Investigation of the Correlation between Texture and Microstrucure on a Submicrometer Scale in the TEM

In recent years the investigation of local texture and microstructure by analysis of electron backscatter diffraction patterns (EBSP) in the SEM has become a very powerful and popular method. With the introduction of SEM with field emission guns (FEG) the spatial resolution of EBSP measurements could be enhanced from 500 nm with a tungsten emitter to better than 50 nm. This evolution of SEM techniques raises the question whether transmission electron microscopy (TEM) still has fields of application in texture research. The present article answers this question with a clear “yes” and presents three examples of investigations where TEM is indispensable. The three examples comprise the investigation of the correlation between dislocation structure and deformation texture, a study on nucleation mechanisms of recrystallization in highly deformed metals and the investigation of microtexture and microstructure in nanocrystalline materials. Together with the presentation of these cases some of the necessary measurement techniques are described briefly. It is shown that TEM has to be applied when highest spatial resolution of orientation determination and imaging and high accuracy of orientation determination are to be reached, when the three‐dimensional and quantitative characterization of lattice defects is required or when materials with a high density of lattice defects are to be investigated.     

Convergent beam electron diffraction — A novel technique for materials characterisation at sub-microscopic levels

This paper presents a review of the developments in Convergent Beam Electron Diffraction (CBED), a technique widely used for determination of structure, symmetry details and atom positions in a crystal as small as 20Å in size. The understanding of this technique is related to the rapid advancements in the field of transmission electron microscopy with respect to development of coherent, finer probes and electron optics for higher spatial resolution. Energy filtering devices enable imaging of several finer features in the CBED pattern from which useful information about a crystal can be obtained. These include (i) three-dimensional information about the reciprocal lattice, (ii) point and space group symmetry details, (iii) lattice parameter from regions as fine as 2 nm, (iv) atom positions within a unit cell and (v) defects in crystals and (vi) thickness. Due to abundant data obtained from microscopic regions, this technique is unique and finds wide application in materials characterization. It has been used for studying problems like identification of the presence of lattice strain, identification of point defects etc. in a material used often in the nuclear industry, namely 9Cr-1Mo steel. The present paper provides the current status of CBED starting from its historical development, the information that can be obtained and its use in a variety of applications.     

二极溅射沉积Fe-N-O薄膜的形貌与结构分析

利用二极溅射的方法在不同衬底上沉积了Fe N O薄膜。通过扫描电子显微镜(SEM)、光电子能谱(XPS)和透射电子显微镜(TEM)等先进实验分析手段对二极溅射沉积Fe N O薄膜的形貌与结构进行了分析。XPS和TEM的结果表明,薄膜的主要成分为FeO和少量的Fe16N2多晶体组成,生长上存在择优取向;表面均匀、致密、平整,晶粒大小在50nm左右。     

改进 ICVI工艺制备 C/C复合材料的基体织构研究

利用偏振光显微镜(PLM)和高分辨透射电镜(HRTEM)从微米到纳米尺度研究了改进等温化学气相沉积(ICVI)技术制备的C/C复合材料基体热解炭织构和精细结构特征.结果表明:纤维周围有3层不同织构的热解炭,由纤维向外,分别为光滑层、粗糙层和暗层.基体与纤维之间以及不同织构基体间的界面结合较好,高织构热解炭内有微裂纹存在,并且裂纹在界面处终止扩展,或以桥连的形式扩展.不同织构热解炭在HRTEM下晶格条纹的近程和长程的择优取向度有明显区别.     

Discrimination and mapping of phase distributions by automated crystal orientation measurement

Abstract

Automated crystal orientation measurement/mapping (ACOM) in the SEM enables a fast phase discrimination and the automated acquisition of phase distribution maps at submicrometre resolution, if the phases belong to different Laue groups or if their lattice constants are at least significantly different. The database can further be used for quantitative determination of phase contents, phase boundary characterisation, and mesoscale texture analysis for each phase, such as crystal orientation mapping (COM), texture analysis (orientation density function, pole figures, misorientation distribution function), characterisation of grain and phase boundaries, and orientation stereology.     

A high resolution electron microscopic study of the microstructure in rapidly solidified Al-Li-Cu-Mg-Zr alloys

The microstructure in rapidly solidified Al-Li-Cu-Mg-Zr alloys has been reexamined by transmission electron microscopy (TEM). The results show that the weakening intermetallic phases, e.g. hexagonal, Z, face centred cubic (f.c.c), T, and tetragonal, H, (new phase) phases, exist in alloys with relatively high contents of Mg besides the strengthening phases. The sizes of these weakening intermetallic phases are on the scale of micrometres. The newly found tetragonal H phase, having parameters of a = 2.8 nm and c = 2.4 nm, was observed to coexist with the Z phase, and has a defined orientation relationship with the Z phase. High resolution images reveal that there are planar defects and 90 ° domains in the Z phase, multiple twins in the T phase, and two well defined crystallographic orientation relationships between the Z and T phases.     

Effect of downscaling nano-copper interconnects on the microstructure revealed by high resolution TEM-orientation-mapping

In this work, a recently developed electron diffraction technique called diffraction scanning transmission electron microscopy (D-STEM) is coupled with precession electron microscopy to obtain quantitative local texture information in damascene copper interconnects (1.8 μm-70 nm in width) with a spatial resolution of less than 5 nm. Misorientation and trace analysis is performed to investigate the grain boundary distribution in these lines. The results reveal strong variations in texture and grain boundary distribution of the copper lines upon downscaling. Lines of width 1.8 μm exhibit a strong <111> normal texture and comprise large micron-size grains. Upon downscaling to 180 nm, a {111}<110> bi-axial texture has been observed. In contrast, narrower lines of widths 120 and 70 nm reveal sidewall growth of {111} grains and a dominant <110> normal texture. The microstructure in these lines comprises clusters of small grains separated by high angle boundaries in the vicinity of large grains. The fraction of coherent twin boundaries also reduces with decreasing line width.     

Quantitative characterization of the composition, thickness and orientation of thin films in the analytical electron microscope

Compositional variations in thin films can introduce lattice-parameter changes and thus create stresses, in addition to the more usual stresses introduced by substrate-film mismatch, differential thermal expansion, etc. Analytical electron microscopy comprising X-ray energy-dispersive spectrometry within a probe-forming field-emission gun scanning transmission electron microscope (STEM) is one of the most powerful methods of composition measurement on the nanometer scale, essential for thin-film analysis. Recently, with the development of improved X-ray collection efficiencies and quantitative computation methods it has proved possible to map out composition variations in thin films with a spatial resolution approaching 1-2 nm. Because the absorption of X-rays is dependent on the film thickness, concurrent composition and film thickness determination is another advantage of X-ray microanalysis, thus correlating thickness and composition variations, either of which may contribute to stresses in the film. Specific phenomena such as segregation to interfaces and boundaries in the film are ideally suited to analysis by X-ray mapping. This approach also permits multiple boundaries to be examined, giving some statistical certainty to the analysis particularly in nano-crystalline materials with grain sizes greater than the film thickness. Boundary segregation is strongly affected by crystallographic misorientation and it is now possible to map out the orientation between many different grains in the (S)TEM.     

The structural and optical properties of ZnO nanowire arrays prepared by hydrothermal synthesis method

ZnO nanowire arrays have been grown on the ZnO film-coated silicon (100) substrates by hydrothermal method, and the deposited nanowires are found to have a uniform size distribution with sharp hexagonal-shaped tips. The structural and optical properties of the nanowires were investigated using atomic force microscopy (AFM), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and cathodoluminescence (CL) techniques. The XRD and SEM results demonstrate that the well-aligned ZnO nanowires are single crystalline structure formed along the c-axis orientation. TEM analysis further confirms that the ZnO nanowires are highly preferred grown along the (002) crystal plane. The spacing between adjacent (002) lattice planes is estimated as 0.52 nm. The optical properties of the nanowires were measured using CL after annealing in oxygen and nitrogen atmospheres at 550 °C for various times. The CL spectra in the visible spectrum exhibit two weak deep-level emission bands that may be attributed to the intrinsic or extrinsic defects. It can be observed that the ZnO nanowires show different optical behaviors after various annealing times. The dependence of the optical properties on the annealing conditions is also discussed.     

Deformation and recrystallisation studied by EBSP: breakthroughs and limitations

Abstract

The use of microtexture investigations by the electron backscattering pattern (EBSP) technique in the SEM for investigations of plastic deformation and recrystallisation is described. The focus is on grain subdivision during deformation and on nucleation and growth during recrystallisation. Specific investigations in which the EBSP technique has been essential to achieve a scientific breakthrough are reviewed. Also the limitations of the EBSP technique are discussed and illustrated by examples of incorrect results which might have been accepted if the EBSP measurements had not been complemented by other methods.     

Evolution of Irradiation‐Induced Vacancy Defects in Boron Nitride Nanotubes

Irradiation‐induced vacancy defects in multiwalled (MW) boron nitride nanotubes (BNNTs) are investigated via in situ high‐resolution transmission electron microscope operated at 80 kV, with a homogeneous distribution of electron beam intensity. During the irradiation triangle‐shaped vacancy defects are gradually generated in MW BNNTs under a mediate electron current density (30 A cm^?2), by knocking the B atoms out. The vacancy defects grow along a well‐defined direction within a wall at the early stage as a result of the curvature induced lattice strain, and then develop wall by wall. The orientation or the growth direction of the vacancy defects can be used to identify the chirality of an individual wall. With increasing electron current density, the shape of the irradiation‐induced vacancy defects changes from regular triangle to irregular polygon.     

透射模式电子背散射衍射技术在纳米材料研究中的应用

为了提高电子背散射衍射技术的空间分辨率, 使之能够对纳米尺度的晶粒或超细粉末进行相鉴定和取向分析, 本研究通过自主设计的透射模式电子背散射衍射技术的样品台, 及调整EBSD探头位置及角度, 收集到清晰、完整的透射电子菊池衍射花样。研究了减薄块体样品厚度对透射电子菊池衍射花样的影响, 对减薄氧化锆涂层样品进行了t-EBSD面分布分析, 其结果的平均角度偏差(MAD)值仅为0.38, 成功鉴定出小于30 nm尺度的纳米氧化锆涂层立方相; 将超声分散后的纳米TiO₂粉体滴在铜网上, 采用t-EBSD对纳米颗粒进行点分析, 成功鉴定了锐钛矿相和金红石相TiO₂, 其中纳米锐钛矿TiO₂粉体的最小尺寸为20 nm左右, 使得扫描电镜中相鉴定的最小分辨率从目前的约100 nm提高到小于30 nm, 大大拓展了电子背散射衍射技术在纳米材料研究中的应用范围。     

Laser surface modification of metals and alloys

In order to understand the properties of solids, the materials scientist frequently needs to characterize the microstructure of a material on as fine a scale as possible. Characterization here is used in its most general sense, i.e. to describe as completely as possible the morphology, crystallography and elemental composition of the material under investigation. Although instruments have been developed over the years that can provide this information, they generally have one common limitation, namely spatial resolution. Analytical electron microscopy (AEM) is the term which is now applied to a new group of analytical techniques used in conjunction with a transmission electron microscope and/or a scanning-transmission electron microscope that can provide high spatial resolution (about 20 nm) analyses from microvolumes of material in thin electron-transparent specimens. The basic principles of microanalysis using AEM are discussed, together with examples of application in both metallurgical and ceramic studies.     

Electron microscopic study of the superstructure,the domain structure and the transition state of CuIn5Te8

The structure and microstructure of the compound CuIn₅Te₈ have been examined. The lattice parameters as deduced from electron microscopy diffraction patterns were found to be a = 0,61 nm and c = 1.22 nm in good agreement with those determined by X-rays. Furthermore the crystals of this compound present a domain structure, consisting of three non-coaxial orientation variants. The examination of this domain structure allowed us to conclude that this compound has a thiogallate-like structure.     

Modeling of effective material properties of pyrolytic carbon with different texture degrees by homogenization method

The elastic properties of pyrolytic carbon material as a function of texture degree were calculated by means of a homogenization method. The material microstructure is modeled as a system of graphite crystals (inclusions) embedded in an infinite homogeneous matrix with unknown effective (overall) parameters. The texture degrees of carbon planes extracted from the experimental selected-area electron diffraction patterns as well as size of coherent domains extracted from high resolution transmission electron microscopy images have been used as reference points for modeling of material properties. The experimental diffraction curves exhibiting a good fitting with the Gauss density function have been used to simulate the spatial orientation of inclusions. After that the overall elasticity tensor is calculated and the influence of the texture degree of pyrolytic carbon material on the engineering elastic parameters is studied.     

一种新型铁素体不锈钢的深冲性能研究

为探究一种新型铁素体不锈钢的深冲性能,在840~920℃不同温度下对新型铁素体不锈钢的冷轧板做再结晶退火处理,通过XRD、SEM和EBSD等分析方法研究了退火2 min或4 min后,材料微观组织、宏观织构的变化规律对深冲性能的影响及其内在机理.研究表明:保持退火时间2 min,退火温度900℃时,试验钢拥有较多的有利γ纤维织构,主要为{111}112取向,并有少量α纤维织构,此时平均塑性应变比r-=1.77,高于其他退火温度下的值;延长退火时间,在900℃下保温4 min,不同取向晶粒获得了长大机会,晶粒尺寸均匀性显著改善,r-值提高至1.82,试验钢有望取得理想深冲性能.     

Microstructural evolution in lubricious ZnO films grown by pulsed laser deposition

Zinc oxide (ZnO) is well known to the electronic industry as a piezoelectric material. Recent research from this laboratory also indicates the potential of ZnO as a tribological material. The current work describes the evolution of microstructure with deposition parameters in pulsed laser deposited ZnO thin films, specifically targeted for friction and wear applications. Films were characterized by high resolution scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). Friction and wear measurements were made using a ball-on-disk tribometer. Films were grown in vacuum (V) as well as in 5 mTorr of oxygen (O₂), while the substrates were kept at room temperature (RT). The RT/V ZnO films have (002) columnar texture with an average column width of 20 nm. The RT/O₂ films also are nanoclumnar with (002) texture, but each column is a mosaic of low-angle boundaries. Deformation mechanisms associated with nanocrystalline grain structure were analyzed with particular reference to sliding contact. Mechanisms to provide the observed low friction of RT/O₂ films (μ=0.15–0.20) have been activated by its mosaic structure.     

Epitaxial growth of nanostructured gold films on germanium via galvanic displacement

This work focuses on the synthesis and characterization of gold films grown via galvanic displacement on Ge(111) substrates. The synthetic approach uses galvanic displacement, a type of electroless deposition that takes place in an efficient manner under aqueous, room temperature conditions. Investigations involving X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques were performed to study the crystallinity and orientation of the resulting gold-on-germanium films. A profound effect of HF(aq) concentration was noted, and although the SEM images did not show significant differences in the resulting gold films, a host of X-ray diffraction studies demonstrated that higher concentrations of HF(aq) led to epitaxial gold-on-germanium, whereas in the absence of HF(aq), lower degrees of order (fiber texture) resulted. Cross-sectional nanobeam diffraction analyses of the Au-Ge interface confirmed the epitaxial nature of the gold-on-germanium film. This epitaxial behavior can be attributed to the simultaneous etching of the germanium oxides, formed during the galvanic displacement process, in the presence of HF. High-resolution TEM analyses showed the coincident site lattice (CSL) interface of gold-on-germanium, which results in a small 3.8% lattice mismatch due to the coincidence of four gold lattices with three of germanium.     

Identification of surface carbides and spinels in welded austenitic stainless steels

Welding of stainless steels has been shown to cause localized changes in the microstructure and chemical composition which could have adverse implications for the mechanical and corrosion properties of the material. The application of several electron-optical techniques, such as transmission and scanning electron microscopies (TEM, SEM) and electron and Auger microprobe analysis (AEM), for the identification of different phases has been illustrated by the investigation of segregation effects in welded steels of AISI types 304, 304L, 316 and 316L. Considerable enhancement of chromium and carbon has been observed in certain welldefined zones on the parent metal and on the weld beads. Enhancement of oxygen was also observed at some of the points in these areas. The localized change in surface composition, particularly in the parent metal is attributed to the formation of the carbide M₂₃C₆ and the spinel FeCr₂O₄. The results were confirmed by the determination of the composition of the segregation zone, as well as the lattice parameter of some of the particles, with TEM, SEM and AEM.