煅烧温度对制备钠快离子导体NaZr_(2)(PO_(4))_(3)粉体的影响

Effect of Calcination Temperature on Properties of Sodium Fast Ionic Conductor NaZr_(2)(PO_(4))_(3) Powders

以八水氧氯化锆(ZrOCl_(2)·8H_(2)O)、二水磷酸二氢钠(NaH_(2)PO_(4)·2H_(2)O)为原料,乙二醇(CH_(2)OH)2为助碾磨试剂,通过简单的低温固相反应合成了NaZr_(2)(PO_(4))_(3)粉体。采用DSC-TG、XRD、FE-SEM、Raman等手段研究了煅烧温度对制备钠快离子导体NaZr_(2)(PO_(4))_(3)粉体的影响,并探讨了其低温形成机理。结果表明,在煅烧温度810℃下保温5h,能够制备出平均粒径为0.5μm,尺寸均匀的NaZr_(2)(PO_(4))_(3)粉体。研磨时发生的固相反应有助于Zr(HPO_(4))2·H_(2)O的产生,有利于NaZr_(2)(PO_(4))_(3)的低温合成。同时原位生成的NaCl与NaPO_(3)形成低共熔熔盐,其加热到低共熔态产生的液相促进了NaZr_(2)(PO_(4))_(3)的晶体生长和均匀分散。

NaZr_(2)(PO_(4))_(3) powders were prepared by using a simple low-temperature solid reaction,with zirconium oxychloride octahydrate(ZrOCl_(2)·8H_(2)O),sodium dihydrogen phosphate dihydrate(NaH_(2)PO_(4)·2H_(2)O)as the raw materials and ethylene glycol(CH_(2)OH)2 as grinding agent.The effect of calcination temperature on properties of the sodium fast ion conductor NaZr_(2)(PO_(4))_(3) powders was studied by using DSC-TG,XRD,FE-SEM and Raman techniques,while the corresponding formation mechanism was also discussed.It was found that homogeneous NaZr_(2)(PO_(4))_(3) powders were obtained after calcination at 810℃for 5 h,with an average particle size of about 0.5μm.The solid phase reaction was beneficial to the formation of Zr(HPO_(4))2·H_(2)O during the grinding process,thus favoring the production of NaZr_(2)(PO_(4))_(3) at relatively low temperatures.In addition,the combination of the in-situ produced NaCl with NaPO_(3) triggered the formation of low eutectic salt,contributing to the growth of well-dispersed NaZr_(2)(PO_(4))_(3) crystalline powders,owing to the production of liquid phase.