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爆轰合成纳米氧化铈的提纯分析

         

摘要

为了提高特种炸药爆轰合成纳米氧化铈的纯度,采用酸洗方法提纯,设计正交实验研究了提纯温度、时间,硝酸、蒸馏水和聚乙二醇(PEG)加入量对提纯结果的影响。利用 X 射线衍射仪、X 射线荧光光谱仪分析氧化铈提纯前后的晶型及杂质含量,以氧化铈纯度为判定标准,确定最佳提纯参数。结果表明:提纯温度过高会导致硝酸浓度降低,时间过长会使过多氧化铈溶解;利用透射电镜观察颗粒表面,加入PEG可改善纳米氧化铈颗粒团聚现象。最佳提纯参数为:温度80℃,时间24h,硝酸量0.333mL/g,蒸馏水量6.666mL/g,PEG 量16.666mg/g,利用此参数提纯后的纳米氧化铈纯度为99.59%。分析杂质残留的原因为爆轰高温条件使 Fe2O3和Al2O3转化为α-Fe2O3和α-Al2O3,导致0.12%Fe2O3和0.17%Al2O3杂质残留。%Pickling was used to improve the purity of nano ceria synthesized by special explosive detonation. Time and temperature of purification , the amount of distilled water , nitrate and polyethylene glycol (PEG) were studied regarding their effects on purity through the design of orthogonal test. Crystal form and impurity content of ceria were analyzed by X ray diffraction and X ray fluorescence spectrometer. The purity of ceria was used as the criterion to determine the optimal purification parameters. The results show that high temperature will lead to reducing the concentration of nitrate,even cause excessive ceria dissolve after long time; adding PEG can ameliorate the agglomeration of nano ceria particles by observing the surface of particles with transmission electron microscopy. The best purification parameters of nano ceria are that temperature is 80℃,time is 24h, the amount of nitrate,distilled water and PEG are 0.333mL,6.666mL and 16.666mg each gram of detonation ash respectively; The purity can reach 99.59% under the best parameters. Detonation temperature makes Fe2O3 and Al2O3 change intoα-Fe2O3 andα-Al2O3,0.12%of Fe2O3 and 0.17%of Al2O3 are left over.

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