中国科学院合肥物质科学研究院固体物理研究所,合肥,230031
纸质出版:2025
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王振,胡晨光,李可为,胡梦恩,张瀚文,黄竹林,胡小晔. 晶种法合成硼化铪粉体及其生长机理研究[J]. 航空制造技术, 2025, 68(3): 84-91.
WANG Zhen, HU Chenguang, LI Kewei, HU Mengen, ZHANG Hanwen, HUANG Zhulin, HU Xiaoye. Synthesis and Growth Mechanism Research of HfB2 Powders Prepared by Crystal Seed-Mediated Method[J]. Aeronautical Manufacturing Technology, 2025, 68(3): 84-91.
王振,胡晨光,李可为,胡梦恩,张瀚文,黄竹林,胡小晔. 晶种法合成硼化铪粉体及其生长机理研究[J]. 航空制造技术, 2025, 68(3): 84-91. DOI: 10.16080/j.issn1671-833x.2025.03.084.
WANG Zhen, HU Chenguang, LI Kewei, HU Mengen, ZHANG Hanwen, HUANG Zhulin, HU Xiaoye. Synthesis and Growth Mechanism Research of HfB2 Powders Prepared by Crystal Seed-Mediated Method[J]. Aeronautical Manufacturing Technology, 2025, 68(3): 84-91. DOI: 10.16080/j.issn1671-833x.2025.03.084.
硼化铪(HfB
2
)超高温陶瓷因其高熔点、高抗氧化性和优异的耐腐蚀性成为热防护领域的最佳候选材料之一,而研制粒径可控的陶瓷粉体对其应用至关重要。以氧化铪(HfO
2
)、氧化硼(B
2
O
3
)和活性碳(C)为原料,通过晶种辅助的硼/碳热还原法合成了高纯HfB
2
陶瓷粉体,研究了晶种粒径对陶瓷粉体粒径的影响规律,探究了晶种法合成HfB
2
粉体的生长机制。通过X 射线衍射分析粉体物相、扫描电子显微镜观察粉体形貌,并测定粉体中C、O 杂质的含量。结果表明,晶种辅助的硼/ 碳热还原反应合成HfB
2
粉体的最佳反应温度约为1500 ℃,保温1 h即可获得纯相HfB
2
。通过调控初始晶种粒径,制备的HfB
2
陶瓷粉体平均粒径在1.08~2.33 μm之间,且粉体粒径随晶种粒径的增大而增大。激光粒度分析表明,添加晶种大幅提高了陶瓷粉体的分散性且促进了粒径的窄分布。此外,试验确定了HfB
2
陶瓷粉体的生长过程分为两个阶段:首先晶种HfB
2
表面被HfO
2
晶粒包覆,HfO
2
晶粒表层形成较小的HfB
2
晶粒;再通过碳和硼的传质由外到内实现HfO
2
到HfB
2
的转化。
Hafnium boride (HfB
2
) ultra-high temperature ceramics have become one of the best candidate materials in the field of thermal protection due to their high melting point
high oxidation resistance and excellent corrosion resistance. The fabrication of ceramic powders with precisely controlled particle sizes is paramount for their effective application. Highpurity HfB
2
ceramic powders were prepared by crystal seed-mediated bor
o/carbothermal reduction method using hafnium oxide (HfO
2
)
boron trioxide (B
2
O
3
)
and carbon (C) powders as raw materials. The influence of crystal seed size on the particle size of HfB
2
powders was studied
and the growth mechanism of HfB
2
powders synthesized by crystal seed-mediated method was explored. Phase and morphology of the obtained powders were analyzed and observed by X-ray diffraction and scanning electron microscope; the contents of C and O impurities in the powders were measured as well. The results show that the optimal reaction temperature for synthesizing pure HfB
2
powders by crystal seed-mediated boro/carbothermal reduction is approximately 1500 ℃ (holding for 1 h). HfB
2
ceramic powders with average particle size of 1.08–2.33 μm were obtained by controlling the initial crystal seed size. Generally
the particle size of HfB
2
increases with the increase of crystal seed size
and laser particle size measurements indicate that the addition of crystal seeds improves the dispersibility and narrows distribution of HfB
2
particle size. It is confirmed that the growth process of HfB
2
ceramic powders is divided into two stages: the cladding of HfO
2
grains on HfB
2
surface with formation of tiny HfB
2
grains
and conversion of HfO
2
to HfB
2
through mass diffusion of carbon and boron from the outside to the inside of HfO
2
particles.
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