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椭圆偏振光谱测量技术及其在薄膜材料研究中的应用

朱绪丹 张荣君 郑玉祥 王松有 陈良尧

朱绪丹, 张荣君, 郑玉祥, 王松有, 陈良尧. 椭圆偏振光谱测量技术及其在薄膜材料研究中的应用[J]. 中国光学(中英文), 2019, 12(6): 1195-1234. doi: 10.3788/CO.20191206.1195
引用本文: 朱绪丹, 张荣君, 郑玉祥, 王松有, 陈良尧. 椭圆偏振光谱测量技术及其在薄膜材料研究中的应用[J]. 中国光学(中英文), 2019, 12(6): 1195-1234. doi: 10.3788/CO.20191206.1195
ZHU Xu-dan, ZHANG Rong-jun, ZHENG Yu-xiang, WANG Song-you, CHEN Liang-yao. Spectroscopic ellipsometry and its applications in the study of thin film materials[J]. Chinese Optics, 2019, 12(6): 1195-1234. doi: 10.3788/CO.20191206.1195
Citation: ZHU Xu-dan, ZHANG Rong-jun, ZHENG Yu-xiang, WANG Song-you, CHEN Liang-yao. Spectroscopic ellipsometry and its applications in the study of thin film materials[J]. Chinese Optics, 2019, 12(6): 1195-1234. doi: 10.3788/CO.20191206.1195

椭圆偏振光谱测量技术及其在薄膜材料研究中的应用

doi: 10.3788/CO.20191206.1195
基金项目: 

国家自然科学基金资助项目 11674062

国家自然科学基金资助项目 61775042

国家自然科学基金资助项目 11174058

国家自然科学基金资助项目 61575048

国家自然科学基金资助项目 69425004

国家自然科学基金资助项目 69178007

国家自然科学基金资助项目 19174013

详细信息
    作者简介:

    朱绪丹(1995—), 女, 湖北荆门人, 博士研究生, 2017年于电子科技大学获得学士学位, 主要从事椭圆偏振光谱检测薄膜光学性质的研究。E-mail:19110720016@fudan.edu.cn

    张荣君(1972—),男,河南信阳人,博士,研究员/教授,博士生导师,主要从事信息功能材料的光学性质、光谱分析系统与光电子器件等方面研究。E-mail:rjzhang@fudan.edu.cn

  • 中图分类号: O484.5;O433.1

Spectroscopic ellipsometry and its applications in the study of thin film materials

Funds: 

National Natural Science Foundation of China 11674062

National Natural Science Foundation of China 61775042

National Natural Science Foundation of China 11174058

National Natural Science Foundation of China 61575048

National Natural Science Foundation of China 69425004

National Natural Science Foundation of China 69178007

National Natural Science Foundation of China 19174013

More Information
  • 摘要: 椭圆偏振光谱测量技术通过测量线偏振光经材料表面反射后光的相对振幅与相位改变量计算得到椭偏参数,再通过椭偏参数的拟合获取样品光学性质。由于其具有非接触、高灵敏度、非破坏性等优势,广泛应用于物理、化学、材料科学和微电子等方面,是一种不可或缺的光学测量手段。本文首先简要回顾了该技术的发展历程,接着阐述了传统椭偏仪的基本原理,按照测量原理的不同可将椭偏仪分为消光式和光度式。随后,本文简单介绍了一些常用椭偏仪的基本架构、测量原理和相关应用,并比较了他们的优缺点,重点展示了复旦大学研制的双重傅立叶变换红外椭偏光谱系统。然后按照椭偏参数处理的基本步骤:测量、建模与拟合3个方面,阐述了其过程,详细剖析了参数拟合所使用的各种光学色散模型,同时通过应用实例介绍了各色散模型的应用情况。最后,对未来椭偏技术的发展方向进行了展望。

     

  • 图 1  1941年至今主题包含“ellipsometry”(椭偏技术)的论文发表情况统计。(a)论文发表篇数统计,(b)发表论文研究方向统计图。(数据来源:Isi Web of Science)

    Figure 1.  Statistical analysis of published papers with the topic of 'ellipsometry' from 1941 to the present. (a)Publication statistics of papers, (b)research direction of published papers. (Source:ISI Web of Science)

    图 2  椭偏仪测试原理示意图[34]

    Figure 2.  Measurement principle of ellipsometry[34]

    图 3  偏振光在介质界面处的反射与折射。(a)s光,(b)p光[34]

    Figure 3.  Reflection and refraction of polarized light at the interface of the medium. (a)s polarization, and (b)p polarization[34]

    图 4  PCSA型消光式椭偏仪结构示意图(图中ψ=45°,Δ=90°,探测器检测此刻为消光状态)[34]

    Figure 4.  Schematic diagram of PCSA null ellipsometry(The (ψ, Δ) values of a sample are assumed to be ψ=45° and Δ=90°. In this measurement, the detected light intensity is zero)[34]

    图 5  RAE光度式椭偏仪示意图[34]

    Figure 5.  Optical configurations of RAE[34]

    图 6  RCE光度式椭偏仪示意图[34]

    Figure 6.  Optical configurations of RCE[34]

    图 7  双重傅立叶变换红外椭偏光谱系统。(a)系统整体结构示意图,1.偏振器;2.分析仪;3.步进电机;4.检测臂旋转平台;5.样品旋转平台;6.样品安装板;7.固定镜;8.移动镜[49],(b)RAP型椭偏仪原理图(其中P和A的方位角相对s轴顺时针旋转)[50]

    Figure 7.  Apparatus configuration of the infrared double-Fourier spectro-ellipsometer. (a)System overall structure diagram, 1.polarizer, 2.analyzer, 3.stepping motors, 4.rotating stage of detection arm, 5.rotating stage of sample, 6.sample mounting plate, 7.fixed mirrors, 8.moving mirror[49], (b)optical configuration of the RAP ellipsometric system(in which the azimuthal angles of the rotating P and A are clockwise to the s axis)[50]

    图 8  PME光度式椭偏仪示意图[34]

    Figure 8.  Optical configuration of PME[34]

    图 9  D.E.Aspnes等人设计的椭偏光谱仪结构示意图[56]

    Figure 9.  Schematic diagram of the optical system of the instrument designed by D. E. Aspnes et al.[56]

    图 10  G.Jin等人设计的成像椭偏仪示意图[59]

    Figure 10.  Schematic diagram of an imaging ellipsometer designed by G.Jin et al.[59]

    图 11  椭圆偏振光谱分析Sn薄膜的光学性质。(a)65°, 70°, 75°入射时测得的Sn薄膜椭偏参数,(b)Sn薄膜的折射率n和消光系数k与波长的关系[65]

    Figure 11.  Optical properties of Sn thin films studied by spectroscopic ellipsometry. (a)Spectral ellipsometry parameters of Sn films measured at 65°, 70°, and 75° at room temperature, (b)refractive index n and extinction coefficient k of the Sn film vary with wavelength[65]

    图 12  椭圆偏振光谱分析得到的~1 μm厚石墨x向和z向的复折射率(此时z向被认为是普通材料)[66]

    Figure 12.  Complex refractive indexes in the x- and z-directions of ~1 μm thick graphite obtained by ellipsometry(optical constants of graphite with z-component being treated as a general material)[66]

    图 13  椭偏分析材料光学性质的基本流程[68]

    Figure 13.  Basic flow chart of the optical properties of materials analyzed by ellipsometric analysis method[68]

    图 14  逐点椭偏参数反演方法分析椭偏参数的基本流程[70]

    Figure 14.  Basic flow chart of ellipsometric parameters analyzed by point-by-point ellipsometric parameter inversion method[70]

    图 15  逐点椭偏参数反演方法分析ZrO2超薄膜。(a)ZrO2超薄膜的光学模型,(b)点对点分析中使用的简化光学模型,(c)厚度为2.72 nm的ZrO2超薄膜在入射光子能量为3~6 eV内的ε2[72]

    Figure 15.  Analysis results of ultrathin ZrO2 films by point-by-point method. (a)Optical model of ZrO2 samples, (b)simplified one for point-by-point analysis in this work, (c)imaginary model of dielectric constants of the effective ZrO2 film with a thickness of 2.72 nm when incident photon energy is 3~6 eV range[72]

    图 16  逐点椭偏参数反演方法分析WS2超薄膜。(a)WS2超薄膜的光学模型,(b)和(c)分别是点对点拟合得到的WS2超薄膜复介电函数实部ε1和虚部ε2(入射光子能量范围为1.2~6.3 eV,S1、S2和S3分别代表溅射时间为20、50和70 s的3种样品)[73]

    Figure 16.  Analysis results of ultrathin WS2 films by point-by-point method. (a)Optical model of WS2 samples, (b) and (c) are real part ε1 and imaginary part ε2 for dielectric function extracted from point-by-point fitting respectively. (the photon energy range is 1.2~6.3 eV, S1, S2 and S3 are represeroted the sample for the sputtering times, 20 s, 50 s, and 70 s, respectively)[73]

    图 17  束缚电子的受力分析示意图[34]

    Figure 17.  Force analysis diagram of bound electron[34]

    图 18  NiOx, PEDOT:PSS和体异质结(BHJ)太阳能电池的复折射率[83]

    Figure 18.  Index of refraction, n and extinction coefficient, k for NiOx, PEDOT:PSS and BHJ solar cells[83]

    图 19  GO薄膜的椭偏光谱分析。(a)Lorentz模型3个振子中心能量按退火温度线性拓展(C1(方块),C2(圆圈),C3(三角));(b)λ=600 nm时不同退火温度下本征GO薄膜和束缚水的GO综合体系的光学常数曲线(本征GO薄膜的nGO(1),kGO(3),混合体系n(2),k(4),阴影部分为除去束缚水层的温度区间)[84]

    Figure 19.  Ellipsometric spectral analysis of GO thin films. (a)Three vibrator center energies of Lorentz model linearly expand according to annealing temperature (C1(squares), C2(circles), and C3(triangles)), (b)optical constant curve of GO synthesis system of intrinsic GO film and bound water nGO(1), kGO(3), and total n(2), k(4) vs. Tann for λ=600 nm. Dashed region denotes temperature interval where water is expelled[84]

    图 20  550 nm处沉积在Si衬底的Ta2O5薄膜折射率实验值和理论值随薄膜厚度的变化[81]

    Figure 20.  Experimental and theoretical refractive indices at 550 nm for the Ta2O5 films deposited on Si vary with thickness[81]

    图 21  椭偏光谱分析得到的~1μm厚石墨x向和z向的复折射率(此时z向被认为是Cauchy材料)[66]

    Figure 21.  Complex refractive indexes in the x- and z-directions of ~1 μm thick graphite obtained by ellipsometry(optical constants of graphite with z-component being treated as a Cauchy material)[66]

    图 22  采用多角度椭圆偏振光谱法分析制备在硅衬底上的石墨烯薄片的光学常数(x向)[66]

    Figure 22.  Reconstructed x-component optical constants of graphene prepared on silicon substrate using multi-angle spectroscopic ellipsometry[66]

    图 23  400 ℃退火后不同厚度的TiO2超薄膜复折射率谱。(a)折射率n,(b)消光系数k。(图(a)的插图显示了峰位置与ALD循环数的关系,图(b)的插图显示了在400 ℃下退火后不同厚度的TiO2超薄膜的(αE)1/2vs.E图)[95]

    Figure 23.  Complex refractive index spectra for TiO2 ultrathin films with different thicknesses after annealing at 400 ℃. (a)Refractive index n spectra, (b)extinction coefficient k spectra.(The insert of (a) shows plot of peak position versus ALD cycles. The insert of (b) shows plots of (αE)1/2vs. E for TiO2 ultrathin films with different thicknesses after annealing at 400 ℃)[95]

    图 24  Al2O3/ZnO纳米层状结构示意图[96]

    Figure 24.  Structure diagram of the Al2O3/ZnO nanolaminates[96]

    图 25  用于椭偏分析多层膜样品的光学模型[96]

    Figure 25.  Optical model of samples for SE analysis[96]

    图 26  生长在SiO2/Si衬底上的纳米层状结构多层膜系统的光学常数。(a)折射率n; (b)消光系数k[96]

    Figure 26.  Optical constants of nanolaminates grown on SiO2/Si substrate. (a)Refractive index n; (b)extinction coefficient k[96]

    图 27  CH3NH3PbI3钙钛矿薄膜椭偏分析。(a)作为光学模型的样品结构,(b)复折射率光谱[98]

    Figure 27.  SE analysis of CH3NH3PbI3 perovskite thin films. (a)Sample structure used for the optical model, (b)refractive index[98]

    图 28  在石英衬底上CH3NH3PbI3膜的表面粗糙层三层膜结构光学模型的示意图[99]

    Figure 28.  Schematic of the three-layer surface roughness model of the CH3NH3PbI3 film on a quartz substrate[99]

    图 29  计算得到CH3NH3PbI3材料的复折射率谱[99]

    Figure 29.  n(λ) and k(λ) results of CH3NH3PbI3 material[99]

    图 30  不同水合物含量的CH3NH3PbI3薄膜复折射率谱。(a)复折射率实部n,(b)复折射率虚部k[101]

    Figure 30.  Complex refractive index of CH3NH3PbI3 film with different levels of hydration water. (a)The refractive index n, (b)the extinction coefficient k[101]

    图 31  半导体中自由载流子吸收示意图。(a)自由载流子吸收,(b)点缺陷对自由载流子的散射[34]

    Figure 31.  Representation of free-carrier absorption in a semiconductor. (a)Free-carrier absorption, (b)scatter between free-carrier and point defect[34]

    图 32  不同厚度纳米金薄膜的复介电函数。(a)实部,(b)虚部[106]

    Figure 32.  Dielectric functions of the nano-thin Au film with different thicknesses. (a)Real parts, (b)imaginary parts[106]

    图 33  指甲的光学常数和实验值(垂直虚线表示从水合作用到脱水作用的变化)[67]

    Figure 33.  Optical constants and experimental values of finger nail.(The vertical dashed line marks the change from hydration to dehydration)[67]

    图 34  有效介质近似理论的物理模型。(a)Maxwell-Garnett模型; (b)Bruggeman模型[34]

    Figure 34.  Physical models for effective medium theories. (a)Maxwell Garnett, (b)Bruggeman[34]

    图 35  β-Sn薄膜样品的光学模型示意图[113]

    Figure 35.  Schematic of the layer structure for the β-Sn film sample[113]

    图 36  用于分析(a)薄膜和(b)纳米结构的椭偏技术和其他表征技术“合作情况”的分布统计图(AFM:原子力显微镜;SEM:扫描电子显微镜;TEM:透射电子显微镜;XPS:X射线光电子能谱;XRD:X射线衍射光谱)[114]

    Figure 36.  Distribution of techniques corroborating spectroscopic ellipsometry(SE) for analysis of (a)thin films and (b)nanostructures(AFM:atomic force microscopy; SEM:scanning electron microscopy; TEM:transmission electron microscopy; XPS:X-ray photoelectron spectroscopy; XRD:X-ray diffraction)[114]

    图 37  基于光纤的椭偏仪结构图[126]

    Figure 37.  Structural diagram of fiber-based ellipsometry[126]

    图 38  (左上)THz FDS椭偏仪的俯视图;(右下)THz FDS椭偏仪的技术制图的俯视图与主要组件(不包括吸波泡沫板和外壳)[136]

    Figure 38.  (Top left) Photograph(top view) of the THz FDS ellipsometer.(Bottom right) technical drawing(top view) of the THz FDS ellipsometer with major components indicated and without absorbing foam sheets and housing[136]

    图 39  双旋转补偿器型穆勒矩阵成像椭偏仪测量原理示意图[146]

    Figure 39.  Scheme of the dual rotating compensator Mueller matrix imaging ellipsometer[146]

    表  1  几种光度式椭偏仪优缺点总结[34]

    Table  1.   Advantages and disadvantages of several photometric ellipsometers[34]

    椭偏仪结构 优点 缺点
    RAE/RPE
    (不含补偿器)
    ①结构简单 ①Stokes的S3分量测试受限(-180°≤Δ<0°)
    ②工作在消光模式 ②在Δ等于0°和180°处有较大的测量误差
    RAE/RPE ①椭偏参数(ψΔ)在全光谱范围可测 ①相比RAE测试时间更长
    ②可以测量去极化谱 ②相比RAE结构更复杂
    ③全光谱范围椭偏参数测量敏感度相同
    RCE ①椭偏参数(ψΔ)在全光谱范围可测 相比RAE结构更复杂
    ②可以测量去极化谱
    ③全光谱范围椭偏参数测量敏感度相同
    PME ①测试快速 ①单次测量无法同时测试Stokes的S1S2分量
    ②在远红外波段可以实时测试 ②椭偏参数(ψΔ)在某些区域测试误差大
    ③可以测量去极化谱
    下载: 导出CSV
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  • 收稿日期:  2018-07-04
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