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采用改进的直接沉淀氟配位法,在常温常压下制备出了α-磷酸锆(α-ZrP),XRD结果表明它的层间距为0.765nm,结晶度较好,并以热重分析法(TG)为手段,对α-ZrP的热分解过程和非等温热分解动力学机理进行了研究。结果显示,在线性升温速率为10℃/min时,α-ZrP在131℃开始脱结晶水;脱去结晶水后形成的Zr(HPO4)2在453℃进行磷羟基缩合,至720℃完全分解为ZrP2O7。脱结晶水和分解过程的失重分别为6.24%和5.64%,与理论值基本相符。动力学研究确定了Zr(HPO4)2分解反应属于Avrami-Erofeev的成核和核成长为控制步骤的Al机理,热分解反应表观活化能为165.6kJ/mol,频率因子为3.50×107s-1。
A-ZrP (α-ZrP) was prepared at room temperature and normal pressure by an improved direct precipitation fluorine coordination method. The XRD results showed that the interlayer spacing was 0.765 nm, the crystallinity was good, (TG) as a means to study the thermal decomposition process of α-ZrP and the kinetic mechanism of non-isothermal pyrolysis. The results showed that α-ZrP began to de-crystallize water at 131 ℃ at a linear heating rate of 10 ℃ / min. Zr (HPO4) 2 formed after de-watering was condensed at 453 ℃ for phosphate hydroxyl group and completely decomposed to 720 ℃ ZrP2O7. The weight loss of dewatered water and decomposition process were 6.24% and 5.64%, respectively, which was in good agreement with the theoretical value. Kinetic studies confirmed the mechanism of the nucleation and nucleation of Zr (HPO4) 2 belonging to Avrami-Erofeev. The activation energy of the pyrolysis reaction was 165.6 kJ / mol and the frequency factor was 3.50 × 107s-1.