Tyrpekl Vaclav, Markova Pavlina, Dopita Milan, Brázda Petr, Vacca Mirko A
Department of Inorganic Chemistry, Faculty of Science , Charles University , Hlavova , 2030 Prague , Czech Republic.
Department of Condensed Matter Physics, Faculty of Mathematics and Physics , Charles University in Prague , Ke Karlovu 5 , Prague , Czech Republic.
Inorg Chem. 2019 Aug 5;58(15):10111-10118. doi: 10.1021/acs.inorgchem.9b01250. Epub 2019 Jul 26.
Cerium dioxide is a scientifically and technologically important material with a wide range of potential applications, particularly in solid oxide fuel cells and catalysis. Herein, we report a study focusing on the synthesis of nanocrystalline cerium dioxide via thermal decomposition of the oxalate salt. Simply by changing reaction conditions (temperature, concentration, acidity, strike) during the precipitation of the cerium solution with oxalic acid, we were able to obtain different morphologies. The main reaction parameters were mapped and linked to the morphology of the final products. Additionally, it was proved that oxalate precipitation is a robust reaction proceeding at relatively extreme contitions. Moreover, the conversion of cerium oxalate to nanocrystalline oxide was followed to monitor the progress of the reaction, the texture evolution, and the grain growth. The results showed that, for unvaried heating cycle, the grain size of converted material is linked to morphology. The thinner was the original microcrystal the smaller were the CeO nanocrystals after calcination. In addition, the grains were found smaller near the edges of the ex-oxalate microcrystals. In both cases, this behavior results from asymmetrical limitations of diffusion during grain growth.
二氧化铈是一种具有重要科学技术意义的材料,具有广泛的潜在应用,特别是在固体氧化物燃料电池和催化领域。在此,我们报告一项关于通过草酸盐热分解合成纳米晶二氧化铈的研究。只需在草酸沉淀铈溶液的过程中改变反应条件(温度、浓度、酸度、搅拌),我们就能获得不同的形貌。绘制了主要反应参数并将其与最终产物的形貌联系起来。此外,还证明了草酸盐沉淀是一种在相对极端条件下进行的稳健反应。此外,跟踪草酸铈向纳米晶氧化物的转化,以监测反应进程、织构演变和晶粒生长。结果表明,对于不变的加热循环,转化材料的晶粒尺寸与形貌有关。原始微晶越薄,煅烧后CeO纳米晶体越小。此外,发现在原草酸盐微晶边缘附近的晶粒较小。在这两种情况下,这种行为都是由晶粒生长过程中扩散的不对称限制导致的。