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Yanping Li, Xue Bian, Yang Liu, Wenyuan Wu, and Gaofeng Fu, Synthesis and characterization of ceria nanoparticles by complex-precipitation route, Int. J. Miner. Metall. Mater., 29(2022), No. 2, pp.292-297. https://dx.doi.org/10.1007/s12613-020-2126-9
Yanping Li, Xue Bian, Yang Liu, Wenyuan Wu, and Gaofeng Fu, Synthesis and characterization of ceria nanoparticles by complex-precipitation route, Int. J. Miner. Metall. Mater., 29(2022), No. 2, pp.292-297. https://dx.doi.org/10.1007/s12613-020-2126-9
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络合沉淀法合成纳米二氧化铈及其表征

摘要: 由于其独特的物理化学性质,纳米二氧化铈是一种良好的无机紫外线屏蔽剂。纳米二氧化铈的制备方法有水热法、溶胶–凝胶法、均相沉淀法、电化学方法等,这些方法通常有操作流程复杂、周期较长等缺点。本文旨在探索一种操作简单,周期短的纳米二氧化铈制备方法。本文以氯化铈为铈源、柠檬酸为沉淀剂,采用络合沉淀法成功合成了纳米二氧化铈。通过元素分析计算了前驱体的组成,并采用比表面积测试、显微组织观察、紫外-可见光透过率曲线研究了纳米二氧化铈的物理性能、微观组织与紫外屏蔽性能的关系。研究结果表明,随着pH的升高,前驱体中Ce(H2Cit)3的比例下降,而Ce(OH)3的比例上升,当pH = 6.5时,前驱体由CeCit和Ce(OH)3组成;随着柠檬酸与Ce3+的摩尔比(n)的增加,前驱体中Ce(H2Cit)3的比例升高,而Ce(OH)3的比例下降。当柠檬酸与Ce3+的摩尔比(n)为0.25、pH为5.5时,纳米二氧化铈在长波紫外线波段的平均透过率为4.42%,在中波紫外线波段的平均透过率为1.56%。良好的紫外屏蔽性能离不开纳米二氧化铈的物理性能和微观组织:比表面积的增大可以提高纳米二氧化铈的紫外屏蔽性能,当柠檬酸与Ce3+的摩尔比(n)为0.25、pH为5.5时,纳米二氧化铈的比表面积最大,为83.17 m2/g。纳米二氧化铈低指数晶面的晶面间距也影响着纳米二氧化铈的紫外屏蔽性能,在合理变化区间内,晶面间距越大,原子排列越密集,紫外屏蔽性能越好。由此得出这样的结论:络合沉淀法制备出的纳米二氧化铈具有优异的紫外屏蔽性能,但是,柠檬酸与Ce3+的摩尔比(n)不宜过大,pH不宜超过5.5。

 

Synthesis and characterization of ceria nanoparticles by complex-precipitation route

Abstract: Ceria (CeO2) nanoparticles were successfully synthesized via a simple complex-precipitation route that employs cerium chloride as cerium source and citric acid as precipitant. The elemental analysis results of carbon, hydrogen, oxygen, and cerium in the precursors were calculated, and the results revealed that the precursors were composed of Ce(OH)3, Ce(H2Cit)3, or CeCit. X-ray diffraction analysis showed that all ceria nanoparticles had a face-centered cubic structure. With the molar ratio of citric acid to Ce3+ (n) of 0.25 and pH of 5.5, the specific surface area of the sample reached the maximum value of 83.17 m2/g. Ceria nanoparticles were observed by scanning electron microscopy. Selected area electron diffraction patterns of several samples were obtained by transmission electron microscopy, and the crystal plane spacing of each low-exponent crystal plane was calculated. The ultraviolet (UV)–visible transmittance curve showed that ceria can absorb UV light and pass through visible light. Among all samples, the minimum average transmittance of ultraviolet radiation a (UVA) was 4.42%, and that of ultraviolet radiation b (UVB) was 1.56%.

 

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