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Detailed microstructure analysis of as-deposited and etched porous ZnO films

机译：沉积和蚀刻后的多孔ZnO薄膜的详细微观结构分析

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ZnO nanostructured materials in thin film forms are of particular interest for photovoltaic or photocatalysis processes but they suffer from a lack of simple methods for optimizing their microstructure. We have demonstrated that microporous ZnO thin films with optimized inter grain accessibility can be produce by radio frequency magnetron sputtering process and chemical etching with 2.75 mM HCl solution for different duration. The as-deposited ZnO thin films were first characterized in terms of structure, grain size, inter grain space, open cavity depth and total thickness of the film by XRD, AFM, SEM, profilometry and optical measurements. A specific attention was dedicated to the determination of the surface enhancement factor (SEF) by using basic geometrical considerations and images treatments. In addition, the porous fraction and its distribution in the thickness have been estimated thanks to the optical simulation of the experimental UV-Visible-IR spectrums using the Bruggeman dielectric model and cross section SEM images analysis respectively. This study showed that the microstructure of the as-deposited films consists of a dense layer covered by a porous upper layer developing a SEF of 12-13 m(2) m(-2). This two layers architecture is not modified by the etching process. The etching process only affects the upper porous layer in which the overall porosity and the inter-grain space increase with the etching duration. Column diameter and total film thickness decrease at the same time when the films are soaked in the HCl bath. The microporous structure obtained after the etching process could generate a great interest for the interfaces electronic exchanges for solar cells, photocatalysis and gas sensors applications. (C) 2015 Elsevier B.V. All rights reserved.
机译：薄膜形式的ZnO纳米结构材料对于光生伏打或光催化过程特别感兴趣，但它们缺乏优化其微结构的简单方法。我们已经证明，可以通过射频磁控溅射工艺和用2.75 mM HCl溶液在不同的持续时间进行化学蚀刻来生产具有最佳晶间可及性的微孔ZnO薄膜。首先通过XRD，AFM，SEM，轮廓测量和光学测量，对沉积的ZnO薄膜进行了结构，晶粒尺寸，晶粒间空间，开腔深度和薄膜总厚度方面的表征。通过使用基本的几何考虑和图像处理，专门致力于确定表面增强因子（SEF）。另外，得益于分别使用Bruggeman介电模型和截面SEM图像分析对实验性UV-Visible-IR光谱进行光学模拟，可以估算出多孔部分及其在厚度中的分布。这项研究表明，沉积薄膜的微观结构由致密层组成，该致密层被形成SEF为12-13 m（2）m（-2）的多孔上层覆盖。蚀刻过程不会修改这两层体系结构。蚀刻过程仅影响上部多孔层，其中总孔隙率和晶间空间随蚀刻持续时间而增加。当将膜浸泡在HCl浴中时，色谱柱直径和总膜厚度会同时减小。蚀刻过程后获得的微孔结构可能引起人们对于太阳能电池，光催化和气体传感器应用的电子交换界面的极大兴趣。 （C）2015 Elsevier B.V.保留所有权利。

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