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基于常规X射线光电子能谱(XPS)和X射线衍射(XRD)技术的透明柔性导电膜薄膜厚度表征

Characterization of Thin-film Thickness Based on Conventional XPS and XRD
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摘要 X射线光电子能谱仪(XPS)和X射线衍射仪(XRD)已越来越成为实验室的常规必备设备。XPS是一种表面分析技术,典型的分析深度约为10 nm,主要用于表征材料表面元素及其化学状态,并可利用刻蚀离子枪对材料元素及其化学态纵深分布进行研究。XRD主要利用晶体对X射线的衍射测定材料的晶体结构;同时可利用材料表面、界面对X射线的反射,研究材料的物性,包括密度、厚度、粗糙度等。利用实验室常规的XPS和XRD联合表征多层薄膜厚度;结合两者各自的优势,通过简单、便捷的方法实现多层薄膜的结构表征。通过XRD测试多层薄膜的反射干涉条纹,运用快速傅里叶变换(FFT)方法得到其厚度信息;通过XPS深度剖析得到膜层组分及其纵向分布的信息,从而完整表征了多层薄膜的结构。所表征的样品为组成和结构未知的透明柔性导电膜。结合XPS和XRD分析得到结果:薄膜为三层复合膜结构,首层由SnO_(2)、In_(2)O_(3)、TiO_(2)和ZnO组成,厚度为42.6 nm;中间为19.2 nm Ag纳米线;靠近基底层由ZnO、In_(2)O_(3)和TiO_(2)组成,厚度为59.0 nm。建立的方法完全避免了建模的繁杂过程和不确定性,方便、快速地得到薄膜结构组成,包括:每层薄膜厚度、组成成分、层间堆叠顺序等。方法在薄膜研究、生产过程质量控制等方面应用都有十分重要意义。 X-ray photoelectron spectrometer(XPS)and X-ray diffractometer(XRD)have increasingly become essential equipment in laboratories.XPS is a surface analysis technique with a typical analysis depth of about 10 nm,mainly used to characterize surface elements and their chemical states of materials.At the same time,the etching ion guns can bee used to study the depth distribution of material elements and their chemical states combined with XPS.XRD mainly utilizes the diffraction of X-rays to determine the crystal structure of materials.At the same time,the reflection of X-rays on the surface and interface of materials can be also utilized to study their physical properties,including density,thickness,roughness,etc.The lab-based conventional XPS and XRD were used to jointly characterize the thickness of multilayers thin-film sample.And combined with the advantages of both,the structural characterization of multilayers thin film was achieved through a facile and convenient method.The reflection interference fringes of multilayers thin film were tested by XRD,and the thickness information of the multilayers thin film was obtained by the Fast Fourier Transform(FFT)method.The chemical composition and longitudinal distribution of the film layers were obtained through XPS depth profiling,thus the structure of the multilayers film was fully characterized.The characterized sample was a transparent flexible conductive film with unknown composition and structure.Based on XPS and XRD analysis results,the characterized thin film was a three-layers composite film structure,with the first surface layer composed of SnO_(2),In_(2)O_(3),TiO_(2)and ZnO,and a thickness of 42.6 nm.The intermediate layer consisted of 19.2 nm Ag nanowires.The substrate side layer was composed of ZnO,In_(2)O_(3)and TiO_(2),with a thickness of 59.0 nm.This method completely avoids the complex modeling process and its uncertainty,and is very convenient and fast to characterize the multilayers thin film structure,including the thickness,composition and stacking sequence,etc.This method is of great significance in the research of thin films,quality control in production processes,and other aspects.
作者 张少鸿 莫家媚 苏秋成 ZHANG Shaohong;MO Jiamei;SU Qiucheng(Guangzhou Institute of Energy Conversion,Chinese Academy of Sciences,Guangzhou,Guangdong 510640,China)
出处 《中国无机分析化学》 北大核心 2025年第1期118-125,共8页 Chinese Journal of Inorganic Analytical Chemistry
基金 国家自然科学基金青年科学基金资助项目(51802305)。
关键词 X射线光电子能谱(XPS) X射线衍射(XRD) 薄膜厚度 深度剖析 X射线反射率(XRR) 快速傅里叶变换(FFT) X-ray photoelectron spectrometer(XPS) X-ray diffractometer(XRD) thin-film thickness depth profiling X-ray reflectivity(XRR) fast Fourier transform(FFT)
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