花状CdO微球的制备及其对高氯酸铵热分解的催化性能

doi:10.11868/j.issn.1001-4381.2019.000287

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摘要

采用溶剂热合成-热分解两步法制得花状CdO微球。以醋酸镉为原料、甲醇为溶剂，采用溶剂热法合成由纳米片自组装而成的花状前驱体微球。将前驱体焙烧后，得到形貌保持良好的花状多孔CdO微球。利用X射线衍射（XRD）、傅里叶变换红外光谱（FT-IR）、热重（TG）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）和N₂吸附-脱附等手段对样品的物相、化学组成、形貌及孔结构进行表征。借助差示扫描量热（DSC）技术对CdO花状微球催化高氯酸铵（AP）热分解的性能进行评价。结果表明：花状CdO微球对AP热分解过程具有一定的催化作用。添加质量分数为2%的CdO可使AP的高温分解峰值温度从444.4℃降低至402.8℃，分解热从586.9 J/g提高到1091.7 J/g，分解活化能从280.5 kJ/mol减小至83.78 kJ/mol。基于实验结果，提出了CdO花状微球催化AP热分解的可能机理。

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	曾凡达
	李纲

关键词 ：氧化镉, 花状微球, 高氯酸铵, 热分解, 催化性能

Abstract：

A two-step method involving solvothermal synthesis and annealing was used to prepare the flower-like CdO microspheres.The flower-like precursor microspheres assembled by nano-flakes were firstly fabricated by the solvothermal method using Cd(Ac)₂ as source materials in methanol system.Through calcining the precursor, CdO porous microspheres with well-preserved morphologies were then obtained.X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FT-IR), thermal gravimetry(TG), scanning electron microscopy(SEM), transmission electron microscopy(TEM) and N₂ adsorption-desorption were used to characterize the phases, chemical composition, morphologies and pore structures of the samples.Differential scanning calorimetry(DSC) was employed to evaluate the catalytic performance of these CdO microspheres for thermal decomposition of ammonium perchlorate(AP).The results show that the as-obtained CdO microspheres play a positive role in catalyzing the thermal decomposition of AP.Adding 2%(mass fraction)CdO microspheres into AP, the peak temperature decreases from 444.4 ℃ to 402.8 ℃ and the heat released increases from 586.9 J/g to 1091.7 J/g.The activation energy of AP decomposition significantly decreases from 280.5 kJ/mol to 83.78 kJ/mol.Based on the results, a possible catalytic mechanism for the thermal decomposition of AP over flower-like CdO microspheres is proposed.

Key words： cadmium oxide flower-like microsphere ammonium perchlorate thermal decomposition cata- lytic performance

收稿日期: 2019-03-27 出版日期: 2020-06-15

中图分类号:

TQ115

基金资助:重庆市基础与前沿研究计划项目(cstc2016jcyjA0438);重庆市教委科学技术研究项目(KJ1600926)

通讯作者: 李纲 E-mail: ligang2015@cqut.edu.cn

作者简介: 李纲(1981—), 男, 副教授, 博士, 主要从事纳米功能材料制备及其应用研究, 联系地址:重庆市巴南区红光大道69号重庆理工大学化学化工学院(400054), ligang2015@cqut.edu.cn

引用本文:

曾凡达, 李纲. 花状CdO微球的制备及其对高氯酸铵热分解的催化性能[J]. 材料工程, 2020, 48(6): 91-97.
Fan-da ZENG, Gang LI. Preparation of flower-like CdO microspheres and its catalytic performances towards thermal decomposition of ammonium perchlorate. Journal of Materials Engineering, 2020, 48(6): 91-97.

链接本文:

http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2019.000287 或 http://jme.biam.ac.cn/CN/Y2020/V48/I6/91

Fig.1 前驱体(a)和产物(b)的XRD谱图

Fig.2 前驱体的FT-IR谱图

Fig.3 前驱体的热重曲线

Fig.4 前驱体(a)，(b)和产物(c)，(d)的SEM图

Fig.5 产物的TEM图
(a)单个纳米片；(b)图 5(a)的局部放大图；(c)单个纳米晶的HRTEM图

Fig.6 产物的N₂吸附-脱附等温线(a)及孔径分布曲线(b)

Fig.7 纯AP及花状CdO/AP混合物的DSC曲线

Fig.8 不同升温速率下CdO/AP混合物的DSC曲线

Fig.9 ln(β/T_m²)与1000/T_m的关系曲线

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