Local Microstructure Research Articles

Nondestructive Single-Atom-Thick Crystallographic Scanner via Sticky-Note-Like van der Waals Assembling-Disassembling.

Crystallographic characteristics, including grain boundaries and crystallographic orientation of each grain, are crucial in defining the properties of two-dimensional materials (2DMs). To date, local microstructure analysis of 2DMs, which requires destructive and complex processes, is primarily used to identify unknown 2DM specimens, hindering the subsequent use of characterized samples. Here, a nondestructive large-area 2D crystallographic analytical method through sticky-note-like van der Waals (vdW) assembling-disassembling is presented. By the vdW assembling of veiled polycrystalline graphene (PCG) with a single-atom-thick single-crystalline graphene filter (SCG-filter), detailed crystallographic information of each grain in PCGs is visualized through a 2D Raman signal scan, which relies on the interlayer twist angle. The scanned PCGs are seamlessly separated from the SCG-filter using vdW disassembling, preserving their original condition. The remaining SCG-filter is then reused for additional crystallographic scans of other PCGs. It is believed that the methods can pave the way for advances in the crystallographic analysis of single-atom-thick materials, offering huge implications for the applications of 2DMs.

Revealing Crack Propagation and Mechanical Behavior of Corroded Aluminum Alloys

The mechanical properties and crack propagation behavior of aluminum alloys, both with and without corroded surfaces, were thoroughly investigated through molecular dynamic (MD) simulations. The study delved into the effects of corrosion depth and width on the mechanical properties of corroded aluminum alloys. It was found that as the corrosion depth increases, the yield strength experiences an initial decrease followed by a subsequent increase. This can be attributed to the impact of increased corrosion depth on the healing of surface roughness, which ultimately leads to significant changes in yield strength. Furthermore, the presence of corrosion pits was identified as a key factor in regulating the local microstructure evolution within the material, leading to pronounced differences in stress distribution localization. This, in turn, influenced the path of crack propagation within the material. These findings not only contribute to a deeper understanding of the behavior of aluminum alloys under corrosion, but also provide valuable insights for the development of aluminum alloys with enhanced mechanical properties.

A novel approach to texture recognition combining deep learning orthogonal convolution with regional input features.

Textures provide a powerful segmentation and object detection cue. Recent research has shown that deep convolutional nets like Visual Geometry Group (VGG) and ResNet perform well in non-stationary texture datasets. Non-stationary textures have local structures that change from one region of the image to the other. This is consistent with the view that deep convolutional networks are good at detecting local microstructures disguised as textures. However, stationary textures are textures that have statistical properties that are constant or slow varying over the entire region are not well detected by deep convolutional networks. This research demonstrates that simple seven-layer convolutional networks can obtain better results than deep networks using a novel convolutional technique called orthogonal convolution with pre-calculated regional features using grey level co-occurrence matrix. We obtained an average of 8.5% improvement in accuracy in texture recognition on the Outex dataset over GoogleNet, ResNet, VGG and AlexNet.

Perspective: Theory and simulation of highly mismatched semiconductor alloys using the tight-binding method

The electronic structure of highly mismatched semiconductor alloys is characterized by carrier localization and strongly influenced by the local alloy microstructure. First-principles calculations can deliver valuable quantitative insight, but their associated computational expense limits alloy supercell size and imposes artificial long-range ordering, which can produce misleading results. The empirical tight-binding method (ETBM) provides a transparent approach to investigate large-scale supercells on an atomistic level, to quantitatively predict the electronic structure of semiconductor alloys. Here, we overview key aspects and considerations for establishing ETBMs. Additionally, we discuss and highlight, given that the ETBM matrix elements are described in the language of overlaps between localized atomic orbitals, that ETBMs have proven highly successful in analyzing the impact of localized and resonant impurity states, as well as disorder, on the optoelectronic properties of highly mismatched alloys. The ETBM continues to provide valuable insight for emerging material systems, including two-dimensional materials, perovskites and their heterostructures, and provides a framework to address technologically relevant questions including the importance of short-range disorder for loss mechanisms such as non-radiative Auger–Meitner recombination. Moreover, the ETBM furnishes a quantitative basis for continuum models such as k⋅p or localization landscape theories, allowing to explicitly incorporate disorder effects in nanostructures to underpin predictive device-level analysis.

Thermal cracking: Clarifying the effects of phases, voids and grains through characterisation and crystal plasticity modelling

Thermally-induced cracking typically occurs during the cooling stage of various manufacturing processes, and is commonly seen in multiphase or the joints of dissimilar materials due to mismatch in their thermo-mechanical properties, such as thermal expansion, elastic-plastic deformation and, in some cases, phase transformation. However, the underlying cracking mechanism associated with local microstructure is still elusive. To improve the mechanistic understanding of thermal cracking, this work uses the diffusion-bonded 9Cr-1Mo steel as an example to study the key microstructural variables, such as interfacial phases, voids, grain boundary migration and crystallographic orientations. Meanwhile, a temperature-dependent crystal plasticity model coupled with a cohesive zone model is developed to provide more insights into the thermal-induced stress distribution at the grain scale. It is found that the stress at the void-free boundary of martensite and ferrite is dominated by shear, and its magnitude is insufficient to nucleate cracks. Whereas voids at phase boundaries can induce significant tensile stress, resulting in cracking at the phase boundaries as well as diffusion-bonded interfaces. Also, the occurrence of interfacial grain boundary migration plays an important role in local stress distribution. These microstructure features and their evolution are experimentally observed and used to verify the developed crystal plasticity models. These findings enhance the understanding of the influence of microstructure features on thermal cracking and provide a guide to designing and fabricating the microstructure with improved thermal crack resistance in various manufacturing processes.

Microstructure manipulation via machining and heat treatments in hybrid manufacturing of 316L stainless steel

Hybrid manufacturing combines additive and subtractive (machining) processes in a single platform to reduce the total time to fabricate a component in its final form. Here we show that if sufficient plastic deformation can be imparted to the material during machining, recrystallization can be triggered during post-fabrication heat treatment. This can enable highly localized microstructure control. We show that stainless steel 316L, when machined without coolant accumulates significant plastic strain compared to when machined with coolant that results in faster recrystallization kinetics during heat treatment. These effects are limited to the surface while the bulk microstructure remains unaffected.

Thermal cycling effects on the local microstructure and mechanical properties in wire-based directed energy deposition of nickel-based superalloy

In additive manufacturing, intrinsic heat treatments take place during deposition that affect the properties of AM-structures. In this work, the influence of thermal cycling on the local microstructure and mechanical properties of nickel-based superalloy in wire-based electron beam directed energy deposition (EB-DED) was investigated. Structures were fabricated using a continuous deposition strategy (CDS) and discontinuous interpass cooling strategy (ICS) revealing changes in thermal profiles, time-temperature history, and microstructure. An altered morphology along the build-up height and interdendritic zones enriched in Nb are formed. Nb and Mo did not show a clear trend of segregation along the build-up height. Lower fractions of the Laves phase and MCs are found for both configurations. Differences between deposition strategies and locations within AM-structures are found for the γ" and δ phase. The higher Nb content in the interdendritic zone promotes the precipitation of γ" and δ phase by shortening the aging times compared to wrought materials. The longer deposition times of ICS favour the precipitation of fine γ" in the interdendritic zone throughout the deposition height. In contrast, the short deposition time of CDS leads to an increase in temperature and a heterogeneous distribution of γ" along the height, i.e. coarsening of the γ" followed by a dissolution along the built-up height. The microstructural changes correlate with the mechanical properties. Structures fabricated with ICS exhibit homogeneous mechanical properties throughout, while the graded microstructure of CDS results in graded mechanical properties and decreasing strength throughout.

Microstructural smoothed particle hydrodynamics model and simulations of discontinuous shear-thickening fluids

Despite the recent interest in the discontinuous shear-thickening (DST) behavior, few computational works tackle the rich hydrodynamics of these fluids. In this work, we present the first implementation of a microstructural DST model in smoothed particle hydrodynamic (SPH) simulation. The scalar model was implemented in an SPH scheme and tested in two flow geometries. Three distinct ratios of local to non-local microstructural effects were probed: zero, moderate, and strong non-locality. Strong and moderate cases yielded excellent agreement with flow curves constructed via the Wyart–Cates (WC) model, with the moderate case exhibiting banding patterns. We demonstrate that a local model is prone to a stress-splitting instability, resulting in discontinuous stress fields and poor agreement with the WC model. The mechanism of stress splitting has been explored and contextualized by the interaction of local microstructure evolution and the stress-control scheme. Analytic solutions for a body-force-driven DST channel flow have been derived and used to validate the SPH simulations with excellent agreement in velocity profiles. Simulations carried out at increasing driving forces exhibited a decrease in flow. We showed that even the simple scalar model can capture some of the key properties of DST materials, laying the foundation for further SPH study of instabilities and pattern formation.

A Methodology for the Rapid Qualification of Additively Manufactured Materials Based on Pore Defect Structures

Additive manufacturing (AM) can create net or near-net-shaped components while simultaneously building the material microstructure, therefore closely coupling forming the material and shaping the part in contrast to traditional manufacturing with distinction between the two processes. While there are well-heralded benefits to AM, the widespread adoption of AM in fatigue-limited applications is hindered by defects such as porosity resulting from off-nominal process conditions. The vast number of AM process parameters and conditions make it challenging to capture variability in porosity that drives fatigue design allowables during qualification. Furthermore, geometric features such as overhangs and thin walls influence local heat conductivity and thereby impact local defects and microstructure. Consequently, qualifying AM material within parts in terms of material properties is not always a straightforward task. This article presents an approach for rapid qualification of AM fatigue-limited parts and includes three main aspects: (1) seeding pore defects of specific size, distribution, and morphology into AM specimens, (2) combining non-destructive and destructive techniques for material characterization and mechanical fatigue testing, and (3) conducting microstructure-based simulations of fatigue behavior resulting from specific pore defect and microstructure combinations. The proposed approach enables simulated data to be generated to validate and/or augment experimental fatigue data sets with the intent to reduce the number of tests needed and promote a more rapid route to AM material qualification. Additionally, this work suggests a closer coupling between material qualification and part certification for determining material properties at distinct regions within an AM part.

Non-synchronous deformation under shot peening post-treatment of SUS304 bar-plate rotary friction weld generates non-monotonic evolution on material and fatigue property

Shot peening post-treatment was conducted at SUS304 austenite steel bar-plate rotary friction welding joint with fatigue property deterioration from welding flash. along the shotting intensity increasing, non-synchronous deformation of the plate and flash resulted in non-monotonically evolution of local microstructure, residual stresses, and make the fatigue life increased to flash-removed joint level.

Strain-life behavior of thick-walled nodular cast iron

Abstract For the design of thick-walled cast iron components used for wind energy turbines, large machines, presses, and engine parts made of nodular cast iron, the assessment of fatigue life of critical component areas is a crucial point to consider. Importance increases with the demand to safe resources by applying a lightweight design in combination with a certain resistance against extreme loads and misuse situations. Moreover, this gets more important when notches or deviations in the local microstructure are present. Nevertheless, due to accessibility, a lack in the description of the local strain-based material behavior still exists. Especially new cast iron grades such as ADI are not well investigated but offer an often-discussed potential for a lightweight design of the structure or to increase the highest admissible load on the structure. To determine the cyclic material behavior of nodular cast iron, different grades EN-GJS-400-18LT, EN-GJS-450-18, EN-GJS-500-14, EN-GJS-600-3, EN-GJS-700-2, and ADI in different wall thicknesses were investigated concerning their elastic–plastic material behavior under strain control. Moreover, new possibilities for the trilinear description of the strain-life and the stress–strain curve and the statistical and technological size effect are discussed in the following based on cyclic stress–strain and strain-life curves.

Prediction of the Secondary Arms Spacing Based on Dendrite Tip Kinetics and Cooling Rate.

Secondary dendrite arm spacing (SDAS) is one of the most important factors affecting macrosegregation and mechanical properties in solidification processes. Predicting SDAS is one of the major parameters in foundry technology. In order to predict the evolution of microstructures during the solidification process, we proposed a simple model which predicted the secondary dendrite arm spacing based solely on the tip velocity (related to the tip supersaturation) and cooling rate. The model consisted of a growing cylinder inside a liquid cylindrical envelope. Two important hypotheses were made: (1) Initially the cylinder radius was assumed to equal the dendrite tip radius and (2) the cylindrical envelope had a fixed radius in the order of the dendrite tip diffusion length. The numerical model was tested against experiments using various Pb-Sn alloys for a fixed temperature gradient. The results were found to be in excellent agreement with experimental measurements in terms of SDAS and dendrite tip velocity prediction. This simple model is naturally destined to be implemented as a sub-grid model in volume-averaging models to predict the local microstructure, which in turn directly controls the mushy zone permeability and macrosegregation phenomena.

A study of local microstructure decay in GCr15 due to rolling contact

This study investigated the microstructural alteration of GCr15 bearing steel under Rolling Contact condition. It was found that Decay Region, a feature microstructure, formed in the subsurface of materials with the dominant effect of cyclic contact stress. The Decay Region is composed of discretely distributed micro-regions where phase transition occurred, presenting a hollow crescent shape. The microstructure after phase transformation was highly susceptible to corrosion by Nital solution. The formation of Decay Region was related to the orthogonal shear stress and there was an upper threshold. Excessively high stress suppressed the appearance of Decay Region. During Rolling Contact, the hardness of materials evolved simultaneously. The evolution of hardness and microstructure exhibited a parallel development, as the dominant stresses were different.

Assessment of the nano-mechanical properties of healthy and atherosclerotic coronary arteries by atomic force microscopy.

Nano-indentation techniques might be better equipped to assess the heterogeneous material properties of plaques than macroscopic methods but there are no bespoke protocols for this kind of material testing for coronary arteries. Therefore, we developed a measurement protocol to extract mechanical properties from healthy and atherosclerotic coronary artery tissue sections. Young's modulus was derived from force-indentation data. Metrics of collagen fibre density were extracted from the same tissue, and the local material properties were co-registered to the local collagen microstructure with a robust framework. The locations of the indentation were retrospectively classified by histological category (healthy, plaque, lipid-rich, fibrous cap) according to Picrosirius Red stain and adjacent Hematoxylin & Eosin and Oil-Red-O stains. Plaque tissue was softer (p < 0.001) than the healthy coronary wall. Areas rich in collagen within the plaque (fibrous cap) were significantly (p < 0.001) stiffer than areas poor in collagen/lipid-rich, but less than half as stiff as the healthy coronary media. Young's moduli correlated (Pearson's ρ = 0.53, p < 0.05) with collagen content. Atomic force microscopy (AFM) is capable of detecting tissue stiffness changes related to collagen density in healthy and diseased cardiovascular tissue. Mechanical characterization of atherosclerotic plaques with nano-indentation techniques could refine constitutive models for computational modelling.

Microstructure Evolution during High-Pressure Torsion in a 7xxx AlZnMgZr Alloy.

A homogenized, supersaturated AlZnMgZr alloy was processed via severe plastic deformation (SPD) using a high-pressure torsion (HPT) technique for different revolutions at room temperature to obtain an ultrafine-grained (UFG) microstructure. The microstructure and mechanical properties of the UFG samples were then studied using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and tensile and hardness measurements. The main purpose was to study the effect of shear strain on the evolution of the microstructure of the investigated alloy. We found a very interesting evolution of the decomposed microstructure in a wide range of shear strains imposed by HPT. While the global properties, such as the average grain size (~200 nm) and hardness (~2200 MPa) appeared unchanged, the local microstructure was continuously transformed. After 1 turn of HPT, the decomposed UFG structure contained relatively large precipitates inside grains. In the sample processed by five turns in HPT, the segregation of Zn atoms into grain boundaries (GBs) was also observed. After 10 turns, more Zn atoms were segregated into GBs and only smaller-sized precipitates were observed inside grains. The intensive solute segregations into GBs may significantly affect the ductility of the material, leading to its ultralow-temperature superplasticity. Our findings pave the way for achieving advanced microstructural and mechanical properties in nanostructured metals and alloys by engineering their precipitation and segregation by means of applying different HPT regimes.

An efficient method for multiscale modelling of the mechanical properties of additively manufactured parts with site-specific microstructures

The ability to modulate microstructures at different locations within a part (i.e., site-specific microstructures) can lead to tailored properties and enhanced performance. However, it remains challenging to efficiently model the mechanical response of such materials due to the need for extensive multiscale analysis. To address this issue, we demonstrate through microstructure-based finite element simulations, that the mechanical properties of a randomly distributed two-phase microstructure are primarily dependent on the phase fraction. Therefore, by establishing a mathematical relationship between the phase fraction and mechanical properties, the local material properties can be efficiently calculated from the local microstructure. Later, these site-specific properties were incorporated into a finite element structure to predict the global mechanical properties of the sample part. To validate the effectiveness of the proposed method, low alloy steel with site-specific microstructures was fabricated using binder jet additive manufacturing by depositing varying concentrations of carbon binder at different locations inside the part. We observed a strong agreement between the experimental and simulation stress-strain responses of the steel samples. This method can potentially pave the way for the development of a non-destructive qualification method for additively manufactured parts, as well as provide an efficient approach to multiscale modeling of material behavior, which may help accelerate the design and innovation of novel material systems.

Quantitative analysis of three‐dimensional fatigue crack path selection in Mg alloy WE43 using high‐energy X‐ray diffraction microscopy

AbstractFatigue short‐cracks in Mg alloys display complex growth behavior due to high plastic anisotropy and crack path dependence on local microstructural features. In this study, the three‐dimensional crystallography of short‐crack paths in Mg alloy WE43 was characterized by mapping near‐field high‐energy X‐ray diffraction microscopy (HEDM) reconstructed grain maps to high‐resolution X‐ray CT reconstructions of the fracture surfaces in the crack initiation and short‐crack growth regions of six ultrasonic fatigue specimens. Crack–grain–boundary intersections were analyzed at 81 locations across the six crack paths. The basal intragranular, non‐basal intragranular, or intergranular character of short‐crack growth following each boundary intersection was correlated to crystallographic and geometric parameters of the trailing and leading grains, three‐dimensional grain boundary plane, and advancing crack front. The results indicate that crack paths are dependent on the combined crystallographic and geometric character of the local microstructure, and crack path prediction can be improved by use of dimensionality reduction on subsets of high‐linear‐correlation microstructural parameters.

Substrate interaction mediated control of phase separation in FIB milled Ag–Cu thin films

Nanofabrication is an integral part of the realization of advanced functional devices ranging from optical displays to memory devices. Focused-ion beam (FIB) milling is one of the most widely used nanofabrication methods. Conventionally, FIB milling has been carried out for patterning single-phase stable thin films. However, the influence of FIB milling on the phase separation of metastable alloy films during subsequent treatments has not been reported. Here, we show how FIB milling of Ag–Cu thin films influences the separation process and microstructure formation during post-milling annealing. The phase-separated microstructure of the film consists of fine, randomly distributed Ag-rich and Cu-rich domains, whereas adjacent to milled apertures (cylindrical holes), we observe two distinctly coarser rings. A combination of imaging and analysis techniques reveals Cu-rich islands dispersed in Ag-rich domains in the first ring next to the aperture, while the second ring constitutes mostly of Ag-rich grains. Copper silicide is observed to form in and around apertures through reaction with the Si-substrate. This substrate interaction, in addition to known variables like composition, temperature, and capillarity, appears to be a key element in drastically changing the local microstructure around apertures. Thus, the current study introduces new avenues to locally modulate the composition and microstructure through an appropriate choice of the film-substrate system. Such an ability can be exploited further to tune device functionalities for possible applications in plasmonics, catalysis, microelectronics, and magnetics.

Linking local microstructure to fracture location in a two-dimensional amorphous solid under isotropic strain.

Brittle fracturing of materials is common in natural and industrial processes over a variety of length scales. Knowledge of individual particle dynamics is vital to obtain deeper insight into the atomistic processes governing crack propagation in such materials, yet it is challenging to obtain these details in experiments. We propose an experimental approach where isotropic dilational strain is applied to a densely packed monolayer of attractive colloidal microspheres, resulting in fracture. Using brightfield microscopy and particle tracking, we examine the microstructural evolution of the monolayer during fracturing. Furthermore, we propose and test a parameter termed Weakness that estimates the likelihood for particles to be on a crack line, based on a quantified representation of the microstructure in combination with a machine learning algorithm. Regions that are more prone to fracture exhibit an increased Weakness value, however the exact location of a crack depends on the nucleation site, which cannot be predicted a priori. An analysis of the microstructural features that most contribute to increased Weakness values suggests that local density is more important than orientational order. Our methodology and results provide a basis for further research on microscopic processes during the fracturing process.

Halogen anions (F−, Cl−, Br−) modulated the localized microstructure of g-C3N4 to facilitate charge separation and transport and enhance photocatalytic activities

A facile surface halide anion (F−, Cl−, Br−) modification strategy was employed to facilitate the charge separation and transport efficiency of g-C3N4, resulting in enhanced photocatalytic performance.