层状磷酸锆纳米晶的低热固相合成及表征  

Preparation of Layered Nanometer Crystalline Zr(HPO_4)_2·H_2O via Low Heat Solid-State Reaction and Its Characterization

作　　者：吴文伟[1] 赖水彬[1] 廖森[1] 吴学航[1] 侯生益[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《稀有金属》2007年第6期798-801,共4页Chinese Journal of Rare Metals

基　　金：广西自然科学基金(0640009);广西大型仪器协作共用网资助基金(360-2006-049)资助项目

摘　　要：以ZrOCl2.8H2O和(NH4)3PO4.3H2O为原料,先在室温下研磨反应混合物使其进行固相反应,然后将其在80℃下密封保温96 h,接着用水洗去混合物中的可溶性无机盐后于80℃下烘干,即得磷酸锆纳米晶产品。采用TG/DTA,IR,XRD和TEM对产品及其热解产品进行表征。结果表明,80℃下保温3 h得到结晶良好、空间群为P21/c(14)、平均粒径约为23 nm的Zr(HPO4)2.H2O,其晶体结构稳定的温度可高达450℃。在900℃下煅烧Zr(HPO4)2.H2O则得到结晶良好、空间群为Pa-3(205)、平均粒径约为31 nm的ZrP2O7晶体。The layered nanometer crystalline Zr（HPO4）2·H2O was obtained when ZrOCl2·8H2O and（NH4）3PO4·3H2O were fully ground via solid-state reaction at room temperature,then mixture was heated at 80 ℃ for 96 h,and washed with water to remove soluble inorganic salts and dried at 80 ℃.Product and its thermal decomposition products were characterized by TG/DTA,IR,XRD and TEM.The results showed that nanometer crystalline Zr（HPO4）2·H2O obtained at 80 ℃ was with high crystallinity,space group P21/c（14）,and average particle size was about 23 nm.Its crystal structure kept stable until 450 ℃.When Zr（HPO4）2·H2O was calcined at 900 ℃ for 3 h,the nanometer crystallinity ZrP2O7 with high crystallinity,space group Pa-3（205）,was obtained,and its average particle size was about 31 nm.

关 键 词：磷酸锆 纳米晶 低热固相合成 表征 

分 类 号：TG13[一般工业技术—材料科学与工程]