Synthesis of Fine AlN Powders by Foamed Precursor-assisted Carbothermal Reduction-nitridation Method

doi:10.15541/jim20190055

Abstract

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

CLC Number:

TQ174

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.

Figures/Tables 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 ℃

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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