Automatic twin statistics from electron backscattered diffraction data

A new computer code has been developed to automatically extract quantitative twin statistics from electron backscatter diffraction data. The new code is an improvement upon previous codes in that it handles materials of any crystal symmetry, type I, Type II and compound twins, and general stress states. Moreover, accuracy of the results has been greatly improved. In addition, twin statistics including number, area fraction, twin thickness and twinning dependencies on orientation, grain size and neighbourhood effects can be routinely analysed. The new code has been applied to scan data from deformed magnesium, zirconium and uranium, and can potentially be used for any twinning material for which reliable electron backscatter diffraction results can be obtained.     

Convergent-beam electron diffraction from GaAs/AlAs superlattices

Convergent-beam electron diffraction patterns were obtained from GaAs/AlAs multilayers, with the electron beam perpendicular to the layers. We report the first observation of extra higher-order Laue zone reflections originating from the superlattice. The fine structure of these reflections is compared with the first-order Laue zone reflections originating from the average lattice.     

Lattice constant measurement from electron backscatter diffraction patterns

Kikuchi bands in election backscattered diffraction patterns (EBSP) contain information about lattice constants of crystallographic samples that can be extracted via the Bragg equation. An advantage of lattice constant measurement from EBSPs over diffraction (XRD) is the ability to perform local analysis. In this study, lattice constants of cubic STN and cubic YSZ in the pure materials and in co‐sintered composites were measured from their EBSPs acquired at 10 kV using a silicon single crystal as a calibration reference. The EBSP distortion was corrected by spherical back projection and Kikuchi band analysis was made using in‐house software. The error of the lattice constant measurement was determined to be in the range of 0.09–1.12% compared to values determined by XRD and from literature. The confidence level of the method is indicated by the standard deviation of the measurement, which is approximately 0.04 Å. Studying Kikuchi band size dependence of the measurement precision shows that the measurement error decays with increasing band size (i.e. decreasing lattice constant). However, in practice, the sharpness of wide bands tends to be low due to their low intensity, thus limiting the measurement precision. Possible methods to improve measurement precision are suggested.     

Convergent-beam electron diffraction study of transverse stacking faults and dislocations

Transverse stacking faults and dislocations have been studied by convergent-beam electron diffraction (CBED). Stacking faults and dislocations induce splitting in some reflections in the CBED patterns. The splitting and unsplitting of the reflections correspond to the visibility and invisibility of the defect in the kinematic theory of diffraction contrast of imperfect crystals of Hirsch, Howie and Whelan. This method provides a powerful means for the study of crystal defects.     

A preliminary electron backscattered diffraction study of sintered NdFeB-type magnets

This paper reports, for the first time, the use of electron backscattered diffraction (EBSD) to study orientation in sintered NdFeB type magnets. The magnetic properties of NdFeB magnets are greatly improved if a strong crystallographic texture is firstly achieved, namely, the direction of the c‐axis is along the direction of magnetization. A systematic survey of sample preparation techniques showed that samples that were mechanically polished and then etched gave the most reliable EBSD data. Analyses were made using both fully automated EBSD scans and by EBSD measurements taken after manual movement of the beam. The EBSD results are presented as secondary electron SEM micrographs, orientation images and 001 pole figures. For the selection of grains investigated, the deviation of the c‐axis was shown to be between 10° and 30° from the ideal [001]//magnetization direction. It is demonstrated that EBSD is a valuable tool for characterizing the microstructure and texture relationships and for assessing the performance of the processing routes of NdFeB magnets.     

Structural study of new hydrocarbon nano-crystals by energy-filtered electron diffraction

A new brittle hydrocarbon has been successfully synthesized in polycrystalline form, and its crystal structure solved by quantitative electron diffraction. By 3D tilting of the nano-crystals, the lattice type and unit cell parameters were determined. (Triclinic, [Formula: see text] A, [Formula: see text] A, [Formula: see text] A, [Formula: see text] degrees, [Formula: see text] degrees, and [Formula: see text] degrees.) Spot diffraction patterns were obtained at -165 degrees C using the Koehler selected-area mode on a LEO 912 TEM fitted with an omega in-column elastic energy filter. The direct methods algorithm was then applied to merged intensities and a trial structure obtained assuming single scattering. This was further refined to obtain good agreement with a small residual of about 10% using multiple scattering calculations. A diagram of the proposed structure is given.     

An improved photographic process for convergent beam electron diffraction applications

The use of a surface developer, pyrocatechol, to process transmission electron microscope negatives has been shown to have significant advantages over the conventional D-19 process. The process described here is tolerant of a large margin of error in the electron exposure and produces a negative that not only retains details both in the highlight as well as the faint regions, but also preserves local contrast. These characteristics are particularly useful in convergent beam electron diffraction applications where one encounters a wide contrast range. Improved acuteness and an enhanced signal to noise ratio due to the prolonged exposures associated with this process have also been observed.     

菲涅耳-夫琅和费衍射区的过渡判据

区分菲涅耳和夫琅和费衍射是光学中一个基本且又十分有意义的问题。然而从菲涅耳衍射到夫琅和费衍射的过渡条件判别,多数文献是通过实验、或者数值计算和模拟仿真给出结论的。基于标量衍射理论,通过数学分析,得到了从菲涅尔衍射过渡到夫琅和费衍射的判别条件(即菲涅耳数的值F=0.203),其结果和一般文献(F=0.223)相一致。     

Reconstruction of grains and subgrains from electron backscatter diffraction maps

Electron backscatter diffraction maps are capable of yielding a substantial amount of quantitative information about grains, subgrains and boundaries, and the amount and quality of the data may be substantially increased if the pixels of the map are re‐analysed so as to ‘reconstruct’ complete grains or subgrains. The paper discusses the various methods of grain reconstruction and the use of such methods to obtain microstructural information correlating the parameters of dimension, position, orientation and misorientation, which cannot usually be obtained by other means. Grain reconstruction also reveals the nature, location and contacts of all the triple junctions in the microstructure, and the paper discusses two important examples of how these data may be further analysed using automated routines. Boundary connectivity and the length and direction of likely paths along which grain boundary events such as creep fracture or stress corrosion may occur can readily be determined. The overall alignment of boundaries in deformed metals, with respect to the crystallography and the deformation geometry, may be determined as a function of the length and misorientation of the boundary segments.     

Interpretation of electron diffraction patterns from amorphous and fullerene-like carbon allotropes

The short range order in amorphous and fullerene-like carbon compounds has been characterized by selected area electron diffraction (SAED) patterns and compared with simulations of model nanoclusters. Broad rings in SAED pattern from fullerene-like CN_x at ∼1.2, ∼2, and ∼3.5 Å indicate short-range order similar to that in graphite, but peak shifts indicate sheet curvature in agreement with high-resolution transmission electron microscopy images. Fullerene-like CP_x exhibits rings at ∼1.6 and 2.6 Å, which can be explained if it consists of fragments with short-range order and high curvature similar to that of C₂₀.     

Automated extraction of regular spot arrays from electron diffraction images*

In order to analyse agglomerate particles, we have developed a computer method that automates the analysis of spots in electron diffraction patterns. The method isolates the zone axis diffraction pattern in a polycrystalline diffraction image by isolating the spots from other features of the image and then by selecting the spots that belong to a regular array. The method gives the basis vectors for the array which can then be used to identify the particle by comparison with standard diffraction data.     

Techniques of convergent beam electron diffraction

The techniques required to record standard convergent beam electron diffraction patterns in an analytical electron microscope are discussed in detail, with emphasis on the design of electron optics in commercial instruments. Practical comments are included on specimen preparation, the influence of crystal defects, tilting to major zone axes, and alignment of the instrument. The influence of parameters under experimental control such as probe size, accelerating voltage, temperature, specimen tickness, and convergence angle is discussed in detail. Some comments are included on the alignment and limitations of large angle patterns formed by a defocused probe.     

First combined electron backscatter diffraction and transmission electron microscopy study of grain boundary structure of deformed quartzite

The structures of boundaries in a deformed and dynamically recovered and recrystallized quartz polycrystal (mylonite) were characterized by transmission electron microscopy, after the misorientation angles across the same grain boundaries had been analysed using electron backscatter diffraction in a scanning electron microscope. In this new approach, a specific sample area is mapped with electron backscatter diffraction, and the mapped area is then attached to a foil, and by the ion beam thinned for transmission electron microscopy analysis. Dislocations in grain boundaries were recognized as periodic and parallel fringes. The fringes associated with dislocations are observed in boundaries with misorientations less than 9°, whereas such fringes cannot be seen in the boundaries with misorientations larger than 17°. Some boundaries with misorientations between 9° and 17° generally have no structures associated with dislocation. One segment of a boundary with a misorientation of 13.5° has structures associated with dislocations. It is likely that the transition from low‐angle to high‐angle boundaries occurs at misorientations ranging from approximately 9° to 14°. Change in the grain boundary structure presumably influences the mobility of the boundaries. In the studied deformed quartz vein, a relative dearth of boundaries between misorientation angles of θ = 2° and θ = 15° has previously been reported, and high‐angle boundaries form cusps where they intersect low‐angle boundaries, suggesting substantial mobility of high‐angle boundaries.     

Backscattered electron imaging and electron backscattered diffraction in the study of bacterial attachment to titanium alloy structure

The application of secondary electron (SE) imaging, backscattered electron imaging (BSE) and electron backscattered diffraction (EBSD) was investigated in this work to study the bacterial adhesion and proliferation on a commercially pure titanium (cp Ti) and a Ti6Al4V alloy (Ti 64) with respect to substrate microstructure and chemical composition. Adherence of Gram‐positive Staphylococcus epidermidis 11047 and Streptococcus sanguinis GW2, and Gram‐negative Serratia sp. NCIMB 40259 and Escherichia coli 10418 was compared on cp Ti, Ti 64, pure aluminium (Al) and vanadium (V). The substrate microstructure and the bacterial distribution on these metals were characterised using SE, BSE and EBSD imaging. It was observed that titanium alloy‐phase structure, grain boundaries and grain orientation did not influence bacterial adherence or proliferation at microscale. Adherence of all four strains was similar on cp Ti and Ti 64 surfaces whilst inhibited on pure Al. This work establishes a nondestructive and straight‐forward statistical method to analyse the relationship between microbial distribution and metal alloy structure.     

Fading and broadening of electron diffraction spot from beam-damaged multiple monolayer films

In contrast to the increase in the extinction dose for thick specimens, observed broadening rates of diffraction spots from behenic acid multiple monolayers were independent of specimen thickness. This result leads to the conclusion that specimens are always decaying at the same rate although the periodicity of crystals still remains in thick specimens. The conclusion is interpreted as being the result of the radiation damage mechanism based on longitudinal motions of long chain molecules. For the evaluation of beam damage effect the broadening rate and the extinction dose should be used as indicator for the radiation sensitivity of crystals and for the possibility of observing diffraction patterns, respectively.