基于非水解sol-gel法的碳热还原氮化合成氮化铝超细粉体  

Synthesis of aluminum nitride ultrafine powder via carbon thermal reduction nitridation process based on non-hydrolytic sol-gel method

作　　者：魏颖娜[1,2,3] 魏恒勇[1,2,3] 赵冬梅[1,3] 卜景龙[1,3] 于云[2] 王瑞生[1,3] 

机构地区：[1]河北联合大学材料科学与工程学院,河北唐山063009 [2]中国科学院特种无机涂层重点实验室,上海200050 [3]河北省无机非金属材料重点实验室,河北唐山063009

出　　处：《功能材料》2013年第17期2546-2549,共4页Journal of Functional Materials

基　　金：国家自然科学基金资助项目(51272066);中国科学院特种无机涂层重点实验室开放课题基金资助项目(KLICM-2011-01);河北省高等学校科学技术研究青年基金资助项目(2011124)

摘　　要：以无水氯化铝和异丙醚为原料,采用非水解溶胶-凝胶法制备出氧化铝凝胶。其经800℃煅烧才析出少量γ-Al2O3晶体,γ-Al2O3向α-Al2O3晶型转变在1200℃附近,经900℃煅烧后比表面积仍高达145m2/g,具有介孔结构。以该高活性氧化铝凝胶作为铝源,采用碳热还原氮化工艺合成氮化铝粉体。结果表明,氧化铝凝胶经300℃预煅烧,按n(C)/n(Al)=7.8与碳黑混合,在流量80mL/min高纯N2中,于1450℃还原氮化2h便可合成出平均粒径在400nm的高纯六方相AlN粉体。The alumina xerogel was prepared by non-hydrolytic sol-gel method using anhydrous aluminium tri- chloride with isopropyl ether as raw materials. After the xerogel was calcined at 800℃, the phase of γ-Al2O3 began to crystallize from the amorphous phase, and then converted to α-Al2O3 near 1200℃. The smaple kept a high specific surface area of 145m2/g to about 900℃, and possessed the mesoporous structure. Using the alu- mina xerogel as the aluminum source, aluminum nitride ultrafine powder was synthesized by the carbon thermal reduction nitridation process. The resluts showed that when the alumina xerogel was pre-calcinated at 300℃, the C/A1 molar ratio amount of the carbon was 7.8, the flow rate of nitrogen was 80mL/min, the synthesis temperture was 1450℃ and the soaking time was 2h, the high purity hexagonal phase aluminum nitride powder with the average size of about 400nm could be obtained.

关 键 词：非水解溶胶-凝胶法 碳热还原氮化法 氮化铝 超细粉体 

分 类 号：TQ174.758.12[化学工程—陶瓷工业]