴极研究现状[J].世界有色金属,2022(24):168-171.
[4] 宋文杰,钟晖,袁艳,等.真空碳热还原法制备高纯TiB₂粉末[J].稀有金属与硬质合金,2006,34(1):9-13+17.
[5] 杨潘,唐洋洋,王静怡,等.TiB₂粉体制备研究进展[J].当代化工研究,2018(9):89-90.
[6] 吴祖璇,张邦胜,王芳,等.超细粉体制备技术研究[J].中国资源综合利用,2020,38(12):108-112.
[7] 李浩,吴利翔,郭伟明,等.基于B₄C还原法合成亚微米级TiB₂粉体的表征研究[J].热加工工艺,2020,49(20):84-87.
[8] Hwang Y,Lee J K.Preparation of TiB₂ powders by mechanical alloying[J].Materials Letters,2002,54(1):1-7.
[9] Krutskii Y L,Bannov A G,Antonova E V,et al.Synthesis of fine dispersed titanium diboride from nanofibrous carbon[J].Ceramics International,2017,43(3):3212-3217.
[10] 张云,王杰.溶胶-凝胶及碳热还原法制备六角形貌的TiB₂粉末[J].稀有金属,2020,44(4):433-439.
[11] 马爱琼,蒋明学,高云琴,等.对TiB₂合成反应体系的优势区相图叠加分析[J].人工晶体学报,2011,40(2):480-485.
[12] 陈滨,王兴国,李欣,等.TiO₂晶型对微波加热制备TiB₂粉体的影响[J].耐火材料,2024,58(1):44-47+52.
[13] Li X,Chen B,Qiao J,et al.Low-temperature synthesis and sinterability of high-purity submicron TiB₂ powder via microwave-assisted carbothermal reduction[J].Journal of the European Ceramic Society,2024,44(7):4549-4557.
[14] Zhao J L,Lin W,Yamaguchi A,et al.Influence of heating temperature,keeping time and raw materials grain size on Al₄O₄C synthesis in carbothermal reduction process and oxidation of Al₄O₄C[J].Journal of the Ceramic Society of Japan,2007,115(1346):654-660.
[15] Huan Y,Wang X H,Fang J,et al.Grain size effect on piezoelectric and ferroelectric properties of BaTiO₃ ceramics[J].Journal of the European Ceramic Society,2014,34(5):1445-1448.
[16] Chen Y,Ye H H,Wang X S,et al.Grain size effects on the electric and mechanical properties of submicro BaTiO₃ ceramics[J].Journal of the European Ceramic Society,2020,40(2):391-400.
[17] Aziz M J,Nygren E,Hays J F,et al.Crystal growth kinetics of boron oxide under pressure[J].Journal of Applied Physics,1985,57(6):2233-2242.
[18] Behrens M A,Franzén A,Carlert S,et al.On the Ostwald ripening of crystalline and amorphous nanoparticles[J].Soft Matter,2025,21(12):2349-2354.
[19] Conry B,Harley J B,Tonks M R,et al.Engineering grain boundary anisotropy to elucidate grain growth behavior in alumina[J].Journal of the European Ceramic Society,2022,42(13):5864-5873.
[20] Gao M,Wen D D,Cao G Q,et al.Study the growth mechanism of AgNi nanoparticles by surface diffusion[J].Applied Surface Science,2023,640:158286.
[21] Lupi L,Hudait A,Molinero V.Heterogeneous nucleation of ice on carbon surfaces[J].Journal of the American Chemical Society,2014,136(8):3156-3164.

微波辅助硼热/碳热合成TiB₂粉体的保温时间作用机制研究

Action mechanism of insulation time in microwave-assisted borothermal/carbothermal synthesis of TiB₂ powder

PDF

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价

[1]	王兴国, 徐晨, 长世伦, 张照磊, 李欣, 陈滨. 原料预处理对制备TiB₂粉体的影响[J]. 耐火材料, 2025, 59(6): 506-510.
[2]	王得憬, 王文武, 叶国田, 曹喜营, 王自强, 周玉栋. 水热合成工艺对硬硅钙石纤维制备及显微形貌的影响[J]. 耐火材料, 2025, 59(3): 192-197.
[3]	彭杰, 刘江昊, 张海军. 硼热/碳热还原法制备过渡金属二硼化物研究进展[J]. 耐火材料, 2025, 59(2): 170-176.
[4]	王兴国, 陈滨, 李欣, 长世伦, 徐晨, 杨建红. 以蔗糖为碳源制备亚微米级TiB₂粉体的研究[J]. 耐火材料, 2024, 58(5): 405-409.
[5]	陈滨, 王兴国, 李欣, 吴纪清, 唐健, 杨建红. TiO₂晶型对微波加热制备TiB₂粉体的影响[J]. 耐火材料, 2024, 58(1): 44-47.
[6]	刘鹏程, 茆忠军, 遇龙, 赵嘉亮, 谢志鹏. 莫来石轻质骨料的制备及性能研究[J]. 耐火材料, 2023, 57(6): 491-494.
[7]	麦海香, 赵飞, 安建成, 王亚利, 连伟康胡杨, 葛铁柱, 刘新红. 热处理温度对矾土基莫来石材料结构及晶体生长的影响[J]. 耐火材料, 2023, 57(4): 314-319.
[8]	董开朝,高帅波,崔晓华,李欣,姜胜南,金星,邢鹏飞. 保温时间对碳热还原法制备B4C的影响[J]. , 2019, 53(3): 207-210.
[9]	宋云飞，王少华，邓承继，祝洪喜. 氮化保温时间对原位合成AlON结合MgAl2O4-C耐火材料的影响[J]. , 2017, 51(3): 181-185.
[10]	牟善浩刘永杰时亚祺邹晓东文川程云. 热处理制度对Al2O3-SiC质低水泥浇注料性能的影响[J]. , 2015, 49(5): 365-368.
[11]	姚义俊,万韬瑜,刘斌,张乐彬,李军. 烧成制度对AlN陶瓷性能及显微结构的影响[J]. , 2014, 48(6): 417-420.
[12]	王朔1),余俊1,2),赵惠忠1,2),李超1),王斌斌1),段连威1). 微波辅助溶液燃烧法制备MgAl2O4粉体[J]. , 2014, 48(6): 421-423.
[13]	王婷杨道媛袁斐冯晓聪屈源超. 微晶β-SiAlON材料的制备[J]. , 2013, 47(6): 414-417.
[14]	刘小林，刘开琪，谢笑虎，刘永锋，罗志勇. 保温时间对反应烧结合成CA6性能和显微结构的影响[J]. , 2012, 46(5): 330-0.
[15]	林少杰，吴一，邹正光. 添加AlN-Y2O3-La2O3烧结助剂的c-BN–β-Si3N4复合材料的超高压烧结[J]. , 2012, 46(3): 197-0.