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X-ray diffraction Rietveld structural analysis of Au–TiO 2 powders synthesized by sol–gel route coupled to microwave and sonochemistry
Journal of Sol-Gel Science and Technology ( IF 2.5 ) Pub Date : 2020-03-09 , DOI: 10.1007/s10971-020-05264-5
Rafael Hernández , J. Rosendo Hernández-Reséndiz , Alejandro Martínez-Chávez , Rodrigo Velázquez-Castillo , Luis Escobar-Alarcón , Karen Esquivel

TiO2 is one of the most studied photocatalyst, however, in order to enhance the photocatalytic activity, several strategies for chemical or physical modifications have been reported. Among these strategies, microwave and sonochemistry assisted synthesis methods have been attracting attention due to the unique characteristics that can be achieved through it. Au–TiO2 nano powders were synthesized via microwave assisted sol–gel method (SG method) and sonochemistry assisted sol–gel method (SC method) with varying gold load, (containing 0.05, 0.1, 0.3, 0.7, 1.0, 3.0 and 5.0 wt% for SG method and 0.05, 0.1, 0.3, 0.7, 1.0 wt% for SC method). Subsequently, a calcination process was carried out at 450 °C for 3 h. Materials obtained were physicochemical analyzed by SEM, XPS, and XRD analysis. According to XRD analysis, the main crystalline phase of the materials was anatase. Average crystallite size and microstrain present in the powders were studied using the Williamson–Hall method and Debye–Scherrer equation. The crystal structure of all samples was refined by the Rietveld method, and a compression on the unit cell parameters was determined. These analyses revealed an increment in the unit cell strain when Au concentration was increased, and a decrease of the crystallinity in the powders when SG method was used. In the case of SC method samples, crystallinity and strain was found to remain constant.



中文翻译:

溶胶-凝胶法耦合微波和声化学法合成Au-TiO 2粉末的X射线衍射Rietveld结构分析

TiO 2是研究最多的光催化剂之一,但是,为了提高光催化活性,已经报道了几种化学或物理修饰的策略。在这些策略中,微波和声化学辅助合成方法由于可通过其实现的独特特性而受到关注。金–TiO 2通过微波辅助溶胶-凝胶法(SG方法)和声化学辅助溶胶-凝胶法(SC方法)合成了金粉含量不同的纳米粉末(SG含量为0.05、0.1、0.3、0.7、1.0、3.0和5.0 wt% (例如,SC法则为0.05、0.1、0.3、0.7、1.0重量%)。随后,在450℃下进行3小时的煅烧过程。通过SEM,XPS和XRD分析对获得的材料进行物理化学分析。根据XRD分析,材料的主要结晶相是锐钛矿。使用Williamson-Hall方法和Debye-Scherrer方程研究了粉末中平均晶粒尺寸和微应变。通过Rietveld方法精炼所有样品的晶体结构,并确定晶胞参数的压缩率。这些分析表明,当Au浓度增加时,晶胞应变增加,而当使用SG法时,粉末的结晶度降低。对于SC方法样品,发现结晶度和应变保持恒定。

更新日期:2020-03-09
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