Preparation of ceria–zirconia (Ce0.75Zr0.25O2) powders by microwave–hydrothermal (MH) route
Preparation of ceria–zirconia (Ce0.75Zr0.25O2) powders by microwave–hydrothermal (MH) route
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DOI：
10.1016/s0254-0584(01)00485-0
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发表时间：
2002-04
影响因子：
4.6
通讯作者：
H. S. Potdar;S. B. Deshpande;A. Deshpande;S. Gokhale;S. Date;Y. Khollam;A. Patil
中科院分区：
文献类型：
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作者：
H. S. Potdar;S. B. Deshpande;A. Deshpande;S. Gokhale;S. Date;Y. Khollam;A. Patil
以ZrO（NO3）2·xH 2 O、Ce（NO3）3·6 H2O为原料，KOH为矿化剂，采用微波-水热反应（200°C，200 psi，30 min）制备了组成为Ce0.75Zr0.25O2的二元混合金属氧化物。分别使用0.025、0.075和1.2M的ZrO（NO3）2·xH 2 O、Ce（NO3）3·6 H2O和KOH溶液用于MH合成。将ZrO（NO3）2·xH 2 O（0.025M）和Ce（NO3）3·6 H2O（0.075M）各自的溶液（7.5ml）与25 ml KOH混合，并在专门设计的容器中使用微波加速反应系统处理，以获得氧化铈-氧化锆固溶体。采用XRD、拉曼、SEM、EDAX、TEM、BET等物理化学技术对所得粉末进行表征。结果表明，所制备的粉末颗粒由具有立方萤石结构的氧化铈-氧化锆的固溶体组成，表面积等于125 m2 g-1。SEM/TEM照片显示，团聚体的分布不同，一次粒径为1.7nm。在低至180°C（127 psi）的温度（压力）和5分钟的时间下获得立方相。
Binary mixed metal oxides, having composition Ce0.75Zr0.25O2were prepared by microwave–hydrothermal (MH) reaction (200°C, 200psi, 30min) using ZrO(NO3)2·xH2O, Ce(NO3)3·6H2O as starting precursors and KOH as mineralizer. 0.025, 0.075 and 1.2M solutions of ZrO(NO3)2·xH2O, Ce(NO3)3·6H2O and KOH, respectively, are used for MH synthesis. Solution (7.5ml) of each of ZrO(NO3)2·xH2O (0.025M) and Ce(NO3)3·6H2O (0.075M) are mixed with 25ml of KOH and treated in specially designed vessels using microwave accelerated reaction system to obtain ceria–zirconia solid solution. Various physico-chemical techniques such as XRD, Raman, SEM, EDAX, TEM, BET, etc. are used to characterize the resultant powders. The results showed that the as-prepared powder particles consisted of solid solution of ceria–zirconia having cubic fluorite structure with surface area equal to 125m2g−1. SEM/TEM photographs for the same showed varied distribution of agglomerates with primary particle size≅7nm. The cubic phase is obtained at a temperature (pressure) and time as low as 180°C (127psi) and 5min.