前驱体法合成氮化铝纳米材料及其生长机制  

Preparation of Aluminum Nitride Nanomaterials by Precursor Method

作　　者：李紫璇 郝留成 张建飞[1] 周小楠 黄鑫 史忠旗 杨建锋[1] 王波[1] LI Zixuan;HAO Liucheng;ZHANG Jianfei;ZHOU Xiaonan;HUANG Xin;SHI Zhongqi;YANG Jianfeng;WANG Bo(State Key Laboratory for Mechanical Behavior of Materials,Xi′an Jiaotong University,Xi'an 710049,China;High Voltage Switch Insulating Materials Laboratory of State Grid,Pinggao Group Co.,Ltd.,Pingdingshan 467001,Henan,China)

机构地区：[1]西安交通大学金属材料国家重点实验室,西安710049 [2]平顶山集团有限公司国家电网公司高压开关设备绝缘材料实验室,河南平顶山467001

出　　处：《硅酸盐学报》2020年第6期787-793,共7页Journal of The Chinese Ceramic Society

基　　金：国家重点研发计划(2017YFB0903800);国家自然科学基金(51872223,51872222,51902241)。

摘　　要：以尿素为固体氮源、AlCl3·6H2O为铝源,通过溶液反应合成金属络合物前驱体Al(CON2H4)6Cl3,前驱体经过1000℃煅烧,制备得到球形h-AlN纳米颗粒。研究了气氛压力及合成时间对AlN纳米颗粒形貌的影响及AlN的形核生长机制。结果表明:在0.1~0.2 MPa的N2压力下,球状AlN颗粒由<10 nm的等轴状细小晶粒与非晶相团聚而成,直径为320~460 nm;随着N2压力增至0.5 MPa,球状AlN直径增加至650 nm,团聚体中棒状AlN晶体出现,随着烧结时间延长,棒状晶尺寸增大,数量增加。AlN纳米颗粒由前驱体分解形成的AlCl3和NH3反应而成,随着N2压力增大,坩埚内气相饱和度增大,促进了AlN的形核与生长,使得非晶相含量减少,AlN结晶度提高。Al(CON2H4)6Cl3 was firstly synthesized as a precursor with urea and AlCl3·6H2O as a nitrogen source and an aluminum source,respectively,and then the precursor was calcined at 1000℃to prepare spherical h-AlN nanoparticles.The effects of atmosphere pressure and sintering time on the morphology and the nucleation-growth mechanism of AlN were investigated.The results show that spherical AlN particles with the sizes of 320–460 nm are formed by equiaxed fine grains of smaller than 10 nm and amorphous phase under N2 pressure of 0.1–0.2 MPa.As the N2 pressure increases to 0.5 MPa,the diameter of spherical AlN increases to 650 nm,and rod-shaped AlN crystals appear in the aggregates.The size and number of rod crystals increase as the sintering time increases.AlN nanoparticles are formed by the reaction of AlCl3 and NH3 due to the decomposition of the precursor.The gas phase saturation in the crucible increases as N2 pressure increases,promoting the nucleation and growth of AlN,reducing the amorphous phase content,and enhancing the crystallinity of AlN.

关 键 词：氮化铝 尿素 前驱体 氮气压力 

分 类 号：TB32[一般工业技术—材料科学与工程]