(1.中国科学技术大学 火灾科学国家重点实验室，合肥 230026；
2. 中国科学技术大学 化学系， 合肥 230026)
摘 要: 用水热法合成了具有良好结晶度和大层间距的α-磷酸锆、α-磷酸锡及α-磷酸钛晶体(记为α-MP， M=Zr，Sn，Ti)，其组成通式为α-(MHPO4)2·H2O。并用XRD，TEM，HREM，IR及TG/DSC等方法对其进行了表征。结果表明，合成3种层状磷酸盐的优化实验条件(反应时间，温度，磷酸浓度)分别为α-ZrP：48h，180.℃， 8mol/L; α-SnP： 6h，180℃，9mol/L;α-TiP： 6h，180℃，10mol/L。水热法是一种较优越的制备层状磷酸盐的方法，得到的晶体形貌规整并具有较高的热稳定性。
关键字: 层状化合物；α-磷酸盐；水热合成； 热分析
stability of layered compound of
tetravalent metal phosphate
（1. State Key Lab of Fire Science， University of Science and
Technology of China，Hefei 230026， P.R.China；
2. Department of Chemistry，University of Science and
Technology of China，Hefei 230026，P.R.China）
Abstract: A series of well crystalline samples of acid salts with ideal general formula of α-M(HPO4)2·H2O (α-Zirconium phosphate(α-ZrP)，α-Tin phosphate(α-SnP) and α-Titanium phosphate(α-TiP)) were prepared by hydrothermal method and characterized by XRD，IR，TEM and TG/DSC. The results suggest that the optimum experiment conditions(time，temperature，phosphoric acid concentration)of forming these layered phosphate are 48h, 180℃, 8mol/L for α-ZrP; 6h, 180℃, 9mol/L for α- SnP and 6h, 180℃, 10mol/L for α-TiP，and hydrothermal synthesis is an optimum route for preparing layered compound of tetravalent metal phosphate. The crystalline samples possess a highly thermal stability and regular morphology.
Key words: layered compound;α-tetravalent metal phosphate; hydrothermal synthesis; thermal analysis
