Synthesis and characterization of doped nano-sized ceria–zirconia solid solutions
Synthesis and characterization of doped nano-sized ceria–zirconia solid solutions
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DOI：
10.1016/j.apcatb.2009.03.031
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发表时间：
2009-08
影响因子：
22.1
通讯作者：
X. Weng;B. Perston;X. Wang;I. Abrahams;Tian Lin;Shoufeng Yang;J. Evans;D. Morgan;A. Carley;M. Bowker;J. Knowles;I. Rehman;J. Darr
中科院分区：
文献类型：
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作者：
X. Weng;B. Perston;X. Wang;I. Abrahams;Tian Lin;Shoufeng Yang;J. Evans;D. Morgan;A. Carley;M. Bowker;J. Knowles;I. Rehman;J. Darr
使用连续水热流合成反应器将基于氧化铈-氧化锆固溶体的两种组合物Ce0.50Zr0.39La0.04Y0.07O2-δ和Ce0.25Zr0.65La0.04Y0.06O2-δ制备为纳米粉末，然后对浆料进行冷冻干燥或热板干燥。然后使每个干燥的纳米粉末在空气中在1000°C、1100°C或1200°C下经受10小时热处理（以模拟加速老化）。使用程序升温还原（TPR）测量氧化样品的还原性和氢消耗，直至1000°C。考察了组成、干燥方式和热处理温度对材料TPR曲线的影响。使用包括UV/维斯光谱（其产生颜色数据）、拉曼光谱、粉末X射线衍射、BET表面积测量和X射线光电子能谱（XPS）的一系列分析方法进一步研究粉末。化学计量学方法被用来研究光谱和总储氧能力（OSC）数据之间的关系。主成分分析（PCA）是用来提供一个简单的解释的各种合成和处理参数的影响拉曼光谱。采用主成分回归法（PCR）建立了TPR中几个设定温度下的拉曼光谱与耗氢峰温度的回归模型。材料的总氢消耗量通常很高，而干燥和热处理条件似乎对所得粉末的最终性质（例如表面积和总储氧能力）具有显著影响。
Two compositions Ce0.50Zr0.39La0.04Y0.07O2−δand Ce0.25Zr0.65La0.04Y0.06O2−δbased on ceria-zirconia solid solutions were prepared as nanopowders using a continuous hydrothermal flow synthesis reactor, followed by either freeze-drying or hotplate-drying of the slurry. Each dried nanopowder was then subjected to 10h heat-treatment at 1000°C, 1100°C or 1200°C in air (to simulate accelerated ageing). The reducibility and hydrogen consumption of the oxidised samples were measured using temperature programmed reduction (TPR) up to 1000°C. The effects of composition, drying method and heat-treatment temperature were evaluated on the TPR profiles of the materials. The powders were further investigated using a range of analytical methods including UV/Vis spectroscopy (which yielded colour data), Raman spectroscopy, powder X-ray diffraction, BET surface area measurements and X-ray photoelectron spectroscopy (XPS). Chemometric methods were used to investigate relationships between the spectroscopic and total oxygen storage capacity (OSC) data. Principal component analysis (PCA) was used to provide a simple interpretation of the effects of various synthesis and treatment parameters on Raman spectra. Principal component regression (PCR) was used to build regression models relating the Raman spectra and the temperature of hydrogen consumption peak at several set temperatures in the TPR. The total hydrogen consumption of the materials was generally high, while the drying and heat-treatment conditions appeared to have a significant effect on the final properties of the resulting powders, such as the surface area and total oxygen storage capacity.