液相前驱体转化法制备ZrB_2粉末  

Preparation of powdered zirconium diboride by a solution precursor conversion method

作　　者：李运涛[1] 陶雪钰[2] 邱文丰[2] 赵京波[1] 赵彤[2] 

机构地区：[1]北京化工大学材料科学与工程学院,北京100029 [2]中国科学院化学研究所高技术材料实验室,北京100190

出　　处：《北京化工大学学报（自然科学版）》2010年第4期78-82,共5页Journal of Beijing University of Chemical Technology(Natural Science Edition)

摘　　要：采用液相前驱体转化法制备ZrB2粉末。首先以聚乙酰丙酮锆、硼酸、酚醛树脂为原料制备了ZrB2前驱体,通过在高温下发生碳热还原反应热解前驱体得到ZrB2粉末。采用傅里叶红外光谱仪(FT-IR)、差热-热重分析仪(TG-DTA)、X射线衍射仪(XRD)、电感耦合等离子光谱发生仪(ICP)和扫描电镜(SEM)对ZrB2前驱体及热解产物进行了表征和分析。结果表明,该ZrB2前驱体易溶于常用溶剂,加工性能优良,可在相对较低的温度(1600℃)下热解得到纯度较高的ZrB2粉末;ZrB2前驱体在pH值不大于4的反应环境下,反应时间越长制备的ZrB2陶瓷粉末纯度越高;ZrB2粉末颗粒尺寸为2～4μm,粉末中存在ZrC晶体、游离碳和少量氧杂质。Zirconium diboride has been prepared by a solution precursor conversion method. The precursor was obtained by reaction of polyzirconoxane （PZO）,boric acid and phenolic resin dissolved in ethanol,and ZrB2 powder was obtained by subsequent pyrolysis of the precursor at relatively low temperature （1600 ℃）. The precursor and product powder were analyzed by FT-IR,TG,XRD,ICP and SEM. The ZrB2 precursor was soluble in common solvents,and possessed good processing capability. The final ZrB2 ceramic had high purity,and its purity increased as the reaction time in the preparation of the precursor was increased at pH ≤4. The impurities in ZrB2 were zirconium carbide,a little free carbon and oxygen-containing materials. The size of the ZrB2 particles was in the range 2-4 μm.

关 键 词：液相前驱体转化 硼化锆 碳热还原反应 

分 类 号：TQ174.75[化学工程—陶瓷工业]