Microstructural Defects Research Articles

Interaction of Stacking Faults with point/extended defects in Fe-He irradiated 6H-SiC

The study explored the microstructure evolution of 6H-SiC that underwent sequential iron and helium ion irradiation with energies of 2.5 MeV and 500 keV, respectively, at room temperature, followed by annealing at 1500°C for two hours. Following irradiation, the entire damaged layer underwent amorphization. However, during subsequent annealing, epitaxial recrystallization took place, resulting in the formation of defected polycrystalline 6H-SiC characterized by the presence of Fe-rich clusters, cavities, and stacking faults. Fe-rich cavities were found to predominantly form at the edges of the stacking faults, as revealed by XTEM. The interaction of microstructural defects is further investigated via first-principles calculations. The periphery of the stacking faults has been identified as the primary location for the emergence of vacancy clusters, serving as favorable sites for the accumulation of point defects, including Fe atoms. This behavior can be attributed to the combined effects of mechanical and electronic energy relaxation mechanisms. Mechanically, the presence of stacking faults allows for the release of elastic energy that had been stored at the boundary. Electronically, the energy relaxation arises from the saturation of C- and Si-dangling bonds. Both of these processes contribute to the observed behavior, highlighting the intricate interplay between mechanical and electronic factors in the system. The low point defect migration energy barriers in the vicinity of the stacking faults promise high recombination, which can limit cavity growth and enhance radiation resistance. The study not only offers valuable insights into the mechanism of cavity/stacking faults interaction, contributing to a better understanding of radiation damage in 6H-SiC but also demonstrates that 6H-SiC material containing stacking faults could serve as a viable alternative to 3C-SiC for nuclear application.

Sb Alloying for Engineering High‐Thermoelectric zT of CuGaTe2

Decades of studies on thermoelectric materials have enabled the design of high‐performance materials based on basic materials properties, such as bandgap engineering. In general, bandgap energies correspond to the temperature at which the peak thermoelectric performance occurs. For instance, CuGaTe2 with a relatively wide bandgap of 1.2 eV has its peak zT > 1 at > 900 K. On the other hand, the zT is usually very low (<0.1) for this material at room temperature. This severely limits its average zT and hence overall performance. In this study, a phase diagram‐guided Sb alloying strategy to improve the low‐temperature zT of CuGaTe2 is used, by leveraging on the solubility limits to control the formation of the microstructural defects. The addition of Sb simultaneously improves the electrical conductivity and decreases the lattice thermal conductivity. For a low‐temperature range of 300–623 K, this Sb‐alloying strategy enables the achievement of a record high average zT of 0.33. The strategy developed in this study targets the improvement of the low‐temperature range of CuGaTe2, which is rarely focused on for wide‐bandgap ABX2 compounds, opening up more opportunities for holistic performance improvements, potentially enabling ultrahigh‐performance thermoelectrics over a wide temperature range.

Structure formation of Np-30KhGSA alloy in wire and arc additive manufacturing

The use of metallic products 3D-printing is a modern, promising technology that improves production efficiency. However, using this technology is associated with a number of problems, for example, with increased microstructural heterogeneity and defects in metal. Therefore, it is necessary to carry out researches to identify 3D-printing modes ensuring the most homogeneous, stable and non-defect structure. In this work, a study was made of the process of structure formation of 30KhGSA steel in the process of Wire and Arc Additive Manufacturing (WAAM) under various printing modes. Microstructural analysis, microhardness measurement and fractal analysis were used for assessment of the obtained billets. In all surfacing modes, a significant structural inhomogeneity of the deposited billet was revealed, which is explained by the thermal effect of the deposited layer on the already crystallized metal. Nevertheless, we found the mode that gives the most favorable microstructure in terms of its uniformity and equiaxed grains. With an increase in WAAM heat input values, an increase in the productivity of the process is observed and a decrease in the number of pores in the material is recorded. However, when the heat input of the surfacing process exceeds 1000 J/mm, the structural inhomogeneity of the material increases and its microhardness significantly decreases. Based on the studies, as a WAAM 3D-printing mode for Np-30KhGSA alloy, a mode with a heat input of about 920 J/mm can be chosen, which provides the lowest structural inhomogeneity and a sufficiently high productivity of the growth process with the absence of defects in the form of pores and elements of not melted wire.

High-resolution Bragg-edge neutron radiography detects grain morphology in PBF-LB/M IN718

One of the main advantages of metal additive manufacturing (MAM) techniques is their ability to produce components with site-specific microstructural features. Nevertheless, microstructural defects and lack of repeatability are still major concerns in MAM. In this study, a laser powder bed fusion (PBF-LB/M) IN718 material, produced using two different scan length vectors, is investigated using Bragg-edge neutron 2D imaging (BENI) combined with electron backscatter diffraction (EBSD) analysis. BENI is able to detect, on a macroscopic scale, process-induced changes in texture in a large field of view covering the entire sample (20×80 mm2). In addition, high-resolution BENI (HR-BENI), with a pixel size of 12.8 µm, provides a micro-scale examination of the local variations of texture and grain morphology, otherwise undistinguishable using the standard resolution. As such, HR-BENI offers a straightforward and detailed way of screening the integrity of MAM parts at cm-length scales.

Formation of Twin Boundaries in Rapidly Solidified Metals through Deformation Twinning.

The rapid solidification process is relevant to many emerging metallurgical technologies. Compared with conventional solidification processes, high-density microstructure defects and residual thermal stress are commonly seen in rapidly solidified metals. Among the various defects, potentially beneficial twin boundaries have been observed in the rapidly solidified nanocrystalline microstructures of many alloy systems. In this work, a pathway for forming twin boundaries in rapid solidification processes is proposed. A detailed derivation of strain inhomogeneities upon thermal shrinkage and the deformation twinning phase field method is given. By calculating cooling-induced thermal strain inhomogeneity in nanocrystalline metals and growth thresholds for deformation twinning using the phase field method, it is shown that residual thermal strain hotspots in the microstructure can reach the threshold for deformation twinning when the shear elastic property of grain boundaries is significantly different from the bulk.

Numerical studies of self-organization of shear bands in one and two dimensions

In the present manuscript we perform a numerical analysis of the self-organization processes of adiabatic shear bands formation in depleted uranium, aluminum alloy, and high-strength steel in one- and two-dimensional cases. Since the processes of shear bands formation are strongly nonlinear, three materials with significantly different parameters considered allow us to generalize obtained dependencies. For all materials, we investigate the evolution of stress, temperature and velocity fields from initial to final stage of localization. It is well known that localization processes occur during the high shear rate loads in the presence of initial microstructural defects in metallic materials. Starting with a random distribution of initial stress, which models microstructural defects, we obtained new dependencies for such significant parameters of the problem considered such as localization time and spacing between shear bands. The influence of initial plastic strain rate on these parameters was also studied. We obtain the linear dependence of localization time on initial strain rate and show that spatial dimension significantly influences on its value. Also, we introduce the method of shear bands selection during computations and present new statistical distributions for band spacing. We show that the interaction between shear bands significant influences on the spacing between them.

A comprehensive study on the influence of the scan pattern in two porosity levels and surface roughness on the fatigue behavior of laser powder bed fusion manufactured specimens made of steel H13

As a developing and immature technique, additive manufacturing (AM) shows some limitations: depending on material and process parameters so far, it usually results in parts with residual porosity, high residual stresses and a surface with a certain level of roughness. Due to its weaknesses and high production costs, AM is more preferably used when the fabricated parts have a high geometry complexity, the material used is very expensive, or the parts can offer additional performance. In order to allocate AM further in industry, a better understanding of the not well-investigated fatigue behavior is necessary. This work focuses on the influences of some general process parameters including laser power, scan speed, scan pattern and postmachining on the resulting fatigue properties of H13 tool steel specimens generated through powder bed fusion (PBF) technique. Results reveal that scan patterns influence fatigue properties by affecting the largest porous defect size and microstructure thus matrix strength. The degree of porosity or roughness resulting from the energy input and postmachining has a significant inferior impact on the fatigue strength. Neither porosity nor tensile properties show a single direct mathematic correlation with the fatigue properties.

Microstructural evolution of extended defects in 25 μ m thick GaN homo-epitaxial layers

Defect origins and their propagation behavior were investigated in 25 μm thick homo-epitaxial GaN layers grown on ammono-thermal and void-assisted separation (VAS) substrates using multi-vector x-ray topography in both transmission and reflection geometries. Complex inclusions were identified and their microstructure was analyzed. Additionally, generation of threading dislocation clusters during epitaxial growth is analyzed. Various defects are delineated from the substrate vs epitaxial layers. Growth on the ammono-thermal substrate led to less defective and flatter epitaxial layers compared to the growth on the VAS substrate. Determining the origins and microstructure of defects is crucial toward developing defect mitigation strategies for reliable GaN devices.

3D hierarchical porous structures printed from a silica-nickel composite paste

Material extrusion of paste as one of the 3D printing techniques is commonly used in additive manufacturing industry. It allows to efficiently obtain structures of complex geometry at a relatively low cost. Ceramics are among the materials eagerly printed with this technique, especially as a support material. Hence, the combination of silica as base material and nickel as catalyst seems to be a highly promising system in processes such as CO2 methanation or hydrogenation processes.The key aspects that should be taken into consideration when designing a new material are the proper material composition, its microstructure, as well as the final properties. From the point of view of the above-mentioned applications, material should have high open porosity. Appropriate micro- and macroporosity enable the optimal flow of liquid and gaseous reagents through the material, ensuring high efficiency of the processes carried out. It is also crucial to select the appropriate catalytic material, hence the use of nickel as a catalytically active metal was proposed for the research.This article demonstrates the development, preparation and characterization of silica-nickel porous structures obtained via material extrusion. The nanosilica-Ni paste with 75 wt% of Ni powder particles was prepared with stirring and degassing for homogenous consistency. 3D printed scaffolds have undergone heat treatment to remove the organic binders and partially sintered to achieve a relevant mechanical strength. The analysis of the paste was performed using the detailed thermal analysis, XRD analysis and Raman spectroscopy for a determination of the optimal thermal processing conditions. In addition, the characterization of the final materials was carried out to confirm the effectiveness of the procedures developed. Application of the reductive atmosphere (mixture of N2+H2) during heat treatment prevented nickel particles from oxidation, as well as strongly eliminated the microstructure defects such as cracking and material shrinkage. The results demonstrate the perspective application of material extrusion as a printing technique of highly porous materials with well-preserved pre-designed 3D geometry.

Half-Heusler alloys as emerging high power density thermoelectric cooling materials

To achieve optimal thermoelectric performance, it is crucial to manipulate the scattering processes within materials to decouple the transport of phonons and electrons. In half-Heusler (hH) compounds, selective defect reduction can significantly improve performance due to the weak electron-acoustic phonon interaction. This study utilized Sb-pressure controlled annealing process to modulate the microstructure and point defects of Nb0.55Ta0.40Ti0.05FeSb compound, resulting in a 100% increase in carrier mobility and a maximum power factor of 78 µW cm−1 K−2, approaching the theoretical prediction for NbFeSb single crystal. This approach yielded the highest average zT of ~0.86 among hH in the temperature range of 300-873 K. The use of this material led to a 210% enhancement in cooling power density compared to Bi2Te3-based devices and a conversion efficiency of 12%. These results demonstrate a promising strategy for optimizing hH materials for near-room-temperature thermoelectric applications.

Influence of heat treatment, microstructure evolution, and damage mechanism on high cycle fatigue behaviour of additively manufactured Ti-modified Al 2024 alloy

The high cycle fatigue behaviour of titanium modified Al 2024 alloy produced by laser powder bed fusion (LPBF) is investigated to elucidate the effect of the microstructural features, residual stress, and defects (such as porosity and lack of fusion) on dynamic behaviour. The titanium acts as a grain refining agent; it can reduce the solidification cracking and produce the ultrafine-grained (UFG) microstructure in aluminium alloys. The 2% titanium addition resulted in the UFG microstructure with an average size of 0.52 μm in as-built samples. The microstructural features were examined through scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electron back-scattered diffraction (EBSD) analysis. The influence of the microstructural features, such as grain size, dislocation density, precipitate-dislocation interaction, etc., on the fatigue life of as built and T6 heat treated samples was analysed in detail. The effect of varying stress amplitude at a stress ratio of 0.1 and a frequency of 30 Hz was investigated for the as-built and heat-treated sample. The T6 heat-treated sample showed 21.9% higher fatigue strength compared to the as-built samples (87.8 MPa in the heat-treated sample compared to 72 MPa in the as-built sample). The corresponding damage mechanisms are thoroughly explored through scanning electron fractography, TEM, and EBSD. The defects like porosity and lack of fusion defects in the surface or sub-surface level were observed to be critical regions as crack initiation sites.

An Investigation into the Deterioration of Copper Surface Quality in Plasma Electrolytic Polishing

Plasma electrolytic polishing (PEP) is widely used in the finishing process of metallic parts. Some parts with narrow structures always suffer from surface quality deterioration in the PEP process. In this paper, the deterioration of surface quality was studied to reveal the vapor film evolution mechanism during the polishing. The conditions for the bump defects generation were investigated with the comparison of polished surface morphology under different voltages and immersion depths. The reasons for the bump defects generation were analyzed through the compositions, the chemical states of the elements, and the microstructure of bump defects. The relationship between the current density, the thickness of the vapor film, and the heat to maintain the vapor film was discussed. The vapor film was maintained by Joule heat generated by itself. During the PEP process, excessive current density on the anode surface made the vapor film thickness greater than the critical value of heat could maintain, leading to the collapse of the vapor film. The anode then came into partial contact with the electrolyte, resulting in bump defects. As a result, it is suggested that the thickness of the vapor film be reduced to prevent the surface quality of narrow structures from deteriorating.

Effect of Cobalt Fraction Mixing WC Clads on Microstructural Evolution, Crack Formation and Tribological Properties by Laser Cladding

In the present work, a ceramic-matrix composite coatings with different weight percentages of Co additive in the WC powders was studied on 45 steel by laser cladding. The effect of cobalt mixture with WC on mechanical properties such as microstructural evolution, hardness, wear and residual stress behavior of the coatings was carried out. The results show that high residual stresses induce significant cracking on 100% WC and that cracking activity is reduced by adding concentrations of 20% Cobalt to WC. Further, the microhardness of the coatings was more than five times higher than that of the substrate. The observation of the microstructural evolution reveals the fracture mechanism is a typical intergranular fracture in the molten zone and the crack propagates through the interior of the unmelted WC at 100% WC. Overall, the additive of high cobalt in WC did not result in a reduction of residual stresses due to less amount of brittle carbide. However, a reduced number of microstructural defects as well as a better wear behavior were obtained for the WC coated layers with suitably added Cobalt alloys.

Nano to micrometer range particle size effect on the electrical and piezoelectric energy harvesting performances of hydroxide mediated crosslinked PVDF composites

The polar phase and piezoelectric response of filler-loaded PVDF-based composites very often depend on the interfacial interaction between the filler surface and PVDF dipoles. In this regard, hydrogen bonding interaction has shown a much stronger effect compared to other interactions. In order to induce hydrogen bonding interaction, the filler surface is commonly modified by various modifiers. In the present work, instead of filler surface modification, we introduce ZnSn(OH)6 filler (hydroxide filler having a high number of –OH groups) into the PVDF matrix in order to facilitate the hydrogen bonding interaction. Not only the hydroxide fillers but the effect of wide particle size variation (from nano to micrometer range) into PVDF has also been shown here for the very first time. ZnSn(OH)6 fillers with similar morphology but different sizes have been synthesized by using a variety of techniques and then incorporated into the PVDF matrix. The microstructural defects of the composite films have been found to be gradually increased with the increase in filler size which in turn caused to gradually increase their space charge polarization. Filler, with 915 nm size has shown the best polar phase formation (∼84 %), dielectric permittivity (∼10 at 1 kHz), and piezoelectric energy harvesting performance (output voltage ∼20 V) of the resulting PVDF-based composite and hence has been used for various real-life applications. All of these results have been suitably explained here on the basis of interfacial interaction, microstructural defect, and the mechanism of formation of space charge polarization.

Effect of retained austenite on the fatigue behavior of modified bainitic 100Cr6 steels considering local phase transformation

Since highly loaded components, such as roller bearings, tend to have relatively high lifetime scatter caused by microstructural defects, an increased defect tolerance of the material can improve the performance as well as the reliability of these highly stressed components. To increase the defect tolerance of the roller bearing steel 100Cr6, two different laboratory melts with either 1.5 wt.-% Al or 1.5 wt.-% Si in addition to the standard composition were developed. After an adapted heat treatment, both steels exhibited a bainitic microstructure with a relatively high content of retained austenite with more than 20 vol.-%. Considering the effects of the retained austenite, a defined mechanical stability is essential to avoid excessive deformation-induced transformation from the retained austenite into α′-martensite, which can lead to shape deviations in components. However, besides the increased deformability of the austenitic phase, local phase transformations in the vicinity of defects can increase the defect tolerance. The fatigue tests performed at ambient temperature (AT) and at T = 100 °C, show a higher fatigue strength of the Si-alloyed steel due to a refined microstructure and revealed for both steels a relatively high austenite stability, since no macroscopic phase transformation was observed. The high austenite stability can be explained by a relatively high carbon content of the austenitic phase. However, in contrast to the Al-alloyed steel, a decrease in the fatigue strength and in the defect tolerance due to the increased temperature were observed for the Si-alloyed steel, which indicates a more pronounced phase transformation at AT. The lower carbon content and the finer distribution of the retained austenite, when compared to the Al-alloyed steel, are supposed to be the reason. While a smaller carbon content decreases the phase stability, the refined austenite distribution results in a higher probability of retained austenite presence in the vicinity of a defect.

Functional Epicardial Conduction Disturbances Due to a SCN5A Variant Associated With Brugada Syndrome

BackgroundBrugada syndrome is a significant cause of sudden cardiac death (SCD), but the underlying mechanisms remain hypothetical. ObjectivesThis study aimed to elucidate this knowledge gap through detailed ex vivo human heart studies. MethodsA heart was obtained from a 15-year-old adolescent boy with normal electrocardiogram who experienced SCD. Postmortem genotyping was performed, and clinical examinations were done on first-degree relatives. The right ventricle was optically mapped, followed by high-field magnetic resonance imaging and histology. Connexin-43 and NaV1.5 were localized by immunofluorescence, and RNA and protein expression levels were studied. HEK-293 cell surface biotinylation assays were performed to examine NaV1.5 trafficking. ResultsA Brugada-related SCD diagnosis was established for the donor because of a SCN5A Brugada-related variant (p.D356N) inherited from his mother, together with a concomitant NKX2.5 variant of unknown significance. Optical mapping demonstrated a localized epicardial region of impaired conduction near the outflow tract, in the absence of repolarization alterations and microstructural defects, leading to conduction blocks and figure-of-8 patterns. NaV1.5 and connexin-43 localizations were normal in this region, consistent with the finding that the p.D356N variant does not affect the trafficking, nor the expression of NaV1.5. Trends of decreased NaV1.5, connexin-43, and desmoglein-2 protein levels were noted; however, the RT-qPCR results suggested that the NKX2-5 variant was unlikely to be involved. ConclusionsThis study demonstrates for the first time that SCD associated with a Brugada-SCN5A variant can be caused by localized functionally, not structurally, impaired conduction.

Flexible and mechanically strong MXene/cellulose-lamellae sheets for electromagnetic interference shielding

MXene, two-dimensional layered transition metal carbides, nitride, or carbonitrides, have shown promise for ultrahigh electromagnetic interference (EMI) shielding in flexible electronics and aerospace due to their intrinsic metallic conductivity and mechanical strength. However, weak interfacial interactions, void microstructure defects, and oxidative degradation can leave MXene sheets in a thermodynamically metastable state, resulting in poor EMI shielding and mechanical strength. Herein, we utilized abundant hydrogen-bonded ultrafine cellulose lamella (UCL) to sequentially bridging induced densification of MXene nanosheets. This resulted in improved the tensile strength, toughness, oxidative stability, resistance to ultrasonic decomposition, and super-foldable conductivity of MXene sheets. The resulting MXene@UCL sheets (MXCS) exhibited high electrical conductivity of up to 7649 S cm−1 and ultrahigh weight-normalized shielding efficiency (SSE/t, 53003.45 dB∙cm2 g−1), making them mechanically strong and highly conductive. The MXCS material has a tensile modulus of up to 10.9 ± 0.7 GPa and provides excellent weight-normalized shielding efficiency. Simultaneously, it is capable of enduring 100,000 repetitions of folding without experiencing any damage to its construction or fluctuations in conductivity. Furthermore, high-strength scalable MXCS sheets can be produced using doctor blade casting, commercial resin bonding, and aerogel calendering methods, without compromising their performance. This has significant scientific and practical application potential.

Characterization of defect microstructure in MgRE (RE=Ce, Nd) alloys after processing by high-pressure torsion using positron annihilation spectroscopy and a high resolution X-ray diffraction

Two MgRE (RE = Ce, Nd) alloys with ultrafine-grain (UFG) microstructures were prepared by high-pressure torsion (HPT) at room temperature. The in-depth distribution of defects was characterized by Doppler broadening –variable energy positron annihilation spectroscopy (DB-VEPAS). The characteristic S parameter increases in bulk after HPT processing relative to an as-received sample and shows a relative stability between ½ and 10 turns, which suggests a rise in the open volume defect density. However, a theoretical analysis of the S(E) depth profile reveals an increase in the positron diffusion length from ∼115 nm for the as-received state to ∼207 nm after 10 HPT turns. Almost all the open volume defect consisted of dislocations (positron lifetime of τ = 260 ps). The dislocation density deduced from high-resolution X-ray diffraction in the HPT disc radial direction was reasonably homogeneous (around 4–6 × 1014 m−2).

(Invited) Application of Synchrotron X-Ray Topography Techniques to the Analysis of Defect Microstructures in Bulk GaN Substrates and Epilayers for Power Devices

The study of defects and strain in GaN substrates and epilayers for vertical device development using synchrotron X-ray topography techniques is presented. Synchrotron monochromatic beam X-ray topography (SMBXT) studies show that ammonothermal-grown GaN substrate wafers have the lowest dislocation densities while patterned hydride vapor phase epitaxy (HVPE) GaN reveal a starkly heterogeneous distribution of dislocations with large areas containing low threading dislocation densities and HVPE GaN substrates contain high dislocation densities. Epitaxial growth does not nucleate new defects but interactions of dislocations with point defects can cause changes in dislocation configurations. Rocking curve Analysis by Dynamical Simulation (RADS) is shown to be effective in analysis of implantation by correlating the depth profile of strain with the doping profile. Removal of lattice damage induced by implantation requires annealing with proper capping or under high pressures to limit loss of material and lattice distortion. Inductively coupled plasma (ICP) etching may introduce strain in GaN material that can be partially recovered by TBCl etching. Diffusion doping does not introduce new strains in GaN material while neutron transmutation doping at low levels can lead to curing of defects while higher levels lead to irradiation damage and nucleation of new defects.

Defect microstructure of a Ti64 alloy under TI2+ ion irradiation. Influence of dose and temperature

The present paper focuses on the microstructural changes in Ti64 alloy after irradiation. The titanium alloys allow a significant decrease in activation and mass with a similar mechanical strength and a similar corrosion resistance than 304 stainless steels, widely used for core internal structures of Pressurized Water Reactors. The use of titanium alloys could be therefore a significant improvement for reactor exploitation and decommissioning. The nature, size and density of the radiation-induced defects are likely to be important parameters governing the in-reactor behavior of the material. The aim of the study was to devise new achievements in thin foil preparation and Transmission Electron Microscopy (TEM) imaging in order to accurately identify and quantify the Ti64 irradiation defects, at temperatures representative of irradiation temperatures in a reactor. The method to image and count the precipitates was developed with samples irradiated by ions at the temperature of 600 °C. Indeed, the microstructure of the sample irradiated at 600 °C was characterized by a low density of tangled dislocations, and big precipitates, that were easily evidenced. Then the process was applied in samples irradiated with ions at 430 °C and 300 °C characterized by a microstructure of tangled dislocations, loops and small precipitates. In 430 °C irradiation condition, the measurement in dark field with a B∼[11–23]α orientation and with a high magnification micrograph provided similar results than Atom Probe Tomography (APT) analyses. In irradiation condition at 300 °C, the precipitates were imaged by TEM as soon as the dose of 1 dpa. However they were not observed at the dose of 0.4 dpa. The precipitates were so small and their density was so high that the measurement by TEM was very imprecise and APT analyses were needed. The results of this microstructural analysis allowed a discussion on the nucleation mechanism of the irradiation defects in Ti64 alloy.