液相前驱体转化法制备ZrB_2粉末

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。

Preparation of powdered zirconium diboride by a solution precursor conversion method

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 ZrB2 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 ZrB2 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 2-4μm.