两步烧结法对AlN原料提纯工艺的研究

doi:10.19964/j.issn.1006-4990.2024-0367

摘要/Abstract

摘要：

氮化铝（AlN）晶体作为超宽禁带半导体材料的代表之一，具有大的禁带宽度、高热导率、高的击穿场强等优异性质，在深紫外光电器件和大功率电子器件等领域具有重要的应用。在氮化铝晶体的生长过程中，AlN原料中的O、C含量过高导致晶体内部缺陷浓度过高或者生长多晶，从而会影响生长后的AlN单晶质量。该研究提出一种两步烧结工艺对AlN原料进行提纯，并使用扫描电子显微镜（SEM），氧氮氢气体分析仪、碳硫气体分析仪对烧结后的样品进行表征。SEM结果表明，AlN粉末的粒径从1~3 μm增加到100 μm左右，比表面积减小，降低了O杂质的吸附，并且烧结之后的AlN粉末颗粒具有良好的结晶性。氧氮氢气体分析仪、碳硫气体分析仪结果表明，O元素杂质含量从7 900 μg/g降低至640 μg/g，C元素杂质从420 μg/g降低至57 μg/g。综上所述，两步烧结工艺是控制AlN粉末比表面积的有效途径，能够有效去除AlN中的O、C等杂质，提高了AlN原料的结晶质量，为高质量AlN晶体生长奠定基础。

关键词: AlN原料, 提纯, 烧结工艺, O杂质, C杂质

Abstract:

Aluminum nitride（AlN） crystal，as one of the representatives of ultra-wideband semiconductor materials，has excellent properties such as large bandwidth，high thermal conductivity，and high breakdown field strength，which has important applications in the fields of deep-ultraviolet optoelectronic devices and high-power electronic devices.During the growth process of AlN crystals，the high O and C content in the AlN source material lead to the high concentration of defects inside the crystals or the growth of polycrystals，which will affect the quality of the AlN single crystals.In this paper，a two-step sintering process was proposed to purify the AlN source material，and the sintered samples were characterized by scanning electron microscope（SEM）、oxygen，nitrogen，and hydrogen gas analyzer、carbon and sulfur gas analyzer.The SEM results showed that the particle size of the AlN powder was increased from 1~3 μm to about 100 μm，the specific surface area was reduced，and the adsorption of the O impurities was reduced，and the sintered AlN particles had good crystallinity.The results of oxygen，nitrogen and hydrogen gas analyzer、carbon and sulfur gas analyzer showed that the O impurity content was reduced from 7 900 μg/g to 640 μg/g，and the C impurity was reduced from 420 μg/g to 57 μg/g.In summary，the two-step sintering process was an effective way to control the specific surface area of the AlN source material，which was capable of effectively removing the O，C and other impurities in the AlN source material，and improved the crystalline quality of the AlN source material，laying a foundation for the growth of high-quality AlN crystal.

Key words: AlN source material, purification, sintering process, oxygen impurities, carbon impurities

中图分类号:

TQ133.1

吕令爽, 曹文豪, 俞瑞仙, 王守志, 王国栋, 朱亚军, 杜家宸, 徐现刚, 张雷. 两步烧结法对AlN原料提纯工艺的研究[J]. 无机盐工业, 2024, 56(12): 51-55.

LÜ Lingshuang, CAO Wenhao, YU Ruixian, WANG Shouzhi, WANG Guodong, ZHU Yajun, DU Jiachen, XU Xiangang, ZHANG Lei. Research on purification process of AlN source material by two-step sintering method[J]. Inorganic Chemicals Industry, 2024, 56(12): 51-55.

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样品	C含量/（μg·g^-1）	O含量/（μg·g^-1）
初始样品	420	7 900
样品1	100	820
样品2	57	640
样品3	240	790

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