(1.中國科學技術(shù)大學 火災(zāi)科學國家重點實驗室，合肥 230026；
2. 中國科學技術(shù)大學 化學系， 合肥 230026)
摘 要: 用水熱法合成了具有良好結(jié)晶度和大層間距的α-磷酸鋯、α-磷酸錫及α-磷酸鈦晶體(記為α-MP， M=Zr，Sn，Ti)，其組成通式為α-(MHPO4)2·H2O。并用XRD，TEM，HREM，IR及TG/DSC等方法對其進行了表征。結(jié)果表明，合成3種層狀磷酸鹽的優(yōu)化實驗條件(反應(yīng)時間，溫度，磷酸濃度)分別為α-ZrP：48h，180.℃， 8mol/L; α-SnP： 6h，180℃，9mol/L;α-TiP： 6h，180℃，10mol/L。水熱法是一種較優(yōu)越的制備層狀磷酸鹽的方法，得到的晶體形貌規(guī)整并具有較高的熱穩(wěn)定性。
關(guān)鍵字: 層狀化合物；α-磷酸鹽；水熱合成； 熱分析
stability of layered compound of
tetravalent metal phosphate
ZHU Yu-rui2，F(xiàn)AN Wei-cheng1，CHEN Zu-yao2
（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
