Effects of different aluminum sources and calcination temperatures on the synthesis of ultrafine AlN powder via carbothermal reduction nitridation
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AlN ultrafine powder was synthesized in N2 via carbothermal reduction nitridation with different aluminum sources (i.e.,Al(OH)3, Al(NO3)3·9H2O, and α-Al2O3) and high-activity nanocarbon black as raw materials. The effects of differentaluminum sources, aluminum dosage, and calcination temperature on the phase composition and microstructure of thesynthesized AlN powder were studied. Thermodynamic analysis of the reaction process was performed and the reactionmechanism of AlN powder was discussed. Results showed that fully nitrided phase-pure AlN powder was synthesized afterincubating the precursor powder samples at 1500 oC for 2 hrs with Al(OH)3 or Al(NO3)3·9H2O as the aluminum source. Ata 1 : 5 molar ratio of Al2O3/C, a weak Al2O3 diffraction peak was present in the AlN powder samples that were synthesizedat 1550 oC with α-Al2O3 as the aluminum source. The quality of AlN powder samples that were synthesized withAl(NO3)3·9H2O as the aluminum source was optimal relative to those of AlN powder samples that were synthesized with thetwo other aluminum sources. Flake-like particles (~ 100-300 nm) in the powder samples exhibited reduced agglomeration. Moreover, approximately spherical structures that were 0.5-1.0 μm in size formed between the flake-like particles. Duringcarbothermal reduction nitriding, Al2O3 in the raw material first underwent carbothermal reduction to produce metallicaluminum vapor and aluminum low valence gas oxides (Al2O), and then underwent further nitriding to form AlN.
Abstract
AlN ultrafine powder was synthesized in N2 via carbothermal reduction nitridation with different aluminum sources (i.e.,Al(OH)3, Al(NO3)3·9H2O, and α-Al2O3) and high-activity nanocarbon black as raw materials. The effects of differentaluminum sources, aluminum dosage, and calcination temperature on the phase composition and microstructure of thesynthesized AlN powder were studied. Thermodynamic analysis of the reaction process was performed and the reactionmechanism of AlN powder was discussed. Results showed that fully nitrided phase-pure AlN powder was synthesized afterincubating the precursor powder samples at 1500 oC for 2 hrs with Al(OH)3 or Al(NO3)3·9H2O as the aluminum source. Ata 1 : 5 molar ratio of Al2O3/C, a weak Al2O3 diffraction peak was present in the AlN powder samples that were synthesizedat 1550 oC with α-Al2O3 as the aluminum source. The quality of AlN powder samples that were synthesized withAl(NO3)3·9H2O as the aluminum source was optimal relative to those of AlN powder samples that were synthesized with thetwo other aluminum sources. Flake-like particles (~ 100-300 nm) in the powder samples exhibited reduced agglomeration. Moreover, approximately spherical structures that were 0.5-1.0 μm in size formed between the flake-like particles. Duringcarbothermal reduction nitriding, Al2O3 in the raw material first underwent carbothermal reduction to produce metallicaluminum vapor and aluminum low valence gas oxides (Al2O), and then underwent further nitriding to form AlN.
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