Inhomogeneous Microstructure Research Articles

Electron Backscatter Diffraction Analysis of Low-Misorientation-Angle Boundary and High-Energy Boundary in the Hot-Rolled Plate of Grain-Orientated Silicon Steel

In order to study the texture evolution and the formation of an inhomogeneous microstructure in hot-rolled plate of grain-orientated silicon steel, Fe3C (hexagonal) and ferrite phases in the subsurface layer were studied using electron backscatter diffraction. The results indicate that fiber texture (ferrite) mainly composed of {441}<104> and (110)[001] Goss oriented grains was formed at a depth of 25% of the thickness of hot-rolled plate. Matrix grains in the subsurface layer were arbitrary separated into irregular large grains (≥40 μm) and fine grains (<40 μm), and the grain boundary characteristics and texture evolution of matrix grains were studied. The results indicated that the formation of the colonies of fine grains was the result of dynamic recrystallization, and high-frequency low-misorientation-angle boundaries (0~20°) were formed between large grains (≥40 μm) and fine grains (<40 μm), which can be considered as the irregularity of large grains caused by solid-state wetting. Due to the texture evolution of large grains (≥40 μm), a large number of high-energy boundaries (20~45°) were formed between irregular large grains (≥40 μm), resulting in rapid consumption between adjacent large grains and the elongation of large grains along the rolling direction. Therefore, it can be assumed that the migration of low-misorientation-angle boundaries (0~20°) under solid-state wetting and high-energy boundaries (20~45°) are important mechanisms for non-uniform grain growth in hot-rolled plate of grain-orientated silicon steel.

On the nature of nano twin-induced shear band formation in a dispersion strengthened copper alloy under micro-mechanical loading

A key challenge in metallic alloys with high ductility is understanding how microstructural inhomogeneities influence shear localization, leading to localized plastic deformation and material failure. In this study, we explore the phenomenon of shear localization in coarse-grained copper, a material traditionally regarded as having low susceptibility to such behavior. Contrary to conventional understanding, our findings reveal that microstructural inhomogeneities play a pivotal role in inducing extensive strain localization during low strain rate micro-mechanical loading. The presence of fine precipitate particles leads to strain localization at small strains and low strain rates by activating shear localization driven by void formation mechanisms. Furthermore, nanoscale precipitates act as sites for dislocation pile-up within deformed structures of shear bands, leading to the formation of nano twins within these bands. Consequently, precipitate particles serve a dual role: contributing to strain localization and potential cracking, while also enhancing the alloy’s strength and ductility through nano-twinning mechanisms. This investigation offers a novel perspective on the interplay between material microstructure and deformation behavior, challenging existing paradigms in materials science.

Part-Scale Microstructure Prediction for Laser Powder Bed Fusion Ti-6Al-4V Using a Hybrid Mechanistic and Machine Learning Model

Laser powder bed fusion (LPBF) Ti-6Al-4V is widely studied for use in structural applications in aerospace and medical industries, but mechanical anisotropy and microstructural inhomogeneity prohibits its wider adoption. Although successful microstructure prediction models have been developed, a remaining challenge is their limited integration across length/time scales and validation by experimental studies. This work proposes a physics-augmented machine learning surrogate model to unite predictions of LPBF temperature, β phase morphology and texture, and α/α’ formation into a single framework that is calibrated and validated with experiments. First, a phase field (PF) model of the martensitic β→α’ transformation is developed and calibrated using data from in-situ synchrotron cyclic heating/cooling studies quantifying the variation of α phase fraction with time. In parallel, an established finite difference-Monte Carlo (FDMC) model predicts the part-scale temperature profile and β grain formation during solidification. A dataset is developed using LPBF cyclic temperature descriptors from the FDMC model as inputs and corresponding α/α’ phase fraction and width from the PF model as outputs. Five machine learning (ML) regression models are tested and optimized, having mean absolute error in testing ≤ 4%, and the k-nearest neighbors (KNN) model is selected as the best performing. The KNN model is called at the nodal level during post-processing of the FDMC model to replace and downscale the response of the PF model. The combined agility and accuracy of the hybrid FDMC-ML model enables part-scale microstructure predictions that can be further used for property predictions to accelerate AM process optimization.

Correlation between microstructural inhomogeneity and architectural design in additively manufactured NiTi shape memory alloys

ABSTRACT Additively manufactured Nitinol (NiTi) architectured materials, designed with unit cell architectures, hold promise for customisable applications. However, the common assumption of homogeneity in modeling and additive manufacturing of these architectured materials needs further investigation because geometric-dependent melt pool behaviour results in inhomogeneous microstructure and thermomechanical properties. This study shows that property inhomogeneity at the mesoscale is one reason for pseudo-linear response and partial superelasticity of the fabricated NiTi body-centered cubic (BCC) architectured materials. We modeled using a phenomenological constitutive relation and additively manufactured NiTi architectured materials with varying relative densities. These fabricated samples showed distinct microstructural textures and compositions that affected their local recoverability. The edge effects and laser turn regions were identified as the causes underlying the observed microstructural inhomogeneity. The dimensionless Fourier number is used to describe the transition of printing modes. This study provides valuable information on rigorous experimental/computational consistency in future work.

Variation in microstructural features of melt-pool structure in laser powder bed fused Al–Fe–Cu alloy at elevated temperatures

The present study was undertaken to understand the effect of annealing on the microstructural features of the melt-pool structure and the associated multiscale mechanical properties of the Al–2.5%Fe–2%Cu alloy manufactured by laser powder bed fusion (LPBF). Microstructural characterizations and tensile tests were conducted for the LPBF-built specimen and those subsequently annealed at various temperatures ranging from 200 to 500 °C. Nanoindentation hardness mapping was used to evaluate the mechanical inhomogeneity of the melt-pool structure and its changes by annealing at different temperatures. The LPBF-manufactured sample exhibited a melt-pool structure containing numerous particles of the Al23CuFe4 phase (oC28, orthorhombic structure) formed because of local melting and rapid solidification during the LPBF process. The relatively coarsened cellular structure localized along the melt-pool boundary resulted in local soft regions. The local vulnerability contributed to the direction dependence of the tensile ductility. A slight variation was observed in the inhomogeneous microstructure of the samples annealed at 200 or 300 °C. The formation of numerous Al23CuFe4 nanoprecipitates in the α-Al supersaturated solid solution prevented strength loss after post-heat treatments. In addition, considerable coarsening of the intermetallic phase after annealing at 500 °C eliminated the melt-pool structure. The tensile performance of the specimens demonstrated a ductile fracture mode, wherein ductile fracture occurred in the α-Al matrix with low hardness while the harder θ-Al13Fe4 stable phase was embedded within it. The anisotropy in the mechanical properties was less pronounced owing to the significant microstructural changes.

Ultrasonic vibration assisted directed energy deposition of titanium alloy: Microstructure control, strengthening mechanisms and fatigue crack behavior

Large-scale titanium alloy structural components fabricated using direct energy deposition (DED) technology have broad application prospects. However, the columnar grain structures and inhomogeneous microstructure due to the inherent characteristics of additive manufacturing seriously affects the mechanical properties of components. In this study, high-intensity ultrasound vibration was introduced into the wire-arc DED deposition of TC4-DT titanium alloy. The results showed that ultrasonic vibration assistance (UVA) significantly improves the grain structure (refine prior-β grain size and weaken α texture) of the as-deposited component, without introducing additional porosity. Compared to conventional wire-arc DED deposited components, the yield strength and tensile strength of UVA alloys increased by 22.23 % and 15.06 %, respectively. Furthermore, the difference in α grain structure caused by UVA results in different fatigue crack growth behaviors. The disorder orientation of the α laths enhanced the fatigue crack initiation resistance of the wire-arc DED component with UVA. This study shows the excellent mechanical properties of UVA DED fabricated TC4-DT alloy, paving the way for the design, fabrication, and application of large structural components of titanium alloys.

Influence of aloe-vera powder addition on microstructure and mechanical properties of wire + arc additively manufactured ER70S-6 steel

ER70S-6 steel Wire Arc Additive Manufactured deposit was fabricated using Gas Tungsten Arc Welding (GTAW) under two conditions: without and with aloe-vera powder. Aloe-vera is added at the interlayer during deposition. The effect on microstructure evolution, hardness and tensile properties due to addition of aloe-vera were investigated. Without aloe-vera deposits recorded non-uniform microstructure from lower to upper zone, resulting in wide variation in hardness. On the other hand, presence of aloe-vera minimized the microstructural inhomogeneities. The presence of aloe-vera also suppressed the formation of bainite phase and stabilize the hardness throughout the deposit. The tensile strength of the aloe-vera added deposit also increases compared to without powder particle deposit.

Achieving efficient hardfacing on stainless steel using single SiC powder in laser directed energy deposition

Generally, in a laser hardfacing process, a mixture of ceramic and metal powder is used to clad a hard surface, resulting in enhanced wear characteristics of metal parts. This study proposes an efficient hardfacing process that uses a single and minimal amount of ceramic powder (0.079 g/min in this work). This process, named as Laser Directed Energy Deposition of Minimal Ceramic Powder (LDED-MCP), features that the melt pool is generated inwardly because only the substrate participates in forming the melt pool. Furthermore, due to the minimal powder flow rate used and sparse particle-melt pool collision events, ripple formations leading to the convective melt pool flow and inhomogeneous microstructures would be suppressed. Consequently, the produced layer is nearly flat and free of incompletely melted metallic particles, thus minimizing post-machining. For a 316 L substrate and SiC powder material combination, a crack-free layer about 560 μm thick with an average hardness of about 417 HV was created through process parameter optimization. This layer showed a eutectic structure composed of γ-austenite and chromium carbides, partially melted SiC particles between dendrites, and in-situ synthesized SiC nanoparticles decorating the cell walls. Through this work, near-net-shape hardfacing of stainless steels is realized through LDED-MCP process minimizing powder pre-processing and post surface machining.

Coordinated deformation characteristics and its effect on microstructure evolution of LA103Z Mg-Li alloy in reciprocating rotary extrusion

The uneven metal flow and inhomogeneous microstructure on the cross-section of the extruded bar are mainly induced by the uncoordinated deformation during the traditional extrusion process, which seriously restricts its production and application. These defects are more prominent for the dual-phase Mg-Li alloy due to the phase transformation and the difference in flow between soft and hard phases. In order to solve the uncoordinated deformation in traditional extrusion, the reciprocating rotary extrusion (R-RE) process based on harmonic oscillation of die is proposed. The experiment and numerical simulations of the reciprocating rotary extrusion process were carried out at rotating frequency of 2.5 and 5 Hz, extrusion velocity of 1 mm/s, forming temperature of 290℃, die extrusion ratio of 12 and die rotating angle of ±6°. The coordinated deformation mechanism from macroscopical flow and microstructure in reciprocating rotary extrusion was investigated deeply. Meanwhile, a novel theoretical method was proposed to describe coordinate deformation characteristics quantitatively. The results indicated that the reciprocating rotary extrusion significantly reduces the forming load and accumulates more strain. The more uniform metal flow contributes to coordinated deformation. The extrusion deformation factors are proposed to reveal the coordinated deformation mechanism. In addition, the deformation body characteristic zone is novelly divided into six zones by combination of flow pattern and microstructure evolution.

Inhomogeneous deformation in melt-pool structure of Al-Fe-Cu alloy manufactured by laser powder bed fusion

Abstract The laser powder bed fusion (L-PBF) processed Al–2.5Fe–2Cu (mass%) alloy exhibited a high tensile strength above 340 MPa and pronounced directional dependence. The sample exhibited a characteristic inhomogeneous microstructure (in melt-pool structure) arising from the local melting and rapid solidification in the L-PBF process. The coarsened cellular structure localized along the melt pool boundary resulted in the local soft regions affected by the melt pool structure. The local vulnerability contributed to the direction dependence of the tensile ductility of the specimen.

Accelerated functional fatigue leading to hysteresis widening in Ti44Ni47Nb9 shape memory alloy with multi-scale Nb-rich particles

Martensitic transformation temperatures are the most important indicators for designing shape memory alloy (SMA) components. Subjected to alternating temperatures in service, they undergo functional fatigue, which affects little the thermal hysteresis. We investigate the thermal cycling induced functional fatigue in Ti44Ni47Nb9 wide hysteresis SMA, decorated with multi-scale Nb-rich particles. We identify an accelerated functional fatigue behavior leading to the hysteresis widening from 58 to 71 K after 20 thermal cycles, in contrast to which hysteresis maintains nearly constant in Ti-Ni binary SMAs. Compared to Ti49Ni51 with similar transformation temperatures and latent heats, the hysteresis widening in Ti44Ni47Nb9 is attributed to accelerated decrease in starting temperature of martensite transformation (Ms).Microscopic characterizations reveal an inhomogeneous microstructure, consisting of (Ti,Nb)Ni B2 matrix and multi-scale Nb-rich particles and (Ti,Nb)2Ni particles. The presence of unique multi-scale Nb-rich particles has been demonstrated at the core of the underlying mechanisms of accelerated functional fatigue. Densely distributed Nb-rich nanoparticles narrow the mean matrix distance of transformation to 156.3 nm, which restricts the size and cross-over of the transformation induced dislocation leaves. Our work provides a new mechanism to widen the thermal hysteresis of SMAs, which is probably applicable to the other SMAs systems with dense nanoparticles.

On comparison of fracture toughness of irradiated and thermally aged decommissioned nuclear weld metals with miniature specimen test technique

This paper investigates the fracture toughness of thermally aged and irradiated weld metals extracted from head and beltline regions of a decommissioned nuclear reactor pressure vessel. Miniature compact tension specimens are fabricated from the thermally aged reactor pressure vessel head weld as well from the circumferential and axial beltline welds having fluences of 2.90 × 1016n/cm2 and 7.94 × 1017n/cm2, respectively. Master curve approach in accordance with the ASTM E1921 is applied to determine the reference temperature T0 and it is found to be − 113.5 °C, −104.4 °C, and − 89.3 °C for the reactor pressure vessel head, axial beltline, and circumferential beltline welds, respectively. In addition, the multimodal reference temperature Tm to assess the homogeneity of welds as well as key curve analysis for the quality assurance of testing are also provided. Fractographic analysis identified variations in crack initiation sites and microstructural inhomogeneities, particularly in the irradiated beltline welds. Overall, fracture mechanical testing of the materials demonstrated that miniature compact tension specimens are effective for characterizing the fracture toughness of limited surveillance weld materials, revealing differences due to irradiation and weld location.

Homogenization Treatment and Plastic Deformation Improve the Carbide Homogeneity of M42 High‐Speed Steel

The mechanical properties of high‐speed steel (HSS) are significantly influenced by the distribution of carbides formed during solidification. Despite extensive research, the nonuniform cooling in large ingots remains an area requiring further investigation. In this study, the microstructure inhomogeneity in M42 HSS with a diameter of 330 mm is examined. Models are developed to predict the dissolution of carbide networks during homogenization, achieving a 39% reduction in hardness variation (Δr) between the center and surface. Further improvements are attained through hot forging and rolling, leading to the fragmentation of the carbide network into a banded structure. Additionally, a detailed carbide tip dissolution model is established, providing a reliable basis for optimizing annealing processes. As a result, the carbide distribution converges significantly, with hardness variations reduced by 88% to only 0.3 hardness Rockwell C scale, showcasing substantial enhancement in material homogeneity.

Micro-milling machinability prediction for crystalline materials via numerical-analytical hybrid modelling and strain rate-dependent grain-scale simulation

Micro-milling is a promising technology to produce miniature-sized components, while the machinability prediction of crystalline material micro-milling is difficult due to the inhomogeneous microstructure, anisotropic properties, nonlinear strain rate sensitivity and complex process characteristics. To achieve accurate and effective micro-milling machinability prediction of crystalline materials, this paper proposes a numerical-analytical hybrid method that comprehensively and simultaneously considers core material and process characteristics of the crystalline material micro-milling technique, which evaluates micro-milling forces and surface roughness via a series of adaptive strain rate-dependent micro-orthogonal cutting emulations in grain-scale and a set of analytical transformations. Taking Inconel-718 as the sample material, grain-scale mechanical parameters under 10−2–104 s−1 strain rate range were calibrated. Strain rate effect-considered grain-scale constitutive theory is proposed and strain rate-dependent micro-orthogonal cutting emulations were executed, which were experimentally verified to be accurate and robust on the forces and surface roughness prediction of micro-cutting. Furthermore, numerical-analytical hybrid modelling and machinability prediction of Incoenl-718 micro-milling process under 12 mm/min and 20 mm/min feed rates were carried out, the relative prediction errors of micro-milling forces and surface roughness are <15 % and 14 %, which confirm that the proposed hybrid method is accurate and robust on the micro-milling machinability prediction of crystalline materials.

Insights into Nb-silicide-based in-situ composite processed by electron beam powder bed fusion

This is the first report introducing the idea of processing Nb-silicide-based in-situ composite through electron beam powder bed fusion (PBF-EB). A high energy input together with a line order strategy resulted in cracking, whilst a lower energy input without the line order led to microstructural inhomogeneity characterised by alternating dark- and bright-contrast bands. In samples printed using the line order strategy, long cracks initiated close to the melt pool boundary and propagated into the previous layer. These cracks were due to the weak interface between the primary Nb3Si columnar grains and the equiaxed (Nb,Ti) solid solution phase or Nb3Si-(Nb,Ti) solid solution eutectic structure. The porosity level increased from 0.122 % to 0.547 % with the increase of area average energy input from 2.22 J/mm2 to 6.67 J/mm2. The density decreased to 6.80 g/cm³ in the line order strategy samples due to the presence of cracks, compared to 6.84 g/cm³ in samples without employing the line order strategy. The dark-contrast band consisted of (Nb,Ti) solid solution, Nb3Si and Nb5Si3, while the bright-contrast band was composed of (Nb,Ti) solid solution and Nb3Si. Within the bright-contrast band, a recurring layered microstructural inhomogeneity appeared, with columnar grains at the bottom, whilst fine- and coarse-grained eutectic networks in the middle and upper regions. The Nb3Si phase exhibited a pronounced {001} texture, whereas the (Nb,Ti) solid solution phase displayed a weaker texture. The Nb-silicide-based in-situ composite fabricated through PBF-EB had a microhardness of ∼700 HV0.5. This value is higher than that achieved through conventional means but falls within the mid-range for laser-based additive manufacturing counterparts.

Fabrication of AA3303 aluminum alloy by powder metallurgy techniques consolidated by sintering

This work analyzes the manufacture of the AA3303 aluminum alloy by powder metallurgy (PM) technique, using the uniaxial cold compaction and solid phase sintering route. The process will start with the AA3303 alloy powder manufactured by high-energy ball milling (HEBM), which will be compacted and then sintered, thus manufacturing a dense solid. This study aims to validate the PM manufacturing technique as an alternative in the production of the alloy studied. The manufactured alloy was characterized using optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and Vickers hardness (HV) tests. The characterization of the manufactured material showed marked porosity, low densification and an inhomogeneous microstructure, but acceptable hardness values were obtained for the alloy under study.

Toward developing remanufactured Ti6Al4V alloys with high fatigue crack growth resistance by in-situ cooling during laser remanufacturing

The fatigue performance of remanufactured titanium alloy blade components has garnered significant attention in recent years. The repaired titanium alloy components using the direct energy deposition (DED) method exhibit structural differences, leading to an inhomogeneous microstructure that directly impacts the service life of the remanufactured component. The work presented here aimed to investigate novel approaches for enhancing the resistance to crack propagation and to gain a deeper insight into the fatigue crack propagation characteristics of the Ti6Al4V remanufactured interface with an inhomogeneous microstructure. The research focused on analyzing the microstructure evolution and fracture properties of remanufactured components using in-situ cooling. The results indicate that in-situ cooling has the potential to decrease the anisotropy of the repaired zone (RZ) and enhance the resistance to crack propagation in the heat-affected zone (HAZ) and base metal (BM). The high cooling rate associated with the in-situ cooling can elevate the presence of high-angle grain boundaries (HAGBs) in the RZ, diminish the phase transformation between the HAZ and BM, and decrease the size of the secondary α phase. The research contributes to a deeper comprehension of fatigue crack propagation in remanufactured components and provides a pathway for the improvement of fatigue performance of remanufactured titanium alloy.

Numerical simulation and experimental validation of microstructure evolution during the upsetting process of a large size martensitic stainless steel forging

The microstructure evolution, plastic deformation, and damage severity during the open die hot forging of a martensitic stainless steel were investigated using finite element (FE) simulation. A microstructure evolution model was developed and combined with a visco-elastoplastic model to predict the strain, the strain rate, and the temperature distribution, as well as the volume fraction and the size of dynamically recrystallized grains over the entire volume of an industrial size forging. The propensity to damage during hot forging was also evaluated using the Cockcroft & Latham model. The three models were implemented in the FE code and the results analyzed in terms of microstructure inhomogeneity and stress levels in different regions of the forging. A good agreement was obtained between the predicted and the experimental results, demonstrating that the simulation provided a realistic representation of the forging process at the industrial scale.

Effects of homogenization and deep cryogenic treatments on microstructure and mechanical property of D2 tool steel fabricated by laser direct energy deposition

The integration of laser direct energy deposition (L-DED) for manufacturing high-hardness D2 tool steel components presents a promising avenue for addressing the increasing complexity of product geometries demanded by modern industry. However, the inherent variability in microstructure and mechanical properties induced by L-DED across the build height necessitates the employment of post-processing techniques to achieve material homogeneity. This study explores the synergistic application of homogenization and deep cryogenic treatment (DCT) as a novel post-processing strategy aimed at mitigating microstructural inhomogeneities and enhancing the mechanical properties of L-DED-fabricated D2 tool steel. Initial analysis of the as-built samples revealed a microstructure characterized by a fine network of eutectic carbides enveloping an FCC matrix, which imposed constraints on martensite transformation during DCT. Homogenization was found to effectively alleviate these constraints, promoting compositional and microstructural uniformity and enabling a more consistent transformation to martensite across the samples upon subsequent DCT. The strategic combination of homogenization and DCT resulted in achieving uniformly distributed high hardness levels exceeding 750 HV throughout the entire sample, regardless of their initial positions within the build. This study demonstrates the potential of combining homogenization with DCT as an effective approach to enhance the structural integrity and mechanical performance of L-DED-fabricated D2 tool steel, offering valuable insights for the development of advanced manufacturing processes for alloyed materials.

Studies of electrical resistivity and magnetic properties of CuFe and CuNiFe films prepared by magnetron sputtering

The Cu-Fe binary alloys exhibit severe elemental segregation, resulting in an inhomogeneous microstructure, which leads to differences in microregion magnetic properties, thus affecting their application. Employing magnetron sputtering to produce films is advantageous for achieving a consistent dispersion of Fe within the Cu matrix. Furthermore, the addition of Ni will result in a more uniform distribution of Fe and facilitate the formation of the ferromagnetic Ni3Fe phase. In this study, Cu100−xFex and Cu100−x(Ni3/4Fe1/4)x series films were prepared by magnetron sputtering technique. The magnetic properties of films are closely related to their ferromagnetic element content. An increase in the content of ferromagnetic elements leads to an improvement in the saturation magnetization (MS) strength and a decrease in the coercivity (HC). The formation of Fe-Fe pairs is more favorable for magnetic properties compared to Ni-Fe pairs. Meanwhile, by comparing with bulk alloys, the distribution of the magnetic elements severely affects the magnetic properties. Moreover, the resistivity of Cu100−xFex films (20.3–96.7 μΩ cm) is much higher than that of Cu100−x(Ni3/4Fe1/4)x films (15.6–60.6 μΩ cm), which depends on the magnetic properties. This study systematically analyzes the effect of the content and distribution of magnetic elements on magnetic and electrical properties.