Using transmission Kikuchi diffraction to study intergranular stress corrosion cracking in type 316 stainless steels

Transmission Kikuchi diffraction (TKD), also known as transmission-electron backscatter diffraction (t-EBSD) is a novel method for orientation mapping of electron transparent transmission electron microscopy specimen in the scanning electron microscope and has been utilized for stress corrosion cracking characterization of type 316 stainless steels. The main advantage of TKD is a significantly higher spatial resolution compared to the conventional EBSD due to the smaller interaction volume of the incident beam with the specimen.Two 316 stainless steel specimen, tested for stress corrosion cracking in hydrogenated and oxygenated pressurized water reactor chemistry, were characterized via TKD. The results include inverse pole figure (IPFZ) maps, image quality maps and misorientation maps, all acquired in very short time (<60 min) and with remarkable spatial resolution (up to 5 nm step size possible). They have been used in order to determine the location of the open crack with respect to the grain boundary, deformation bands, twinning and slip. Furthermore, TKD has been used to measure the grain boundary misorientation and establish a gauge for quantifying plastic deformation at the crack tip and other regions in the surrounding matrix. Both grain boundary migration and slip transfer have been detected as well.     

Applications of the electron backscatter diffraction technique to ceramic materials

A technique with a relatively high spatial resolution is required for an effective analysis of the microstructure of ceramic materials. The recently developed electron backscatter diffraction (EBSD) technique, which works within a scanning electron microscope, enables a spatially highly resolved study of crystallographic orientations while recording Kikuchi patterns on a user-defined grid. However, such an EBSD texture analysis was until now not often performed on ceramic materials – in contrary, the technique is widely employed in the analysis of metallic materials, including the investigation of various types of steels. The use of ceramics possesses a variety of problems for EBSD investigations like: (i) complicated crystal structure, (ii) difficult surface preparation, and (iii) problems arising from a low conductivity of the ceramic materials. Here, we discuss these problems and present solutions in order to obtain high-quality Kikuchi patterns from such ceramics.     

Case studies on the application of high-resolution electron channelling contrast imaging – investigation of defects and defect arrangements in metallic materials

In 1967, Coates discovered the electron channelling contrast of backscattered electrons (BSEs) in scanning electron microscopy, and by this the possibility to investigate arrangements of lattice defects in deformed microstructures of materials. Since that time, a straightforward development of the scanning electron microscopes as well as of the electron channelling contrast technique took place. Nowadays, the performance of scanning electron microscopes is high enough that the resolution of electron channelling contrast imaging (ECCI) micrographs is comparable with conventional bright field transmission electron microscopy (TEM) micrographs. In the first part of the present paper, a historical review on the development of the ECCI technique starting from its discovery more than 45 years ago up to the combination with other advanced methods of scanning electron microscopy like electron backscatter diffraction or high-resolution selected area channelling patterning in the last few years is given. Major important investigations using this technique for the visualization of individual lattice defects like stacking faults (SFs) and dislocations or dislocation arrangements are chronologically summarized. The second part demonstrates that nowadays, ECCI micrographs taken in high-resolution scanning electron microscopes can be called high-resolution ECCI (HR-ECCI). It is shown that the resolution of individual SFs and dislocations in the HR-ECCI micrographs is comparable to that of conventional TEM (about 15 nm defect image width). Furthermore, the paper is demonstrating that HR-ECCI micrographs can be obtained for various types of materials after different mechanical loadings and different grain sizes ranging from large grain size of 500 μm (cast steel) down to less than 2 μm (γ-TiAl).     

Correlative microscopy of a carbide-free bainitic steel

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite–austenite (M–A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M–A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation.     

Advanced microstructural analysis of ferrite materials by means of electron backscatter diffraction (EBSD)

The analysis of the achieved texture is of great importance for the performance of ferrite materials, either bulk or thin films. The recently developed electron backscatter diffraction (EBSD) technique enables a spatially resolved study of the crystallographic orientations by means of recording of Kikuchi patterns. To our knowledge, such a thorough EBSD analysis was not yet performed in any oxidic magnetic material, and only very recently on magnetite thin films by us. A good surface polishing/cleaning is essential for this analysis, as the method requires an undisturbed surface area for a high image quality (IQ). This information is recorded to each measured Kikuchi pattern, together with a parameter describing the quality of indexation. Here, the spatially highly resolved EBSD mappings provide additional information as compared to the standard analysis techniques, which can contribute to an optimization of the growth process. Furthermore, an analysis of the grain aspect ratio is possible which provides further insight to the microstructural dependence of the magnetic properties of ferrites.     

EBSD analysis of electroplated magnetite thin films

By means of electron backscatter diffraction (EBSD), we analyse the crystallographic orientation of electroplated magnetite thin films on Si/copper substrates. Varying the voltage during the electroplating procedure, the resulting surface properties are differing considerably. While a high voltage produces larger but individual grains on the surface, the surfaces become smoother on decreasing voltage. Good quality Kikuchi patterns could be obtained from all samples; even on individual grains, where the surface and the edges could be measured. The spatial resolution of the EBSD measurement could be increased to about 10 nm; thus enabling a detailed analysis of single magnetite grains. The thin film samples are polycrystalline and do not exhibit a preferred orientation. EBSD reveals that the grain size changes depending on the processing conditions, while the detected misorientation angles stay similar.     

Electron channelling contrast imaging of dislocations in a conventional SEM

Abstract

Dislocations in shock loaded tantalum single crystals were imaged using both transmission electron microscope (TEM) and electron channelling contrast image (ECCI) in a scanning electron microscope with a conventional backscattered electron detector. The results were compared with backscattered electron intensity profiles across dislocations calculated via the dynamic theory of electron diffraction. A one-to-one correspondence between ECCI and TEM is established. High voltage and low index reflections should be used to obtain the highest dislocation contrast and greatest imaging depth.     

位错的会聚束电子衍射研究

从硅位错附近得到的会聚束电子衍射图样表明高阶劳厄带线和菊池线分裂,晶体学等效的衍射显示不同的分裂或不分裂,这些结果可以用晶体缺陷的衍衬理论来解释,不分裂的衍射相当于位错的不可见,即g·b=0,会聚束电子衍射提供了强有力的研究缺陷的高空间分辨率手段。 关键词：     

Mesoscale strain measurement in deformed crystals: A comparison of X-ray microdiffraction with electron backscatter diffraction

Mapping of residual stresses at the mesoscale is increasingly practical thanks to technological developments in electron backscatter diffraction (EBSD) and X-ray microdiffraction using high brilliance synchrotron sources. An analysis is presented of a Cu single crystal deformed in compression to about 10% macroscopic strain. Local orientation measurements were made on sectioned and polished specimens using EBSD and X-ray microdiffraction. In broad strokes, the results are similar to each other with orientations being observed that are on the order of 5° misoriented from that of the original crystallite. At the fine scale it is apparent that the X-ray technique can distinguish features in the structure that are much finer in detail than those observed using EBSD even though the spatial resolution of EBSD is superior to that of X-ray diffraction by approximately two orders of magnitude. The results are explained by the sensitivity of the EBSD technique to the specimen surface condition. Dislocation dynamics simulations show that there is a relaxation of the dislocation structure near the free surface of the specimen that extends approximately 650 Å into the specimen. The high spatial resolution of the EBSD technique is detrimental in this respect as the information volume extends only 200 Å or so into the specimen. The X-rays probe a volume on the order of 2 µm in diameter, thus measuring the structure that is relatively unaffected by the near-surface relaxation.     

Strain Field in GaAs/GaN Wafer-Bonding Interface and Its Microstructure

The strain fields in a wafer-bonded GaAs/GaN structure are measured by electron backscatter diffraction （EBSD）. Image quality （IQ） of EBSD Kikuchi patterns and rotation angles of crystal lattices as strain sensitive parameters axe employed to chaxacterize the distortion and the rotation of crystal lattices in the GaAs-interface-GaN structure, as well as to display the strain fields. The results indicate that the influence region of the strains in the wafer-bonded GaAs/GaN structure is mainly located in GaAs side because the strength of GaAs is weaker than that of GaN. The cross-sectional image of transmission electron microscopy （TEM） further reveals the distortion and the rotation of crystal lattices induced by strains systematically.     

Analysis of the spatial orientation distribution of building blocks in polycrystals as determined using transmission electron microscopy and a backscattered electron beam in a scanning electron microscope

The advantages and disadvantages of the method of automatic analysis of electron backscattering diffraction (EBSD) patterns for studying spatial orientation distributions are considered as compared to transmission electron microscopy (TEM). A misorientation spectrum in a test alloy (Kh20N80 alloy) having a high content of annealing twins is experimentally studied using both TEM and EBSD, and the results obtained are compared.     

Structure and orientation of an intermetallic phase in a W-Ni-Co alloy

The aim of this investigation is crystal structure determination of an intermetallic phase formed in a W-Ni-Co alloy during a heat-treatment carried out at a temperature of 800°C. This intermetallic phase is expected to play a critical role on the final microstructure (fine tungsten particles in an FCC matrix that is present in between large tungsten grains) and thereby, on the properties of the alloy. 92W-5.3Ni-2.7Co alloy was prepared through powder metallurgy route (liquid phase sintering) followed by heat-treatment at 800°C for 5?h. The intermetallic phase formed at this temperature was characterised using transmission and scanning electron microscopes. The intermetallic phase was found to have orthorhombic crystal structure with Pnam (62) space group as determined using automated diffraction tomography along with precession electron diffraction. Chemical analysis in TEM suggested that the intermetallic phase is based on stoichiometry (Co,Ni)₂W. Orientation imaging of the phase was also carried out in TEM and EBSD to understand its evolution. Equiaxed or lath morphology of the intermetallic phase was found to depend on the crystallographic orientation relationship of the phase with the tungsten grains and the matrix phase.     

High resolution electron backscatter diffraction (EBSD) data from calcite biominerals in recent gastropod shells

Electron backscatter diffraction (EBSD) is a microscopy technique that reveals in situ crystallographic information. Currently, it is widely used for the characterization of geological materials and in studies of biomineralization. Here, we analyze high resolution EBSD data from biogenic calcite in two mollusk taxa, Concholepas and Haliotis, previously used in the understanding of complex biomineralization and paleoenvironmental studies. Results indicate that Concholepas has less ordered prisms than in Haliotis, and that in Concholepas the level of order is not homogenous in different areas of the shell. Overall, the usefulness of data integration obtained from diffraction intensity and crystallographic orientation maps, and corresponding pole figures, is discussed as well as its application to similar studies.     

Ultramicrotomy reveals crystallographic information on a sectioned surface of a metallic block specimen

Ultramicrotomy is widely regarded as a thin section preparation method for transmission electron microscopy (TEM) investigations. It is shown that ultramicrotomy can also provide a simple path for microstructure analysis and assessment of mechanical properties for a sectioned block-face. Furthermore, electron backscatter diffraction (EBSD) analysis can be applied directly on ultramicrotomed surfaces without any additional polishing or etching. EBSD analysis relates the inherent cutting artefacts to the crystallographic orientations of the grains, hence delivering a rough assessment of their deformation resistance. TEM investigations revealed that crystallographic-related cutting artefacts, which exhibit a wave-like pattern, are the result of the dislocation pile-ups close to the knife–specimen interface. This technique is considered suitable to be coupled with EBSD for three-dimensional microstructure reconstructions when used for serial sectioning of large volumes.     

Application of automated crystallography for transmission electron microscopy in the study of grain-boundary segregation

Analytical Electron Microscopy (AEM) has brought significant progress in the study of grain-boundary segregation. Using X-ray energy-dispersive spectrometry (XEDS) in the AEM, elemental segregation information can be related to the crystallographic character of the same boundary via conventional Transmission Electron Microscope (TEM) diffraction techniques. While significant efforts have been made to improve XEDS analysis of sub-nanometer segregation layers, the methods for crystallographic characterization of grain boundaries have remained the same for several decades and labor-intensive processes. Recently, a method termed Automated Crystallography for TEM (ACT) was developed, which automates crystallographic characterization of grains under TEM observation. In the present work, we combine ACT and X-ray mapping via EDS in AEM for the study of Sb grain-boundary segregation in a rapidly solidified Cu-0.08 wt % Sb alloy. In contrast with previous reports, a large degree of anisotropy in Sb segregation level between different boundaries is found. ACT results suggest that one of the several grain boundaries observed with no detectable Sb segregation is very close to a Sigma 3 coincidence-site lattice structure. The reason for the observed anisotropy in the present alloy is discussed, based upon McLean's theory of segregation.     

Determination of elastic strain fields and geometrically necessary dislocation distributions near nanoindents using electron back scatter diffraction

The deformation around a 500-nm deep Berkovich indent in a large grained Fe sample has been studied using high resolution electron back scatter diffraction (EBSD). EBSD patterns were obtained in a two-dimensional map around the indent on the free surface. A cross-correlation-based analysis of small shifts in many sub-regions of the EBSD patterns was used to determine the variation of elastic strain and lattice rotations across the map at a sensitivity of ～±10^?4. Elastic strains were smaller than lattice rotations, with radial strains found to be compressive and hoop strains tensile as expected. Several analyses based on Nye's dislocation tensor were used to estimate the distribution of geometrically necessary dislocations (GNDs) around the indent. The results obtained using different assumed dislocation geometries, optimisation routines and different contributions from the measured lattice rotation and strain fields are compared. Our favoured approach is to seek a combination of GND types which support the six measurable (of a possible nine) gradients of the lattice rotations after correction for the 10 measurable elastic strain gradients, and minimise the total GND line energy using an L¹ optimisation method. A lower bound estimate for the noise on the GND density determination is ～±10¹² m^?2 for a 200-nm step size, and near the indent densities as high as 10¹⁵ m^?2 were measured. For comparison, a Hough-based analysis of the EBSD patterns has a much higher noise level of ～±10¹⁴m^?2 for the GND density.     

Formation and crystallographic orientation study of quasicrystal, 2/1 and 1/1 approximants in Cd–Mg–Y system using electron backscatter diffraction (EBSD)

A partial isothermal ternary phase diagram of the Cd–Mg–Y system including icosahedral quasicrystal (i-QC) and 1/1 approximant (APP) was obtained at 673?K. The stability of the i-QC and APPs in terms of composition and temperature was studied, as a result of which the 2/1 APP phase was discovered at 773?K. Moreover, the i-QC phase was found to be stable at lower Y concentrations of ～12–13?at.%, as compared to the 1/1 APP, which showed ～15–16?at.% Y. Single i-QC, 2/1 and 1/1 APP grains were also synthesized applying centrifuging system. Electron backscatter diffraction (EBSD) characterization of the obtained i-QC and APPs revealed almost the same Kikuchi patterns for the i-QC and 2/1 APP, indicating high resemblance of their structures. However, the Kikuchi pattern acquired from the 1/1 APP was distinguishable from the one obtained from the i-QC as it showed split bands. The occurrence of the split bands was associated with significant deviation from a perfect icosahedral symmetry. This was also confirmed by analysing calculated electron diffraction and Kikuchi patterns along pseudo-five-fold axes of the 2/1 and 1/1 APPs. Finally, orientation relationships between the i-QC, 1/1 APP and α-Mg were investigated by analysing acquired EBSD Kikuchi patterns from the respective domains. Accordingly, three perpendicular two-fold axes of the i-QC and {100} axes of the 1/1 APP occur along three mutually orthogonal {0001}, {10-10} and {11-20} axes of the α-Mg.     

苝四甲酸二酐有机单晶纳米结构的制备及形成机理的研究

在分子束外延(MBE)系统中, 利用物理气相沉积(PVD)的方法在阳极氧化铝(AAO)模板上制备了有机 染料分子苝四甲酸二酐(PTCDA)的不同纳米结构; 并使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、 高分辨透射电子显微镜(HRTEM)以及选区电子衍射(SAED)技术进行了系统的研究. 结果发现, 当衬底温度(T_s)为330 ℃时得到的是纳米丝、针、带以及棒; T_s为280 ℃, 230 ℃, 180 ℃时得到的主要是纳米棒, 并且纳米棒的长度随T_s的降低而变短; T_s为50 ℃时只能得到连续的PTCDA薄膜. HRTEM以及SAED结果证实了纳米针与棒为单晶. 依据SEM结果, 提出纳米结构的生成主要受T_s以及衬底表面曲率的影响.     

Challenges and strategies of surface modification of electrogalvanized coatings for electron microscopy analysis

Despite wide usage of electrogalvanized coatings in various applications, characterization studies on their micro/crystal structure, and the understanding of how they correspondingly affect the properties, such as corrosion, are rather limited. This is mainly attributed to some difficulties in preparing and examining the zinc coating layers, owing to their intrinsically low corrosion resistance and refined nano-scaled crystallite size. This study aims to examine such challenges systematically and propose some mitigation strategies. Particularly, sample preparation processes, including surface finishing for metallography and sample thinning processes are explored. Furthermore, a range of electron microscopy techniques, including scanning electron microscopy (SEM), electron back scattered diffractometry (EBSD), and transmission electron microscopy (TEM) are investigated in relation to the achievable clarity of microstructural details of electrogalvanized coatings.