Abstract：The calculation of platinum nanocrystal size in Pt/C catalyst for fuel cell by transmission electron microscopy (TEM) is a commonly used method with good accuracy. However, it has some disadvantages, such as high cost, poor representativeness in statistics, and complex measurement. A batch of Pt/C catalysts for fuel cell were prepared. First, the average size of platinum nanocrystals in the catalyst was measured by TEM. Then, the average size of platinum nanocrystals was calculated by Scherrer formula and Rietveld refinement of TOPAS software, respectively. The calculation results were compared with the TEM method. Compared with TEM method, the relative error of average size of platinum nanocrystals calculated by Rietveld refinement of TOPAS software was only 1.3%. In other words, the measurement results of average size of platinum nanocrystals by X-ray diffraction analysis combined with TOPAS software were very close to those of intuitive TEM method, thus realizing the efficient and reliable measurement of platinum nanocrystals.
[1] 于江江.新能源汽车安全分析及发展研究[J].科学技术创新(Scientific and Technological Innovation),2020(19):174-175. [2] 王敏键,陈四国,邵敏华,等.氢燃料电池电催化剂研究进展[J].化工进展,2021,40(9):4948-4961. WANG Minjian,CHEN Siguo,SHAO Minhua,et al.Recent advances of electrocatalysts in hydrogen fuel cells[J].Chemical Industy and Engineering Progress,2021,40(9):4948-4961. [3] 郑孙洁,严新焕. 形貌可控的Pt纳米催化剂的制备及其应用进展[J].化工进展,2011,30(3):513-519,529. ZHENG Sunjie,YAN Xinhuan.Shape-controlled synthesis of platinum nanocatalysts for catalytic and electrocatalytic applications[J].Chemical Industy and Engineering Progress,2011,30(3):513-519,529. [4] 杨卫亚,凌凤香,刘全杰,等.HAADF与TEM表征Ru/C催化剂贵金属分散性的对比研究[J].理化检验(物理分册),2019(4):232-235. YANG Weiya,LING Fengxiang,LIU Quanjie,et al.Comparative studies on noble metal dispersion of Ru/C catalyst characterized by HAADF and TEM[J].Physical Testing and Chemical Analysis (Part A:Physical Testing),2019(4):232-235. [5] 韩力涛.高性能纳米Cu-Fe,Cu-Fe-X(Cr, Zr, P)合金的制备,结构及性能研究[D].合肥:中国科学技术大学,2019. [6] 王乐,王永在,刘胜,等.X-射线全谱拟合法测量钛白粉的晶粒度[J].山东化工(Shandong Chemical Industry),2014,43(12):75-76. [7] 黎爽,邓平晔.应用Topas和Eva软件计算纳米材料晶粒尺寸的数值观察[J].人工晶体学报,2018,47(4):879-884. LI Shuang,DENG Pingye.Observation for crystallite size of nanoparticals calculated by Topas and Eva software[J].Journal of Synthetic Crystals,2018,47(4):879-884. [8] Soares A F,Tatumi S H,Rocca R R,et al.Morphological and luminescent properties of HfO2 nanoparticles synthesized by precipitation method[J].Journal of Luminescence,2020,219:116866. [9] Runcˇevski T.Rietveld refinement practical powder diffraction pattern analysis using TOPAS[J].Journal of Applied Crystallography,2019,52(5):1238-1239. [10] 甘延玲,金头男,聂光临,等.全谱拟合定量分析方法及其影响因素的研究[J].分析科学学报,2016,32(1):89-94. GAN Yanling,JIN Tounan,NIE Guanglin,et al.Study on the effecting factors of quantitative analysis by Rietveld method[J].Journal of Analytical Science,2016,32(1):89-94. [11] Popa N C,Balzar D.Size-broadening anisotropy in whole powder pattern fitting.Application to zinc oxide and interpretation of the apparent crystallites in terms of physical models[J].Journal of Applied Crystallography,2008,41(3):615-627. [12] 骆军,朱航天,梁敬魁.晶粒尺寸和应变的X射线粉末衍射法测定[J].物理,2009,38(4):267-275. LUO Jun,ZHU Hangtian,LIANG Jingkui.Determination of crystallite size and strain by X-ray powder[J]Physics,2009,38(4):267-275.
