层状磷酸锆的溶剂热合成与表征

Solvothermal Synthesis and Characterization of the Layered Compound of α-Zirconium Hydrophosphate

用溶剂热法合成了α 磷酸锆 (α ZrP)晶体 ,并采用XRD、IR、TEM和TG/DSC等方法对其进行了表征 ,结果显示 ,用该法制得的α ZrP ,具有良好的结晶度 ,层间距达到7.6 3 .α ZrP晶体的结晶水在 1 2 5℃到 430℃之间被脱除 ,其层板羟基在 430℃开始缓慢脱除 ,直到 5 80℃才完全脱除 ,表明其热稳定性较高 .得到了溶剂热法合成α ZrP的优化实验条件为 :体系中磷酸浓度为 5M至 1 0M和 1 80℃下反应 48h以上 .

Crystalline samples of α Zirconium hydrophosphate (α ZrP) were prepared by solvothermal method and characterized by XRD, IR, TEM and TG DSC. They are highly crystalline with an interlayer distance of 7.63 ? and hexagonal flakes in α ZrP. Meanwhile, it is shown that α ZrP possesses a high thermal stability, which dehydrates the water of crystallization between 125 ℃ and 430 ℃ and the hydroxyl groups in the layers between 430 ℃ and 580 ℃. The results suggest that the optimum experimental condition for solvothermal method is 180 ℃ beyond 48 hours in 5 M～10 M phosphoric acid.