( 1. 北京科技大學(xué) 材料科學(xué)與工程學(xué)院，北京 100083；
2. 天津理工大學(xué) 材料科學(xué)與工程學(xué)院， 天津 300191；
3. 中南大學(xué) 粉末冶金國家重點實驗室， 長沙 410083)
摘 要: 以硝酸鋁和碳黑為原料， 利用化學(xué)沉淀法制備出混合均勻的Al2O3+C前驅(qū)物，并以該前驅(qū)物為原料采用碳熱還原法制備了AlN粉末。 研究了氮化反應(yīng)溫度、 pH值、 表面活性劑、 溶液濃度、 氮?dú)饬髁亢吞间X比等工藝參數(shù)對氮化反應(yīng)的影響， 得出的最佳工藝參數(shù)分別為: 以0.4 mol/L的硝酸鋁溶液和比表面積為156 m2/g的碳黑為原料， 控制原料中碳鋁比為3∶1， 添加適量的硬脂酸（SA）和聚乙二醇（PEG）作為表面活性劑， 控制沉淀過程中pH=9， 通過共沉淀工藝得到分散性好、團(tuán)聚程度小的前驅(qū)物， 并將此前驅(qū)物在常壓和氮?dú)饬髁繛? L/min的條件下于1 550 ℃煅燒4 h，最后將反應(yīng)產(chǎn)物在650 ℃的空氣中除碳4 h， 制備出氮含量為33.20%， 氧含量為0.98%， 比表面積為4.26 m2/g的AlN粉末。
關(guān)鍵字: AlN粉末； 沉淀前驅(qū)物； 碳熱還原
precipitated precursor
（ 1. School of Materials Science and Engineering,
University of Science and Technology Beijing, Beijing 100083, China;
2. School of Materials Science and Engineering,
Tianjin University of Technology, Tianjin 300191, China;
3. State Key Laboratory of Powder Metallurgy,
Central South University, Changsha 410083, China）
Abstract: A homogenous mixture precursor of Al2O3+C was prepared by the chemical precipitation method and AlN powders were fabricated by carbon thermal reduction nitridation of the precipitated precursor. The effect factors on the nitridation conditions and the properties of AlN powders, including nitridation temperature, pH value, surface active agent, solution concentration, N2 flow rate and molar ratio of carbon to aluminum, were investigated. An optimal process was obtained through synthesizing fine and pure AlN powders. Firstly, a homogenous and good dispersion precursor was prepared by the precipitation process using 0.4 mol/L Al(NO3)3 solution and 156 m2/g carbon black as materials at pH=9, the molar ratio of carbon to aluminum was controlled to 3∶1 and a certain amount of stearic acid and ethylene glycol was added as surface active agents. Then, the precursor was heated at 1 550 ℃ for 4 h under common pressure at N2 flow rate of 5 L/min. Finally, AlN powders with nitrogen content of 33.20%, oxygen content of 0.98%, specific surface area of 4.26 m2/g were produced after decarbonization of the nitridation products in air for 4 h at 650 ℃.
Key words: AlN powders; precipitated precursor; carbothermal reduction
