Theoretical estimation for correlations of diffraction patterns from objects differently oriented in space

Coherent diffraction imaging of single biomolecules is expected to open unique opportunities for studies of non-crystalline samples. There are, however, still many technical and physical issues that need to be resolved in a more quantitative manner, especially if one aims for structural information at high resolution. Signal recorded from an object after a single shot is low. As primarily proposed in Spence and Doak (2004) and Huldt et al. (2003) [1] and [2], averaging over the diffraction patterns from many different shots is necessary, in order to achieve a signal-to-noise ratio sufficient for image reconstruction. The images of the randomly oriented molecules have to be sorted out in order to identify those corresponding to the similar spatial orientations of the objects. This procedure is called the classification of diffraction images. Here we approach the classification in the framework of pattern-to-pattern correlations, and analyse theoretically the correlations between diffraction images of differently oriented objects.     

In situ electron backscattered diffraction of individual GaAs nanowires

We suggest and demonstrate that electron backscattered diffraction, a scanning electron microscope-based technique, can be used for non-destructive structural and morphological characterization of statistically significant number of nanowires in situ on their growth substrate. We obtain morphological, crystal phase, and crystal orientation information of individual GaAs nanowires in situ on the growth substrate GaAs(111) B. Our results, verified using transmission electron microscopy and selected area electron diffraction analyses of the same set of wires, indicate that most wires possess a wurtzite structure with a high density of thin structural defects aligned normal to the wire growth axis, while others grow defect-free with a zincblende structure. The demonstrated approach is general, applicable to other material systems, and is expected to provide important insights into the role of substrate structure on nanowire structure on nanowire crystallinity and growth orientation.     

The scanning low-energy electron microscope: First attainment of diffraction contrast in the scanning electron microscope

Using small Pb crystals deposited in situ on a partially contaminated Si (100) crystal, we demonstrate that a commercial scanning electron microscope (SEM) can easily be converted into a scanning low-energy electron microscope (SLEEM). Although the contrast mechanism is much more complicated than that in nonscanning LEEM because not only one diffracted monochromatic beam and its close environment are used for imaging, but several diffracted beams and a wide energy spectrum of electrons of different origin (secondary electrons, inelastically andelastically scattered electrons) are used, SLEEM is a valuable addition to the standard SEM because it provides an additional structure- and orientation-sensitive contrast mechanism in crystalline materials, a low sampling depth, and high intensity at low energies.     

Progressive steps in the development of electron backscatter diffraction and orientation imaging microscopy

Ten years ago electron backscatter diffraction (EBSD) became available to a wider group active in materials research. This paper highlights some of the more significant developments in camera technology and software developments that have arisen since then. The use of slow‐scan charge couple device cameras for phase identification and rapid determination of orientation image micrographs is reviewed. The current limiting spatial resolution of the technique is shown to be less than 10 nm. A procedure for improving lattice spacing measurement by utilizing the full resolution of the camera is described with experimental measurements on silicon and nickel showing relative errors of plus/minus 3%. An investigation of partially recrystallized aluminium shows how the recrystallized fraction can be extracted with confidence but that the mapping of substructure in the highly deformed regions is questionable. Phase identification is described for complex cases in which the phase data tabulated in standard databases do not correspond to what is observed in the EBSD patterns. Phase mapping in a complex mineral in which chemical data and EBSD data are collected simultaneously is shown to be improved by recording both the chemical and the EBSD data into computer memory and proceeding with the phase discrimination and orientation measurement in off‐line analysis.     

10-kV diffractive imaging using newly developed electron diffraction microscope

A new electron diffraction microscope based on a conventional scanning electron microscope (SEM), for obtaining atomic-level resolution images without causing serious damage to the specimen, has been developed. This microscope in the relatively low-voltage region makes it possible to observe specimens at suitable resolution and record diffraction patterns. Using the microscope we accomplished 10-kV diffractive imaging with the iterative phase retrieval and reconstructed the structure of a multi-wall carbon nanotube with its finest feature corresponding to 0.34-nm carbon wall spacing. These results demonstrate the possibility of seamless connection between observing specimens by SEM and obtaining their images at high resolution by diffractive imaging.     

Cryo‐scanning x‐ray diffraction microscopy of frozen‐hydrated yeast

We developed cryo‐scanning x‐ray diffraction microscopy, utilizing hard x‐ray ptychography at cryogenic temperature, for the noninvasive, high‐resolution imaging of wet, extended biological samples and report its first frozen‐hydrated imaging. Utilizing phase contrast at hard x‐rays, cryo‐scanning x‐ray diffraction microscopy provides the penetration power suitable for thick samples while retaining sensitivity to minute density changes within unstained samples. It is dose‐efficient and further minimizes radiation damage by keeping the wet samples at cryogenic temperature. We demonstrate these capabilities in two dimensions by imaging unstained frozen‐hydrated budding yeast cells, achieving a spatial resolution of 85 nm with a phase sensitivity of 0.0053 radians. The current work presents the feasibility of cryo‐scanning x‐ray diffraction microscopy for quantitative, high‐resolution imaging of unmodified biological samples extending to tens of micrometres.     

About the role of boundary conditions on compositional imaging with a scanning electron microscope

We consider the effects of different boundaries on the visibility of a specimen detail providing a compositional contrast in scanning electron microscopy, operating with backscattered electrons or secondary electrons. An object characterized by a gradual variation in composition, an As-doped region in Si, is investigated. The different boundaries in the cross-sectioned specimen correspond to the absence or presence of a poly-Si layer on top of the implanted region, deposited after the annealing treatment. It is shown that the interpretation model used for image formation is of paramount relevance for understanding the experimental results, indicating that the boundaries of the doped region are important in hindering or enhancing its visibility. The relevance of experimental parameters such as electron energy and probe dimension is also reported.     

谐衍射中、长波红外超光谱成像系统设计

为了充分利用中波红外和长波红外的光谱信息,建立了谐衍射中、长波红外超光谱成像系统。利用谐衍射元件独特的色散特性,将谐衍射透镜应用于中、长波红外超光谱成像系统中,使系统在中波红外3.7~4.8μm和长波红外8.5~12μm的2个谐振波段内获取二百多个不同波长的图像信息。设计结果显示,在中波红外波段18lp/mm处,光学调制传递函数0.52;长波红外波段13lp/mm处,光学调制传递函数0.51;光学系统的点斑均方根直径在中波红外波段小于27μm,在长波红外波段小于34μm。得到的结果表明,光学调制传递函数在各个波长处均接近衍射极限,点斑的均方根直径完全可以与国内现有探测器的像元尺寸匹配。     

Towards sub-A atomic resolution electron diffraction imaging of metallic nanoclusters: a simulation study of experimental parameters and reconstruction algorithms

A simulation study is carried out to elucidate the effects of dynamical scattering, electron beam convergence angle and detection noise on atomic resolution diffraction imaging of small particles and to develop effective reconstruction procedures. Au nanoclusters are used as model because of their strong scattering. The results show that the dynamical effects of electron diffraction place a limit on the size of Au nanoclusters that can be reconstructed from the diffraction intensities with sufficient accuracy. For smaller Au nanoclusters, the simulations show that diffraction patterns recorded under the experimental conditions can be reconstructed using a combination of phase retrieval algorithms. The use of a low-resolution image is shown to be effective for reconstructing diffraction patterns without the central beam. A new algorithm for estimating the object support is proposed.     

Microstructural and microtextural characterization of oxide scale on steel using electron backscatter diffraction

High‐temperature oxidation of steel has been extensively studied. The microstructure of iron oxides is, however, not well understood because of the difficulty in imaging it using conventional methods, such as optical or electron microscopy. A knowledge of the oxide microstructure and texture is critical in understanding how the oxide film behaves during high‐temperature deformation of steels and more importantly how it can be removed following processing. Recently, electron back‐scatter diffraction (EBSD) has proved to be a powerful technique for distinguishing the different phases in scales. This technique gives valuable information both on the microstructure and on the orientation relationships between the steel and the scale layers. In the current study EBSD has been used to investigate the microstructure and microtexture of iron oxide layers grown on interstitial free steel at different times and temperatures. Heat treatments have been carried out under normal oxidation conditions in order to relate the results to real steel manufacturing in industry. The composition, morphologies, microstructure and microtexture of selected conditions have been studied using EBSD.     

Visualization and electron diffraction on cryosections of stratum corneum: a utopia?

The skin acts as an effective barrier to protect the body against penetration of substances from the environment and against desiccation. The main barrier function resides in the stratum corneum, and more specifically in the intercellular lipid domains. Several techniques have been used to elucidate the local lipid crystal arrangements in these domains, but they either needed an extensive pretreatment of the skin with the risk of damaging the native structure, or were not suited to obtain local structure information as bulk quantities of stratum corneum were required. In this paper a method of performing local structure analysis (electron diffraction) on cryo-fixed specimens is described. Therefore a cold chain procedure was used to obtain cryosections of stratum corneum. On these sections visualization and electron diffraction at low temperature were carried out.
Using a so-called tape sandwich method, cryosections were prepared in which corneocytes and lipid matrix could easily be distinguished. Moreover, detailed cellular components such as desmosomes and intracellular lipid domains were observed. However, probably due to the limited amount of intercellular lipids in the stratum corneum, electron diffraction on cryosections did not result in diffraction patterns that were undoubtedly originating from the intercellular lipids. In the electron diffraction patterns of a skin lipid model system reflections were present that were indicative of hexagonal and orthorhombic sublattices. The d-spacings of these reflections were similar to the spacings of the high-intensity reflections of the X-ray diffraction pattern of the same mixture. This showed agreement between a bulk and a local technique, X-ray and electron diffraction.     

Low angle boundary migration of shot‐peened pure nickel investigated by electron channeling contrast imaging and electron backscatter diffraction

Study on recrystallization of deformed metal is important for practical industrial applications. Most of studies about recrystallization behavior focused on the migration of the high‐angle grain boundaries, resulting in lack of information of the kinetics of the low angle grain boundary migration. In this study, we focused on the migration of the low angle grain boundaries during recrystallization process. Pure nickel deformed by shot peening which induced plastic deformation at the surface was investigated. The surface of the specimen was prepared by mechanical polishing using diamond slurry and colloidal silica down to 0.02 μm. Sequential heat treatment under a moderate annealing temperature facilitates to observe the migration of low angle grain boundaries. The threshold energy for low angle boundary migration during recrystallization as a function of misorientation angle was evaluated using scanning electron microscopy techniques. A combination of electron channeling contrast imaging and electron backscatter diffraction was used to measure the average dislocation density and a quantitative estimation of the stored energy near the boundary. It was observed that the migration of the low angle grain boundaries during recrystallization was strongly affected by both the stored energy of the deformed matrix and the misorientation angle of the boundary. Through the combination of electron channeling contrast imaging and electron backscatter diffraction, the threshold stored energy for the migration of the low angle grain boundaries was estimated as a function of the boundary misorientation.     

A study on the indexing method of the electron backscatter diffraction pattern assisted by the Kikuchi bandwidth

Bitumen is a widely used material employed as a binder in pavement engineering and as a surface sealant in construction. Its surface microstructure and microscale properties have been shown to be temperature-dependent, with effects manifesting themselves on surface composition and texture, including the formation of the visually striking catana ‘bee’-like structures. Despite the importance of a good performance of bitumen in subzero environments (<0°C), the behaviour of bitumen surface texture and composition at cold temperatures, affecting cracking, degradation and road icing, has received practically no attention. In particular, such knowledge is relevant to world regions experiencing long periods of subzero temperatures during the year. Employing advanced atomic force microscopy combined with infrared spectroscopy (AFM-IR) and an environmental chamber, we demonstrate the ability to characterise surface structure and composition with nanoscale precision for a broad range of temperatures. We show that cooling bitumen to subzero temperatures can have several interesting effects on its surface microtexture, nanotexture and composition, especially on its three surface domains, catana, peri and para. We found that the para domain coarsens and extends to form an interfacial transition domain (characterised by increasing surface roughness with peri domain composition) between the para and peri domains. We show that the catana and peri domains have a similar composition, but have different mechanical and chemical properties compared to the para domain. The essential findings of this work improve our understanding of the behaviour of bitumen in subzero environments, aiding us in our quest towards attaining better road and sealant performance.     

Analytical transmission electron microscopy and electron diffraction for characterization of multiphase Ni-P-Ti surface layer on Ti-6Al-4V alloy

The microstructure, chemical and phase composition of the hard Ni‐P‐Ti layer formed on the Ti‐6Al‐4V alloy after duplex surface treatment were investigated by light microscopy, X‐ray diffraction, scanning electron microscopy and analytical/high‐resolution transmission electron microscopy. These investigations showed that the improved mechanical and tribological properties of the surface‐treated alloy were related to the presence of a multilayered microstructure containing several phases from the Ni‐Ti‐P‐Al system.     

Nanobeam electron diffraction and high resolution imaging analysis of InN films grown on sapphire

A JEOL JEM-3000F field emission, analytical, high-resolution transmission electron microscope (HRTEM) was used to study InN films grown on sapphire substrates. It was found that, while the InN films maintained the hexagonal (wurtzite) structure, InN nanodomains with a cubic (zincblende) structure were also formed in the films. Nanobeam electron diffraction techniques were applied for identification of the cubic phase. The identification of the cubic InN was confirmed by HRTEM structural imaging. The cubic InN nanodomains are 3-10 nm in diameter, and are orientated in two different orientations with their [110](cubic) and [110](cubic) axes parallel to each other and their (111)(cubic) planes parallel to the (0001)(hex) plane of the hexagonal InN.     

Construction of an organic crystal structural model based on combined electron and powder X-ray diffraction data and the charge flipping algorithm

The structure of an organic dye 1,5-diaminoanthraquinone (DAAQ) nanowire was studied by both electron diffraction and X-ray powder diffraction. The unit cell of the crystal was determined from a series of tilted selected area electron diffraction patterns (monoclinic: a=3.78 Å, b=9.73 Å, c=15.01 Å and β=82.4°). By using precession electron diffraction, the following extinction conditions were determined, 0k0: k=2n and 00l: l=2n, which give the space group as P2₁/C (no. 14). The powder charge flipping algorithm was applied to resolve the phase problem and the structural model of the DAAQ crystal was built.     

Research on precision‐calibration techniques for selected area electron diffraction patterns of pyrocarbon

The key techniques for determining orientation angle (OA) and interlayer space (d002) of pyrocarbon were investigated by analyzing selected area electron diffraction (SAED) patterns. A series of algorithms, which mainly include the five‐point center‐determined technique, the integral factor for the ellipse detection, the background subtraction operation and the Gaussian multipeak fitting algorithm, were designed for intensity sampling, data correction, and data fitting. The contribution ratio of the reflection intensity to the average d002 was considered. The algorithms were programmed and applied to evaluate SAED patterns of pyrocarbon in C/C composites by chemical vapor infiltration. Results showed that the proposed techniques can be effectively used to measure various SAED patterns, with a beam stop image or not, of pyrocarbon. The azimuthal intensities along the (002) arcs essentially obey the Gaussian distribution, although this is not obvious for the lower textural pyrocarbon. It is necessary for accurate OA to use the Gaussian multipeak fitting algorithm. Microsc. Res. Tech., 2009. © 2008 Wiley‐Liss, Inc.     

Distinguishing crystallographic misorientations of lanthanum zirconate epilayers on nickel substrates by electron backscatter diffraction

Electron backscatter diffraction (EBSD) was used for distinguishing crystallographic orientations and local lattice misfits of a La₂Zr₂O₇ (LZO) buffer layer epitaxially grown on a cube textured Ni-5.%W (Ni-W) substrate for a YBCO superconductor film. Orientation data were obtained from the LZO epilayer using low energy primary electrons (5 keV) and from the Ni-W substrate by increasing the voltage to 15 keV. In-plane and out-of-plane orientations of the LZO epilayer were revealed with respect to its Ni-W substrate. A strong {1 0 0} 〈0 1 1〉 rotated-cube texture in the LZO epilayer was formed on the {1 0 0} 〈0 0 1〉 cube-textured Ni-W substrates. LZO and Ni in-plane crystallographic axes are related by an expected 45° rotation. The step-misorientations and the local misfit strains between the LZO epilayer and the substrate were also analyzed.