二硼化锆粉体合成研究现状与展望

doi:10.11896/cldb.20070327

材料导报

2021, Vol. 35

Issue (21): 21159-21168 https://doi.org/10.11896/cldb.20070327

无机非金属及其复合材料

二硼化锆粉体合成研究现状与展望

骆吉源, 肖国庆, 丁冬海, 种小川, 任金翠

西安建筑科技大学材料科学与工程学院,西安 710055

Research Status and Prospect of Synthesis of Zirconium Diboride Powders

LUO Jiyuan, XIAO Guoqing, DING Donghai, CHONG Xiaochuan, REN Jincui

College of Materials Science and Engineering, Xi'an University of Architecture and Technology, Xi'an 710055, China

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摘要二硼化锆(ZrB₂)陶瓷的优异性能使其作为航空航天推进系统结构材料的潜力巨大。然而,其分子中的强共价键和低晶界扩散速率使ZrB₂烧结致密化困难,且ZrB₂陶瓷固有脆性大、对裂纹较为敏感、服役可靠性不高,限制了ZrB₂的应用。通过合成性质优良的粉体促进ZrB₂陶瓷烧结致密化、改善其固有脆性具有重要现实意义。
减小粉体粒径、降低氧杂质含量是促进ZrB₂烧结致密化的关键。此外,高长径比一维粉体可有效提高基体的强韧性。因此,超细、低氧含量和一维ZrB₂粉体合成是近年来ZrB₂粉体合成领域的研究热点。
合成反应原理及制备工艺决定了ZrB₂粉体的性质。超细粉体的合成关键在于降低反应温度,优化现有反应体系具有一定成效但限制较大,通过新反应体系可在低温下合成粒径为25~35 nm的超细粉体;ZrB₂中氧杂质主要是未完全反应的ZrO₂,使反应物适度过量可有效提高反应进行程度,氧杂质含量可降至0.14%(质量分数);原位合成的一维ZrB₂粉体长径比不高,高长径比纤维仍主要通过静电纺丝工艺制备,但纤维产率较低,因此原位合成高长径比ZrB₂粉体仍是一大挑战。
本文分析了元素合成、碳热还原、硼热还原、硼/碳热还原、镁热还原及铝热还原合成ZrB₂粉体的反应过程与原理;总结了自蔓延高温合成法、熔盐法、机械合金化、溶胶凝胶法和静电纺丝法等制备工艺的优缺点;综述了ZrB₂在超细、低氧含量及一维粉体合成三个方向的最新进展;分析了在ZrB₂粉体合成过程中影响粒径、氧杂质含量的因素及晶体生长机制,并对未来ZrB₂粉体合成研究进行了展望。

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	骆吉源
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	任金翠

关键词: 二硼化锆合成原理制备工艺发展方向

Abstract: Zirconium diboride (ZrB₂) ceramics have been proved to be a promising structural material in aerospace propulsion system owing to its remarkable properties. However, the application of ZrB₂ is hindered to a great extent due to the difficulty to be densified, sensitivity to cracks and poor service reliability because of its strong covalent bonds in the molecules and low grain boundary diffusion rate. Hence, it is important to synthesize high-quality ZrB₂ powders with excellent properties to promote its sintering densification and overcome its inherent brittleness.
The activity of ZrB₂ powders is influenced by the particle size and oxygen impurity content. In addition, with the incorporation of powders with high aspect ratio, a higher strength and toughness can be achieved for ZrB₂ ceramics. Thus, the synthesis of ultra-fine, low-oxygen content and one-dimensional ZrB₂ powders has attracted plenty of interest.
Thermodynamic and kinetic principles in synthesis as well as preparation technologies have great effects on the quality of ZrB₂ powders. It is essential to lower the reaction temperature in the synthesis of ultra-fine ZrB₂ powders. Optimization of existing reaction systems is effective but there are many limitations. Nano ZrB₂ powders with particle size 25—35 nm can be obtained under a lower temperature in a new system. The oxygen impurity in ZrB₂ powders is mainly the unreacted ZrO₂ and it can be effectively reduced to 0.14%(mass fraction) by introducing excessive reactants appropriately. In-situ synthesizing ZrB₂ powders with high aspect ratio is still a challenge and continuous fibers are still mainly prepared by electrospinning.
The processes and reaction mechanisms of ZrB₂ powders synthesis were reviewed, including element synthesis, carbothermal reduction, borothermal reduction, boro/carbothermal reduction, magnesiothermic reduction and aluminothermic reduction. The advantages and disadvantages of self-propagating high temperature synthesis, molten salt method, mechanical alloying, sol-gel method and electrospinning were overviewed. The latest developments of ZrB₂ powders synthesis were introduced from the aspects of ultra-fine, low-oxygen content and one-dimensional powders preparation. The factors affecting the particle size and oxygen content as well as the crystal growth mechanism were analyzed. Finally, the studies on the synthesis of ZrB₂ powders were prospected.

Key words: zirconium diboride synthesis mechanism preparation technology development direction

出版日期: 2021-11-10 发布日期: 2021-11-30

ZTFLH:

TQ174.75

基金资助: 国家自然科学基金(51502236;51572212;51772236);陕西省重点研发计划项目(2018ZDXM-GY-128)

通讯作者: xiaoguoqing@xauat.edu.cn

作者简介: 骆吉源,2018年毕业于西安建筑科技大学,获得工学学士学位。现为西安建筑科技大学材料科学与工程学院博士研究生,在肖国庆教授指导下进行研究。目前主要研究领域为模板法制备二硼化锆纤维。
肖国庆,西安建筑科技大学材料科学与工程学院教授,博士研究生导师,2005年获西安交通大学材料科学与工程专业博士学位,2005年晋升教授,2008.10-2009.10英国谢菲尔德大学访问学者。主要从事结构功能一体化陶瓷基复合材料、低碳耐火材料研究,以第一作者及合作者在国内外期刊发表学术论文100多篇。目前主持国家级科研项目2项、省部级科研项目5项,受邀担任Composites A、Ceramics International、International Journal of the Applied Ceramic Technology等10余种国际期刊审稿人。

引用本文:

骆吉源, 肖国庆, 丁冬海, 种小川, 任金翠. 二硼化锆粉体合成研究现状与展望[J]. 材料导报, 2021, 35(21): 21159-21168.
LUO Jiyuan, XIAO Guoqing, DING Donghai, CHONG Xiaochuan, REN Jincui. Research Status and Prospect of Synthesis of Zirconium Diboride Powders. Materials Reports, 2021, 35(21): 21159-21168.

链接本文:

http://www.mater-rep.com/CN/10.11896/cldb.20070327 或 http://www.mater-rep.com/CN/Y2021/V35/I21/21159

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