Large-angle Convergent-beam Electron Diffraction Research Articles

Large-Angle Rocking Beam Electron Diffraction of Large Unit Cell Crystals Using Direct Electron Detector.

We report a large-angle rocking beam electron diffraction (LARBED) technique for electron diffraction analysis. Diffraction patterns are recorded in a scanning transmission electron microscope (STEM) using a direct electron detector with large dynamical range and fast readout. We use a nanobeam for diffraction and perform the beam double rocking by synchronizing the detector with the STEM scan coils for the recording. Using this approach, large-angle convergent beam electron diffraction (LACBED) patterns of different reflections are obtained simultaneously. By using a nanobeam, instead of a focused beam, the LARBED technique can be applied to beam-sensitive crystals as well as crystals with large unit cells. This paper describes the implementation of LARBED and evaluates the performance using silicon and gadolinium gallium garnet crystals as test samples. We demonstrate that our method provides an effective and robust way for recording LARBED patterns and paves the way for quantitative electron diffraction of large unit cell and beam-sensitive crystals.

Strain visualization using large-angle convergent-beam electron diffraction

In this study, we report a strain visualization method using large-angle convergent-beam electron diffraction (LACBED).11large-angle convergent-beam electron diffraction (LACBED); scanning transmission electron microscopy (STEM); nanobeam electron diffraction (NBD); personal computer (PC); diffraction pattern (DP); transmission electron microscopy (TEM); convergent beam electron diffraction (CBED); four-dimensional (4D); gigabytes (GB); region of interest (ROI); Gatan Microscopy Suite (GMS); selected area (SA); focused ion beam (FIB); embedded SiGe (eSiGe); complementary metal-oxide semiconductor (CMOS); full width at half maximum (FWHM); cross-correlation (CC); shallow trench isolations (STIs). We compare the proposed method with the strain maps acquired via STEM-NBD, a combination of scanning transmission electron microscopy (STEM) and nanobeam electron diffraction (NBD). Although STEM-NBD can precisely measure the lattice parameters, it requires a large amount of data and personal computer (PC) resources to obtain a two-dimensional strain map. Deficiency lines in the transmitted disk of LACBED reflect the crystalline structure information and move, curve, or disappear in the deformed area. Properly setting the optical conditions makes it possible to acquire real-space images over a broad area in conjunction with deficiency lines on the transmitted disk. The proposed method acquires images by changing the relative position between the specimen and the deficiency line and can grasp the strain information with a small number of images. In addition, the proposed method does not require high-resolution images. It can reduce the required PC memory or storage consumption in comparison with that of STEM-NBD, which requires a high-resolution diffraction pattern (DP) from each point of the region of interest. Compared with the two-dimensional maps of LACBED and NBD, NBD could detect large distortions in the area where the deficiency line curved, moved, or disappeared. The curving or moving direction of the deficiency line is qualitatively consistent with the NBD results. If quantitative strain values are not essential, strain visualization using LACBED can be considered an effective technique. We believe that the strain information of a sample can be obtained effectively using both methods.

Observation of threading dislocations with a c + m type Burgers vector in HVPE GaN substrates using multi-photon excitation photoluminescence and TEM

Dislocations that have a large Burgers vector are potential leakage current pathways in power devices. In this study, we analyzed the dislocations under a large pit (L-pit) produced by chemical etching in a hydride-vapor-phase-epitaxy GaN substrate by using multi-photon excitation photoluminescence (MPPL) and transmission electron microscopy (TEM). Three-dimensional dislocation images reconstructed from MPPL clearly showed that two threading dislocations (TD-1 and TD-2) approached each other laterally while propagating along the growth direction [0001]. They interacted near the sample surface and merged into a single dislocation whose large Burgers vector was responsible for the L-pit formation. A TEM observation operated in large-angle convergent-beam electron diffraction mode unambiguously identified the Burgers vectors of the two dislocations as bTD-1=13[2-1-1-3] (c + a type) and bTD-2 = [10–1–1] (c + m type). The c + m type is extremely rare in GaN. The merged dislocation appeared to constitute Burgers vectors of all three components of c, m, and a.

Prospects of the multislice method for CBED pattern calculation

Abstract We recently showed that the Multisclice method can be used to elucidate the crystal volume contribution to a CBED pattern. Here, we demonstrate in more detail how the directions of each HOLZ line, their Laue zone order, and the specimen thickness determine the volume segment of the Bragg scattering cone of the electron beam and show that secondary rescattering from this volume must take place for deficient line formation in the (000) CBED disk. Moreover, additional prospects of the multislice method are demonstrated such as calculation of line splitting in bent crystals, hollow cone dark-field CBED, large-angle CBED, and whole diffraction patterns including Kikuchi lines.

Identification of type of threading dislocation causing reverse leakage in GaN p\u2013n junctions after continuous forward current stress

Power devices are operated under harsh conditions, such as high currents and voltages, and so degradation of these devices is an important issue. Our group previously found significant increases in reverse leakage current after applying continuous forward current stress to GaN p–n junctions. In the present study, we identified the type of threading dislocations that provide pathways for this reverse leakage current. GaN p–n diodes were grown by metalorganic vapor phase epitaxy on freestanding GaN(0001) substrates with threading dislocation densities of approximately 3 × 105 cm−2. These diodes exhibited a breakdown voltage on the order of 200 V and avalanche capability. The leakage current in some diodes in response to a reverse bias was found to rapidly increase with continuous forward current injection, and leakage sites were identified by optical emission microscopy. Closed-core threading screw dislocations (TSDs) were found at five emission spots based on cross-sectional transmission electron microscopy analyses using two-beam diffraction conditions. The Burgers vectors of these dislocations were identified as [0001] using large-angle convergent-beam electron diffraction. Thus, TSDs for which b = 1c are believed to provide current leakage paths in response to forward current stress.

Machine learning calculation of large-angle convergent-beam electron diffraction patterns

Machine learning calculation of large-angle convergent-beam electron diffraction patterns

Propagation of threading dislocations and effects of Burgers vectors in HVPE-grown GaN bulk crystals on Na-flux-grown GaN substrates

The propagation behavior of threading dislocations (TDs) and the effects of Burgers vectors in hydride vapor phase epitaxy (HVPE) GaN bulk crystals generated on Na-flux-grown GaN and in a commercially available HVPE-grown GaN bulk crystal were investigated. Analyses based on chemical etching and transmission electron microscopy (TEM) revealed a close correlation between the etch pit sizes and the Burgers vector of these TDs. The existence of TDs with the unique Burgers vector b = 1m + 1c was observed for the first time ever using a large-angle convergent-beam electron diffraction technique and plan-view bright-field scanning TEM. Multi-photon excitation photoluminescence microscopy observations showed that TDs with b = 1c had a meandering morphology in contrast to the linear morphology of TDs with b = 1a, 1a + 1c, or 1m + 1c in both types of HVPE-grown GaN crystals. The inclinations of TDs with b = 1a and 1a + 1c in HVPE-grown GaN on Na-flux-grown GaN were greatly affected by large symmetrical hexagonal hillocks. The TDs with b = 1a were inclined in the slope directions of the hillock planes, while those with b = 1a + 1c were inclined in the a directions parallel or antiparallel to the a component in their Burgers vector. These inclinations were readily explained by the isotropic elastic theory of an individual TD. The hillocks were produced around pairs of parallel mixed TDs for which the a components were opposite to one another. This phenomenon was attributed to inclusions at the interface between the Na-flux-grown GaN substrate and the HVPE-grown layer. The origins of other TDs including unusual ones having b = 1m + 1c are also discussed herein.

A new electron diffraction approach for structure refinement applied to Ca3Mn2O7.

The digital large-angle convergent-beam electron diffraction (D-LACBED) technique is applied to Ca3Mn2O7 for a range of temperatures. Bloch-wave simulations are used to examine the effects that changes in different parameters have on the intensity in D-LACBED patterns, and atomic coordinates, thermal atomic displacement parameters and apparent occupancy are refined to achieve a good fit between simulation and experiment. The sensitivity of the technique to subtle changes in structure is demonstrated. Refined structures are in good agreement with previous determinations of Ca3Mn2O7 and show the decay of anti-phase oxygen octahedral tilts perpendicular to the c axis of the A21am unit cell with increasing temperature, as well as the robustness of oxygen octahedral tilts about the c axis up to ∼400°C. The technique samples only the zero-order Laue zone and is therefore insensitive to atom displacements along the electron-beam direction. For this reason it is not possible to distinguish between in-phase and anti-phase oxygen octahedral tilting about the c axis using the [110] data collected in this study.

Evaluation of accuracy in the determination of crystal structure factors using large-angle convergent-beam electron diffraction patterns.

The accuracy of electron density distribution analysis using large-angle convergent-beam electron diffraction (LACBED) patterns is evaluated for different convergence angles. An orbital ordered state of FeCr2O4 is used as an example of the analysis. Ideal orbital-ordered and non-ordered states are simulated by using orbital scattering factors. LACBED patterns calculated for the orbital-ordered state were used as hypothetical experimental data sets. Electron density distribution of the Fe 3d orbitals has been successfully reconstructed with a higher accuracy from LACBED patterns with convergence angles larger than 15.2 mrad, which is 4 times as large as that for conventional convergent-beam electron diffraction patterns. Excitation of particular Bloch waves with the aid of LACBED patterns has a key role in the accurate analysis of electron density distributions.

Nanoestructuras y su caracterización por medio de microscopía electrónica de transmisión; ciencia y arte

En el presente trabajo se describen de forma didáctica los alcances de la Microscopia Electrónica de Transmisión (TEM) para el estudio de nanosistemas. Para ilustrar el uso de las técnicas TEM, se utilizaron nanopartículas de Au y películas de Si adelgazadas con iones.Se describen técnicas de estudio convencional en TEM, como campo claro (BF), camp obscuro (DF), HAADF, SAED y EELS; además se mencionan las ventajas que ofrece el empleo de técnicas menos convencionales como CBED, LACBED y PED. También se brindan algunas sugerencias prácticas que permitirán describir y diferenciar de forma sencilla el contraste observado en las distintas técnicas disponibles en el TEM con el objetivo de ofrecer una visión, llamativa, clara y didáctica de los alcances actuales de la microscopia electrónica en México.

Observation of dislocations in β-Ga2O3 single-crystal substrates by synchrotron X-ray topography, chemical etching, and transmission electron microscopy

To reveal dislocations in β-Ga2O3 and categorize them by their Burgers vectors, we have carried out a comprehensive dislocation characterization by synchrotron X-ray topography (XRT), chemical etching, and transmission electron microscopy (TEM). An important type of dislocation confirmed by XRT is the screw-type dislocations extending in the 〈010〉 direction at a density of about 4.2 × 104 cm−2. These dislocations had length in millimeters and seldom bent to other directions. Chemical etching using molten KOH + NaOH at 200 °C formed hillocks with multiple crystallographic facets on the (010) surface. These hillocks showed various geometrical features that indicated the direction of the dislocation lines. TEM observation confirmed that the hillocks were related to dislocations. Finally, the feasibility of using TEM weak-beam dark-field images and large-angle convergent-beam electron diffraction to identify dislocation Burgers vectors was examined, which seemed to be problematic due to the low-symmetry of the monoclinic crystal structure of β-Ga2O3.

Dislocation Analysis in SiGe Heterostructures by Large-Angle Convergent Beam Electron Diffraction

Dislocations play a crucial role in self-organization and strain relaxation mechanisms in SiGe heterostructures. In most cases, they should be avoided, and different strategies exist to exploit their nucleation properties in order to manipulate their position. In either case, detailed knowledge about their exact Burgers vectors and possible dislocation reactions are necessary to optimize the fabrication processes and the properties of SiGe materials. In this review a brief overview of the dislocation mechanisms in the SiGe system is given. The method of choice for dislocation characterization is transmission electron microscopy. In particular, the article provides a detailed introduction into large-angle convergent-beam electron diffraction, and gives an overview of different application examples of this method on SiGe structures and related systems.

Direct evaluation of threading dislocations in 4H-SiC through large-angle convergent beam electron diffraction

ABSTRACTIn this study, the structures of threading dislocations (TDs) in a 4H-SiC epilayer were directly characterised using large-angle convergent beam electron diffraction (LACBED) via transmission electron microscopy (TEM), by examining the splitting of reflections due to the presence of dislocation lines. Previously, X-ray topography (XRT) mapping in combination with ray-tracing simulations has been shown to be an efficient method for imaging and differentiating common TD types and variants in 4H-SiC. In this work, the validity of XRT-based results was verified by LACBED through direct evaluation and differentiation of the Burgers vectors and physical crystallographic features of all threading edge, threading screw, and threading mixed dislocations variants. The LACBED results agreed with the XRT-based results with respect to TD type and variant. The screw-sense or half-plane orientation and Burgers vector determined from LACBED analysis for each TD were self-consistent. For the case of -TEDs, atomic-resolution analysis of the core structure, through high-angle annular dark field scanning TEM, directly revealed two half-planes, each with a Burgers vector component, and the sum of these components was confirmed to be . Finally, an algorithm for efficient LACBED analysis of TDs in 4H-SiC was discussed.

Structure refinement from ‘digital’ large angle convergent beam electron diffraction patterns

We use semi-automated data acquisition and processing to produce digital large angle CBED (D-LACBED) patterns. We demonstrate refinements of atomic coordinates and isotropic Debye–Waller factors for well-known materials using simulations produced with a neutral, spherical independent atom model. We find that atomic coordinate refinements in Al2O3 have sub-pm precision and accuracy. Isotropic DWFs are accurate for Cu, a simple fcc metal, but do not agree with X-ray measurements of GaAs or Al2O3. This lack of agreement is probably caused by bonding and change transfer between atoms. While it has long been appreciated that CBED is sensitive to bonding, examination of D-LACBED data shows that some regions exhibit large changes in diffracted intensity from small changes in the periodic crystal potential. Models of bonding will be essential to fully interpret D-LACBED data.

A New and Unexpected Spatial Relationship Between Interaction Volume and Diffraction Pattern in Electron Microscopy in Transmission.

The finding of this study is that the interaction volume in electron microscopy in transmission is well ordered laterally, with a remarkable and unexpected consequence being that lateral subsections of the interaction volume produce subsections of the Kikuchi diffraction pattern. It makes the microstructure of samples directly visible in Kikuchi patterns. This is first illustrated with polycrystalline Ti-10Al-25Nb with an on-axis transmission Kikuchi diffraction set-up in a scanning electron microscope. It is then shown via a Monte Carlo simulation and a large-angle convergent-beam electron diffraction experiment that this phenomenon finds its origin in the nature of the differential elastic and quasi-elastic cross sections. This phenomenon is then quantified by a careful image analysis of Kikuchi patterns recorded across a vertical interface in a silicon sample specifically designed and fabricated. A Monte Carlo simulation reproducing all the geometric parameters is conducted. Experiments and simulations match very well qualitatively, but with a slight quantitativity gap. The specificity of the thermal diffuse scattering cross-section, not available in the simulation, is thought to be responsible for this gap. Beside Kikuchi diffraction, the case of diffraction spots and diffuse background present in the pattern is also discussed.

Investigation of nanoscale twinning in an advanced high manganese twinning-induced plasticity steel

A twinning induced plasticity (TWIP) steel, developed for automotive applications, was characterized down to the nanoscale to investigate the nature of the strengthening mechanisms. Both tensile-deformed and non-deformed materials were studied by light optical microscopy, X-ray diffraction, electron backscatter diffraction, and transmission electron microscopy. The investigated TWIP steel showed extensive twinning upon deformation. With high-resolution transmission electron microscopy, nano-twins as small as 3 nm in width were observed, and large-angle convergent-beam electron diffraction identified the pole mechanism as one of the twinning mechanisms in this TWIP steel. This study emphasizes that a thoughtful combination of techniques is necessary to fully capture the microstructure of this TWIP steel and explain the origin of superior mechanical properties compared to other TWIP steel grades.

Electric-field-induced domain intersection in BaTiO3 single crystal

Large-angle convergent beam electron diffraction was used to determine the directions of polarization vectors in a BaTiO3 single crystal. Domain intersections driven by an electric field were investigated by in situ transmission electron microscopy. The dark triangles observed in the domain intersection region can be accounted for by dislocations and the strain field. Domains nucleate at the domain tip depending on the dislocations and strain field to relieve the accumulated stress. Schematic representations of the intersecting domains and the microscopic structure are given, clarifying the special electric-field-induced domain structure.

Observation of reaction between a-type dislocations in GaN layer grown on 4-in. Si(111) substrate with AlGaN/AlN strained layer superlattice after dislocation propagation

Dislocation reaction in a GaN layer grown on 4-in. Si(111) with AlGaN/AlN strained layer superlattice was observed by transmission electron microscopy. The reaction between a dislocation (b=1/3[12¯10]) and another dislocation (b =1/3[112¯0]) to form a dislocation segment (b =1/3[21¯1¯0]) was demonstrated by plan-view observation using weak-beam dark-field and large-angle convergent-beam electron diffraction methods. Observed reaction occurred with dislocation motion after dislocation propagation with epitaxial growth.

Characterization of Threading Screw Dislocations of Burgers Vectors with A-Components in 4H-SiC

We characterized threading screw dislocations to investigate the influence on device performance. The Burgers vectors of the threading screw dislocations (a total of 28dislocations) in 4H-SiC were determined by large-angle convergent-beam electron diffraction. A new type of TSD, b=c+2a dislocation was identified. And all of the four types of TSD predicted were identified. The frequency of their occurrence observed experimentally is in good agreement with theoretical prediction. In addition, we investigated relations of Burgers vector and the dislocation line direction. It has been confirmed that the Burgers vector of TSD does not necessarily coincide with the direction of dislocation lines. Looking ahead, we need to investigate how the angle between Burgers vector and dislocation line influence device performance.

Propagation and annihilation of threading dislocations during off-axis growth of heteroepitaxial diamond films

Threading dislocations in heteroepitaxial diamond films deposited on Ir/YSZ/Si(001) substrates with an off-axis angle of 4° towards [100] have been studied by cross-section transmission electron microscopy using the weak-beam dark-field (WBDF) technique for Burgers vector identification and large-angle convergent beam electron diffraction (LACBED) in order to facilitate a precise crystallographic determination of the local growth surface. Close to the diamond/iridium interface the films contain a high density of dislocations of both 90° and 45° types. Within the first micron of film growth their density decreases drastically by annihilation or mutual interaction resulting in a preference for 45° type dislocations. Vicinal growth surfaces cause a tilt of the dislocation line vector away from the crystallographic [001] axis in the step-flow direction. Tilting is influenced by gas phase impurities. With 100ppm nitrogen in the feed gas, step bunching produces a structured surface consisting of an alternating sequence of terraces with reduced off-axis angle crystallographically close to (001) and risers with increased off angle. The dislocations with lines close to [001] during terrace growth abruptly tilt by more than 20° at the transition to riser growth. The appearance of several discrete tilt angles during nitrogen free growth without pronounced step bunching is attributed to the corresponding Burgers vectors which cause either effective climb for the lower angles or effective glide for the higher ones. The present observations are of high relevance for improved strategies towards a further dislocation density reduction and an efficient control of intrinsic stress formation.