碳热还原氮化法结合泡沫前驱体制备超细氮化铝粉体

doi:10.15541/jim20190055

摘要/Abstract

摘要：

本研究使用改良的碳热还原氮化法合成超细氮化铝粉体。以γ氧化铝和蔗糖作为铝源和碳源, 先预处理制备成多孔泡沫, 再通过碳热还原氮化法合成氮化铝粉体。反应过程和产物通过X射线衍射分析、SEM和TEM确定。X射线衍射分析表明整个反应过程不存在氧化铝的相转变。高分辨透射电子显微镜显示γ-Al₂O₃颗粒被无定型碳包裹, 从而抑制了γ-Al₂O₃到α-Al₂O₃的相转变。泡沫的多孔结构促进了氮气的扩散和反应副产物的释放, 使得最低反应温度降低至1450 ℃。SEM结果表明得到的氮化铝颗粒粒径大约为50 nm。本研究合成的氮化铝粉体可用于制备高热导氮化铝陶瓷。

关键词: 氮化铝, 泡沫, 粉体, 合成

Abstract:

A modified carbothermal reduction-nitridation (CRN) method was proposed to synthesize fine AlN particles using γ-Al₂O₃ and sucrose as raw materials which were pre-treated as cellular foams. The reaction procedure and the produced AlN were investigated by XRD, SEM and TEM. XRD result suggests that γ-Al₂O₃ transferred into AlN without transformation into α-Al₂O₃. HRTEM shows that γ-Al₂O₃ particles are covered by amorphous carbon from sucrose inhibiting the transformation of α-Al₂O₃ from γ-Al₂O₃ in the synthesis procedure. The foamed structure is of benefit to the diffusion of N₂ and the produced CO. The minimum reaction temperature is 1450 ℃ for full conversion of Al₂O₃ to AlN. SEM photographs show the particle size of synthesized AlN is 50 nm. This study demonstrated an efficient way to synthesize fine AlN powders which are urgently required for the manufacture of advanced AlN ceramics.

Key words: aluminum nitride, foams, particles, synthesis

中图分类号:

TQ174

茅茜茜, 徐勇刚, 毛小建, 张海龙, 李军, 王士维. 碳热还原氮化法结合泡沫前驱体制备超细氮化铝粉体[J]. 无机材料学报, 2019, 34(10): 1123-1127.

MAO Xi-Xi, XU Yong-Gang, MAO Xiao-Jian, ZHANG Hai-Long, LI Jun, WANG Shi-Wei. Synthesis of Fine AlN Powders by Foamed Precursor-assisted Carbothermal Reduction-nitridation Method[J]. Journal of Inorganic Materials, 2019, 34(10): 1123-1127.

图/表 7

Fig. 1 DTA and TG analysis of sucrose pyrolysis procedure from room temperature to 1000 ℃ in N2 atmosphere

Fig. 2 SEM images of the foam heated at (a) 1000 and (b) 1550 ℃ with sucrose/Al2O3 ratio of 2.0

Fig. 3 XRD patterns of the sucrose/Al2O3 powders synthesized at different temperatures

Fig. 4 TEM images of particles heated at different temperatures (a) 1250 ℃; (b) 1350 ℃; (c) 1450 ℃; (d) 1550 ℃

Fig. 5 (a) HRTEM image of particles synthesized at 1250 ℃ and (b) selective electron diffraction pattern

Fig. 6 SEM photographs of the AlN powders synthesized at different temperatures for 2 h (a) 1450 ℃; (b) 1500 ℃; (c) 1550 ℃; (d) 1600 ℃

Table 1 Nitrogen and oxygen content of AlN powders with various sucrose/Al2O3 ratios and synthesizing at 1550 ℃

Element content/wt%	Sucrose/Al₂O₃
Element content/wt%	2.0	2.5	3.0
Nitrogen	29.3	29.4	30.2
Oxygen	2.4	2.0	1.6

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