微纳尺度表征的俄歇电子能谱新技术
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摘要
随着纳米结构材料的广泛应用,新型微纳尺度表征技术成为纳米科学技术的重要组成部分。发展在纳米尺度下的各种检测与表征手段,以用于观测纳米结构材料的原子、电子结构,和测量各种纳米结构的力、电、光、磁等特性,日益引起人们的重视。针对目前广泛使用的各种光子谱技术、X射线衍射和精细吸收谱、高分辨的电子显微术等技术的局限性,本论文基于以电子束为探针的俄歇电子能谱(Auger electron spectroscopy),发展了纳米尺度的检测与表征新技术。
本论文从俄歇电子能谱基础出发,基于俄歇电子物理机制,着重讨论价带俄歇谱的理论表述和物理意义。采用第一性原理计算方法,模拟GaN和ZnO基半导体不同物理条件下的理论价带俄歇谱;通过实验测量相关半导体的俄歇电子能谱,分别建立材料应力、电荷及电场分布、结构和导电类型等宏观参量的微纳尺度测量技术。主要取得如下研究成果:
提出俄歇电子能谱广义位移的概念,把所有能导致俄歇价电子谱的动能位移及其谱峰相对强度改变的因素(包括化学、物理等)都统一起来。建立了材料微纳米尺度宏观特性的俄歇价电子能谱表征新技术。其主要包括:采用第一性原理计算各种环境下的电子结构;卷积相关价电子态密度;拟合实验谱确定组合系数,模拟计算理论的俄歇价电子能谱的广义位移;标定宏观参量与俄歇电子谱广义位移的定量关系;测量实际材料表面的俄歇价电子能谱,根据标定关系曲线获得相应的宏观参量。该技术兼备测量宏观参量的简便性和俄歇电子能谱固有的高空间分辨率,使得其定量测量材料的微纳结构特性具有明显的优势。
建立了纳米微区应力测量技术。通过第一性原理计算模拟GaN在不同双轴压应力场中的电子结构,根据拟合实验谱确定的组合系数,模拟出不同应变/应力下的N KVV的理论俄歇价电子谱;标定应变/应力与俄歇电子谱广义位移的定量关系。以侧向外延GaN表面和剖面不同结构区域应变/应力分布为对象,测量N KVV谱广义位移及其局域应变/应力分布。所测结果与通过Raman散射E_2模移动测量确定的结果相吻合,完全符合失配应力逐渐释放的机制;而且观察到传统上只能靠理论的应力分布模拟方能得到的细节,说明建立的俄歇价电子能谱测量应力技术的正确性和精确性。
建立了非接触性纳米微区电学测量技术。利用第一性原理方法分别计算了不同Al组分的Al_xGa_(1-x)表面的N原子周围局域电子密度和相应的态密度,模拟不同电子密度N KVV论俄歇价电子谱主峰强度N_(pp)与次峰的N_(sp)的比值,发现了比值随电子密度的增加而线性增加的现象。以N_(pp)/N_(sp)相对比与局域电荷密度的关系曲线作为标定电子密度与俄歇电子谱广义位移(谱峰强度变化)的定量关系。以GaN/Al_xGa_(1-x)N/GaN异质结构电荷分布为对象,测量N KVV谱峰相对强度变化及其局域电荷密度分布。精确获得了GaN/Al_xGa_(1-x)N/GaN异质两界面处电子和空穴的二维电子气分布,证明了界面净电荷的存在,与采用俄歇芯态电子能谱的能量移动确定的局域电场变化的结果一致。
建立了纳米微区结构相的测量分析技术。采用俄歇价电子谱的理论和实验方法,确定纤锌矿和闪锌矿结构相GaN的俄歇价电子谱广义位移特征,建立了纳米微区结构相的测量分析技术。将建立的纳米微区结构相的测量分析技术应用于四脚ZnO的脚和芯的结构测量,证明脚处的纤锌矿结构和芯部的闪锌矿结构。结果与Raman谱的实验和计算相符合,证明了俄歇价电子能谱确定微区晶体结构相方法的正确性,可应用于纳米尺度结构相的确定。
Inspired by the rapid progresses and wide applications of nanostructure materials, high-resolution characterization techniques have played the important role in nanoscience.To investigate properties,e.g.,atomic and electronic structures,force field, electrical features,optical properties,magnetic responses et al.in nano-materials and nano-devices,exploration and development of new methods and techniques of nanoscale characterizations becomes more and more crucial.Although conventional tools such as XRD,XAFS,Raman spectroscopy,SEM,HRTEM,and STM have been widely used in various nanoscale investigations,however,ever and again they meet their ends in approaching many nano-scale characterizations.Therefore,built upon the Auger electron spectroscopy with electron beam probe,here we report the establishments of advanced nanoscale,intrinsic,and non-contact characterization methods and techniques.
In this thesis,based on the fundamentals of Auger electron spectroscopy,the physical essence was discussed and the theoretical expression of valence-band Auger spectrum was described.By first-principles calculations,the electronic structures of GaN and ZnO were obtained and the theoretical Auger spectra under different physical environments were simulated.In practice,a couple of advanced nanoscale characterization techniques for important physical quantities,including local stress field, intrinsic local charges,internal electric field,local structural phase,conducting type et al.,have been established on Auger electron spectroscopy.Main approaches in our works are following:
In theory,the concept of General Auger Shift were proposed for the first time. Based on this concept,it unifies all(including the chemical,physical,ect.)factors leading to the energetic shift and the lineshape deformation of the valence-band Auger spectra.Thus,the methods of novel measurements of important quantities in materials were setup:(Ⅰ)Calculations of electronic structures under different environments;(Ⅱ) Fitting of the theoretical Auger spectrum by convolution integration of density of electron states;(Ⅲ)Calibration of relationship between the specific quantities with the General Auger Shift;(Ⅳ)Characterization of specific object by surveying valence-band Auger spectra at local area of interest and obtaining the properties.The sensitivity and high-resolution of these AES techniques shows their power in the investigations for weak signals and local properties for nano-structured materials.
Establishment of measurement of local stress field in nanoscale.The electron densities of states(DOS)of GaN under different biaxial stress field were calculated. The theoretical Auger spectra N KVV of various stress conditions were obtained by convoluting the DOS and fitting the experimental spectra.Then the relation between biaxial stress and the energetic shift of N KVV peak was determined for measurement use.In practice,the mapping of stress field distributions of epitaxial-lateral-overgrowth GaN was carried out and the value on GaN surface is consistent well with that by Raman scattering.These results reveal the refined distribution of stress field,which could only be simulated by theoretical methods before,and the complex mechanism of stress release in the lateral region.The accuracy and pertinence of this technique was verified.
Establishment of non-contact nanoscale measurement of local electrical properties (local charge and local electric field).The local electron concentration of N atom in Al_xGa_(1-x)N with different Al mole fraction were calculated and the concentration was found to increase with the increase of Al fraction.At the same time,acquirement of N KVV Auger spectra in different Al_xGa_(1-x)N showed the proportional relation of peak height ratio N_(pp)N_(sp)with the Al mole fration,also.Therefore,the calibration curve of N_(pp)/N_(sp)as a function of local charge concentration was obtained.With this approach, the measurement of internal electric field was established.Applying in heterointerfaces of GaN/Al_xGa_(1-x)N/GaN,the embedded polarization charges and distribution of internal electric field at the interfaces were precisely detected,which demonstrates the existence and accurate value of 2 dimension electron gas at different interfaces.
Establishment of techniques of structural phase identification for local area.With theoretical and experimental methods,the relation of the General Shift of valence-band Auger spectrum was determined for zinc-blend and wurtzite GaN structures.The techniques of structural identification for local nano-area were achieved.In applications, the complex structural phases of ZnO tetrapod nanocrystals were investigated and determined.The results showed the wurtzite and zinc-blend phase in the leg part and the core part,respectively,which also agreed well with the Raman spectra and calculation data.This approach proved the validity of this advanced measurement technique and its capability in the phase determination for nano-structured systems.
本论文从俄歇电子能谱基础出发,基于俄歇电子物理机制,着重讨论价带俄歇谱的理论表述和物理意义。采用第一性原理计算方法,模拟GaN和ZnO基半导体不同物理条件下的理论价带俄歇谱;通过实验测量相关半导体的俄歇电子能谱,分别建立材料应力、电荷及电场分布、结构和导电类型等宏观参量的微纳尺度测量技术。主要取得如下研究成果:
提出俄歇电子能谱广义位移的概念,把所有能导致俄歇价电子谱的动能位移及其谱峰相对强度改变的因素(包括化学、物理等)都统一起来。建立了材料微纳米尺度宏观特性的俄歇价电子能谱表征新技术。其主要包括:采用第一性原理计算各种环境下的电子结构;卷积相关价电子态密度;拟合实验谱确定组合系数,模拟计算理论的俄歇价电子能谱的广义位移;标定宏观参量与俄歇电子谱广义位移的定量关系;测量实际材料表面的俄歇价电子能谱,根据标定关系曲线获得相应的宏观参量。该技术兼备测量宏观参量的简便性和俄歇电子能谱固有的高空间分辨率,使得其定量测量材料的微纳结构特性具有明显的优势。
建立了纳米微区应力测量技术。通过第一性原理计算模拟GaN在不同双轴压应力场中的电子结构,根据拟合实验谱确定的组合系数,模拟出不同应变/应力下的N KVV的理论俄歇价电子谱;标定应变/应力与俄歇电子谱广义位移的定量关系。以侧向外延GaN表面和剖面不同结构区域应变/应力分布为对象,测量N KVV谱广义位移及其局域应变/应力分布。所测结果与通过Raman散射E_2模移动测量确定的结果相吻合,完全符合失配应力逐渐释放的机制;而且观察到传统上只能靠理论的应力分布模拟方能得到的细节,说明建立的俄歇价电子能谱测量应力技术的正确性和精确性。
建立了非接触性纳米微区电学测量技术。利用第一性原理方法分别计算了不同Al组分的Al_xGa_(1-x)表面的N原子周围局域电子密度和相应的态密度,模拟不同电子密度N KVV论俄歇价电子谱主峰强度N_(pp)与次峰的N_(sp)的比值,发现了比值随电子密度的增加而线性增加的现象。以N_(pp)/N_(sp)相对比与局域电荷密度的关系曲线作为标定电子密度与俄歇电子谱广义位移(谱峰强度变化)的定量关系。以GaN/Al_xGa_(1-x)N/GaN异质结构电荷分布为对象,测量N KVV谱峰相对强度变化及其局域电荷密度分布。精确获得了GaN/Al_xGa_(1-x)N/GaN异质两界面处电子和空穴的二维电子气分布,证明了界面净电荷的存在,与采用俄歇芯态电子能谱的能量移动确定的局域电场变化的结果一致。
建立了纳米微区结构相的测量分析技术。采用俄歇价电子谱的理论和实验方法,确定纤锌矿和闪锌矿结构相GaN的俄歇价电子谱广义位移特征,建立了纳米微区结构相的测量分析技术。将建立的纳米微区结构相的测量分析技术应用于四脚ZnO的脚和芯的结构测量,证明脚处的纤锌矿结构和芯部的闪锌矿结构。结果与Raman谱的实验和计算相符合,证明了俄歇价电子能谱确定微区晶体结构相方法的正确性,可应用于纳米尺度结构相的确定。
Inspired by the rapid progresses and wide applications of nanostructure materials, high-resolution characterization techniques have played the important role in nanoscience.To investigate properties,e.g.,atomic and electronic structures,force field, electrical features,optical properties,magnetic responses et al.in nano-materials and nano-devices,exploration and development of new methods and techniques of nanoscale characterizations becomes more and more crucial.Although conventional tools such as XRD,XAFS,Raman spectroscopy,SEM,HRTEM,and STM have been widely used in various nanoscale investigations,however,ever and again they meet their ends in approaching many nano-scale characterizations.Therefore,built upon the Auger electron spectroscopy with electron beam probe,here we report the establishments of advanced nanoscale,intrinsic,and non-contact characterization methods and techniques.
In this thesis,based on the fundamentals of Auger electron spectroscopy,the physical essence was discussed and the theoretical expression of valence-band Auger spectrum was described.By first-principles calculations,the electronic structures of GaN and ZnO were obtained and the theoretical Auger spectra under different physical environments were simulated.In practice,a couple of advanced nanoscale characterization techniques for important physical quantities,including local stress field, intrinsic local charges,internal electric field,local structural phase,conducting type et al.,have been established on Auger electron spectroscopy.Main approaches in our works are following:
In theory,the concept of General Auger Shift were proposed for the first time. Based on this concept,it unifies all(including the chemical,physical,ect.)factors leading to the energetic shift and the lineshape deformation of the valence-band Auger spectra.Thus,the methods of novel measurements of important quantities in materials were setup:(Ⅰ)Calculations of electronic structures under different environments;(Ⅱ) Fitting of the theoretical Auger spectrum by convolution integration of density of electron states;(Ⅲ)Calibration of relationship between the specific quantities with the General Auger Shift;(Ⅳ)Characterization of specific object by surveying valence-band Auger spectra at local area of interest and obtaining the properties.The sensitivity and high-resolution of these AES techniques shows their power in the investigations for weak signals and local properties for nano-structured materials.
Establishment of measurement of local stress field in nanoscale.The electron densities of states(DOS)of GaN under different biaxial stress field were calculated. The theoretical Auger spectra N KVV of various stress conditions were obtained by convoluting the DOS and fitting the experimental spectra.Then the relation between biaxial stress and the energetic shift of N KVV peak was determined for measurement use.In practice,the mapping of stress field distributions of epitaxial-lateral-overgrowth GaN was carried out and the value on GaN surface is consistent well with that by Raman scattering.These results reveal the refined distribution of stress field,which could only be simulated by theoretical methods before,and the complex mechanism of stress release in the lateral region.The accuracy and pertinence of this technique was verified.
Establishment of non-contact nanoscale measurement of local electrical properties (local charge and local electric field).The local electron concentration of N atom in Al_xGa_(1-x)N with different Al mole fraction were calculated and the concentration was found to increase with the increase of Al fraction.At the same time,acquirement of N KVV Auger spectra in different Al_xGa_(1-x)N showed the proportional relation of peak height ratio N_(pp)N_(sp)with the Al mole fration,also.Therefore,the calibration curve of N_(pp)/N_(sp)as a function of local charge concentration was obtained.With this approach, the measurement of internal electric field was established.Applying in heterointerfaces of GaN/Al_xGa_(1-x)N/GaN,the embedded polarization charges and distribution of internal electric field at the interfaces were precisely detected,which demonstrates the existence and accurate value of 2 dimension electron gas at different interfaces.
Establishment of techniques of structural phase identification for local area.With theoretical and experimental methods,the relation of the General Shift of valence-band Auger spectrum was determined for zinc-blend and wurtzite GaN structures.The techniques of structural identification for local nano-area were achieved.In applications, the complex structural phases of ZnO tetrapod nanocrystals were investigated and determined.The results showed the wurtzite and zinc-blend phase in the leg part and the core part,respectively,which also agreed well with the Raman spectra and calculation data.This approach proved the validity of this advanced measurement technique and its capability in the phase determination for nano-structured systems.
引文
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