Heterogeneous Microstructure Research Articles

Phase reversion mediated the dual heterogeneity of grain size and dislocation density in an equiatomic CrCoNi medium-entropy alloy

An ultra-high strain rate (104 s-1) dynamic plastic deformation treatment at liquid nitrogen temperature (LNT-DPD) followed by annealing is carried out to obtain dual heterogeneity of grain size and dislocation density in an equiatomic CrCoNi medium entropy alloy (MEA). Such extreme loading conditions resulted in extensive phase transformation in this MEA. Subsequent annealing at 650°C for 1 h further induced reverse phase transformation and partial recrystallization, forming a complex heterogeneous microstructure characterized by nested trimodal grain sizes and partitioned dislocation density. A superior yield strength of ∼800MPa and a good ductility of ∼40% were simultaneously achieved in this heterogeneous alloy. In order to reveal the effects of grain size and dislocation density distributions on the mechanical property improvements, the underlying deformation mechanisms were systematically discussed. High density of geometrically necessary dislocations (GNDs) would be induced in complex heterogeneous structures during tensile deformation due to strain gradients or partitioning between different regions, which would lead to additional strengthening and work hardening. These results provide a novel approach to overcome the strength-ductility trade-off dilemma for FCC-structured MEAs.

Modulating NFO@N‐MWCNTs/CC Interfaces to Construct Multilevel Synergistic Sites (Ni/Fe‐O‐N‐C) for Multi‐Heavy Metal Ions Sensing

AbstractA hierarchical heterogeneous composite electrode of NiFe2O4@nitrogen‐doped multi‐walled carbon nanotubes/carbon cloth (NFO@N‐MWCNTs/CC) is prepared via a dip‐coating method, followed by a hydrothermal process. The flexible carbon cloth (CC) substrate provides robust support and the cross‐linked nitrogen‐doped multi‐walled carbon nanotubes (N‐MWCNTs) on the CC form a highly porous network with a large specific area that facilitates electron‐transfer. The stable support strengthens the framework and prevents pore structure disorder within the porous network, that could lead to the structural instability of the active sites. The decorated NiFe2O4 nanoparticles offer abundant active sites for enhanced electrocatalytic activity. Benefiting from the synergistic effect of the 3D hierarchical heterogeneous microstructure and multilevel bimetallic oxide active site (Ni/Fe‐O‐N‐C) constructs, the NFO@N‐MWCNTs/CC electrode achieves stable detection of multiple heavy metal ions (HMIs) with high reproducibility. The modified electrode allowed stable detection of multiple heavy metal ions with high reproducibility. The sensitivities of the electrode for Cd(II), Pb(II), Bi(III), and Hg(II) are 344.98, 441.02, 176.484, and 371.099 µA µm−1, respectively. The assay recoveries ranged from 95.3% to 106.8%, highlighting its practical applicability. This study provides innovative composites and theoretical insights to facilitate further advances in the simultaneous high‐performance detection of heavy metal ions.

Microstructure and mechanical properties of thin-walled TA1 titanium pipes fabricated by high-frequency induction welding

High frequency induction welding (HFIW) was effectively employed for the high-speed fabrication of thin-walled TA1 titanium pipes (TWTPs) with a nominal wall thickness of ∼0.6 mm. The microstructure and mechanical properties of TWTPs manufactured under varying welding parameters were investigated. The weld zone (WZ) exhibits a waist shape measuring ∼622 μm in width, and the width of the heat-affected zone (HAZ) spans between 763 and 864 μm. Both the WZ and HAZ are composed of a mixture of coarse serrated α grains with fine acicular and twins, while the BM retains equiaxed grains. This unique microstructure was resulted from the thermal cycling during HFIW, contributing to a notable increase in microhardness within the WZ compared to both the HAZ and the BM. Optimal manufacturing conditions were identified at a welding power of 14.4 kW, a welding speed of 60 m/min, an opening angle of 6°, and a squeeze displacement of 0.2 mm, yielding the TWIP with a tensile strength of ∼307 MPa and tensile elongation of ∼27%. Tensile fracture analysis revealed that failure predominantly occurred within the BM, underlining a ductile fracture mode characterized by pronounced dimple formations. The enhanced mechanical performance of the weld joints can be attributed to the heterogenous microstructure in the WZ, where the presence of large serrated α-grains enhances ductility, and the fine martensite and twins contribute to the high strength.

Synergetic effect of in-situ TiB2 reinforcement and nano precipitation on wear behavior of ZE41 magnesium matrix composite

The rise in carbon dioxide pollution and energy consumption has increased the demand for lightweight materials such as magnesium in automotive and aerospace industries. However, magnesium alloys face challenges like poor wear resistance and mechanical strength. To overcome these limitations, a promising approach involves developing heterogeneous hybrid microstructures through reinforcement addition and microstructural engineering. This study focuses on the tribological performance of a newly developed in-situ sub-micron sized TiB2/ZE41 composite under various microstructural conditions, comparing it to the unreinforced ZE41 Mg alloy. Wear experiments were conducted using a pin-on-disc tribometer under normal loads of 10, 20, 40, and 60 N at a sliding velocity of 1 m/s. Scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) was used to analyze the worn surfaces in order to identify damage types and surface distortions. By correlating worn surface microstructures with test parameters, predominant wear mechanisms for each material condition under specific loads were determined. Results consistently showed that the presence of in-situ TiB2 reinforcements, β-phase, and rare-earth precipitates enhanced wear resistance regardless of the load conditions. Additionally, the study established a scientific understanding of the wear behavior of ZE41 Mg alloy, with and without in-situ TiB2 particles and precipitates, through analysis of dominant wear mechanisms, wear-induced subsurface deformation mechanisms, kernel average misorientation, grain orientation spread, and microhardness evaluation.

Parallel two‐scale finite element implementation of a system with varying microstructure

AbstractWe propose a two‐scale finite element method designed for heterogeneous microstructures. Our approach exploits domain diffeomorphisms between the microscopic structures to gain computational efficiency. By using a conveniently constructed pullback operator, we are able to model the different microscopic domains as macroscopically dependent deformations of a reference domain. This allows for a relatively simple finite element framework to approximate the underlying system of partial differential equations with a parallel computational structure. We apply this technique to a model problem where we focus on transport in plant tissues. We illustrate the accuracy of the implementation with convergence benchmarks and show satisfactory parallelization speed‐ups. We further highlight the effect of the heterogeneous microscopic structure on the output of the two‐scale systems. Our implementation (publicly available on GitHub) builds on the deal.II FEM library. Application of this technique allows for an increased capacity of microscopic detail in multiscale modeling, while keeping running costs manageable.

Evolution of Graded Surface Microstructure and Property of Ti6Al4V Threads Processed by Surface Rolling

The surface rolling process is important for the forming property of titanium alloy bolts. This study systematically investigated the evolution of the surface microstructure and property of Ti6Al4V threads induced by surface rolling processes with different feeding times. Gradient surface microstructure and property, as characterized by the depth-dependent variations of refined and deformed grains and hardness, were revealed. A comparative analysis of the microstructure and property of the topmost and subsurface layers in different characteristic areas (root, flank, and crest) of the thread was specifically carried out. The surface microstructure and properties are highly heterogeneous in different areas of the rolled thread. Meanwhile, a gradient microstructure and hardness along the depth from the surface was revealed in the surface layer. Our results showed that the highly heterogeneous surface microstructure and property can be attributed to the close correlation between the different stress/strain levels at different depths from the surface and the different deformation mechanisms in the characteristic surface areas of the thread. The present study has indicated that the distinctive microstructure and property in the different characteristic areas of the rolled thread should be featured by those of surface layers at different depths.

Effect of Microalloying Rare-Earth Nd on Microstructure Evolution and Mechanical Property of Cu Alloy

Cu alloys have been widely used in the manufacture of liners because of their high density, good plasticity, and excellent thermal conductivity. In order to achieve excellent jet stability and penetration performance, it is necessary to further improve the mechanical properties of Cu-based liners. Nevertheless, the simultaneous enhancement of strength and ductility of the Cu alloys remains a huge challenge due to the strength–ductility trade-off phenomenon of metals/alloys. In this study, the microstructure evolution of rare earth Nd-modified Cu alloy and its effect on mechanical properties were investigated using OM, SEM, EBSD, and TEM techniques. The results show that the ultimate tensile strength (218 MPa) and elongation (50.7%) of sample 1 without Nd are the lowest. With increasing Nd content; the tensile strength and elongation of the samples increase; and the mechanical properties of sample 4 are the best, with a tensile strength of 278.6 MPa and elongation of 65.2%. In addition, with the increase in Nd content, not only is the grain size of the Cu-Nd alloy refined, but also the strength and plasticity are improved so that the strength–ductility trade-off phenomenon is improved. The strength improvement is mainly attributed to grain refinement strengthening, dispersion strengthening, and strain hardening. The increase in ductility is mainly related to the improvement of the microstructure heterogeneity by the Nd element.

Evaluation on tension-compression anisotropic behavior of recycled asphalt mixture

The utilization of recycled asphalt pavement (RAP) is the effective way to improve resource conservation and reduce energy consumption. The asphalt mixture is a kind of typical anisotropic pavement materials due to its heterogeneity in composition and microstructure. This could lead to the differences of mechanical response between the tensile and compressive direction. However, there are limited researches to study the effect of RAP on the tension-compression anisotropic behavior of asphalt mixture. The strength, modulus and fatigue resistance tests are carried out and different loading modes are adopted. The results show that the tension-compression anisotropic behavior is more prominent with the increase of RAP content. The regenerant served as a kind of typical additive could alleviate this effect. In addition, the result of dynamic modulus test shows that the tension-compression anisotropic behavior has an increasing trend with the decrease of frequency and the increment of temperature. The ranking of fatigue life is opposite for the direct tensile and compressive loading mode, and the fatigue life ratio of compression to tension also show positive relation with the RAP content. Due to the difference in the stress mode, the fatigue life between the indirect tensile loading and four-point bending loading also show opposite trend, and the indirect tensile fatigue life has a larger discreteness.

Impact of Asymmetric Microstructure on Ion Transport in Ti3C2Tx Membranes.

Consolidation or densification of low-dimensional MXene materials into membranes can result in the formation of asymmetric membrane structures. Nanostructural (short-range) and microstructural (long-range) heterogeneity can influence mass transport and separation mechanisms. Short-range structural dynamics include the presence of water confined between the 2D layers, while long-range structural properties include the formation of defects, micropores, and mesopores. Herein, it is demonstrated that structural heterogeneity in Ti3C2Tx membranes fabricated via vacuum-assisted filtration significantly affects ion transport. Higher ion permeabilities are achieved when the dense "bottom" side of the membrane, rather than the porous "top" side, faces the feed solution. Characterization of the membrane reveals distinct differences in flake alignment, surface roughness, and porosity across the membrane. The directional dependence on permeability suggests that one region of the membrane experiences stronger internal concentration polarization, potentially suppressing permeability through the porous side of the membrane.

Effect of flax and hemp flour on the nutritional value of turkey-duck meat pate

This study focused on developing a nutritionally enhanced turkey meat pate, incorporating plant-based ingredients like flaxseed and hemp flour. Two canned pate samples were produced: a control sample with turkey meat, liver, heart, fat, skin, beans, onions, and spices, and an experimental sample where 20% of turkey meat was replaced with duck meat, and beans were substituted with zucchini, flaxseed, and hemp flour. The experimental pate showed significant differences in chemical composition compared to the control. It had lower moisture and fat content but higher protein, ash, and carbohydrate content. The energy value slightly decreased from 153.01 kcal/100g to 146.9 kcal/100g. The sensory evaluation found similarities in appearance, consistency, and colour, with the experimental pate receiving a slightly higher colour rating. The amino acid profile of the experimental pate was significantly altered, with increases in methionine, isoleucine, threonine, glutamic acid, alanine, and cysteine. Vitamin and mineral content also significantly increased, particularly vitamins A, D, E, and B group vitamins, calcium, potassium, magnesium, and iron. Microscopic analysis revealed a more heterogeneous microstructure in the experimental pate due to the plant ingredients. This research demonstrates the potential of developing a healthier turkey meat pate using plant-based ingredients, catering to the growing demand for healthier food options.

Spectroscopic analysis of Nd3+doped Ba3Bi(PO4)3 phosphor for near-infrared laser application

Near infrared (NIR) emission plays a crucial role in various applications, driving ongoing research to identify new hosts capable of NIR emission. This article explores NIR emission in the Ba3Bi(PO4)3 host. X-ray diffraction (XRD) patterns confirm that the Ba3Bi(PO4)3 belongs to Eulytite family (I4¯3d). Electron micrographs revealed the development of heterogeneous microstructures with noticeable agglomeration. Nd3+ was used as an activator to achieve NIR emission. In the emission spectra characteristic lines were observed. Among them the one at 1062 nm (Nd3+: 4F3/2 → 4I11/2) is the most intense. Results on the effect of increasing activator concentration on luminescence intensity are also presented. The highest intensity is observed for the composition Ba3Bi0.095Nd0.05(PO4)3. A decrease in intensity beyond 5.0 mol% is attributed to concentration quenching. Based on these findings, the critical distance, Rc was evaluated as 22.29 Å. These results indicate that the optimized Nd3+doped Ba3Bi(PO4)3 phosphor has potential as NIR-emitting materials for laser applications and infrared bioimaging.

Damage sensing in multi-functional nanocomposite polymer bonded energetics with embedded multi-walled carbon nanotube sensing networks

Abstract This experimental investigation evaluates the strain and damage sensing abilities of multi-walled carbon nanotube (MWCNT) networks embedded in the binder phase of polymer-bonded energetics (PBEs). PBEs are a special class of particulate composite materials that consist of energetic crystals bound by a polymer matrix, wherein the polymer matrix serves to maintain the composite’s shape and form. The structural health monitoring (SHM) approach presented in this work exploits the piezoresistive properties of the distributed MWCNT networks. Major challenges faced during such implementation include the low binder concentrations of PBEs, the presence of conductive/non-conductive particulate phases, the high degree of heterogeneity in the PBE microstructure, and achieving the optimal MWCNT dispersion. In this study, ammonium perchlorate (AP) crystals as the oxidizer, Aluminum grains as the metallic fuel, and Polydimethylsiloxane (PDMS) as the binder are used as the constituents for fabricating PBEs. To study the effect of each constituent on the MWCNT network’s SHM abilities, various materials systems are comprehensively studied: MWCNT/PDMS materials are first evaluated to study the binder’s electromechanical response, followed by AP/MWCNT/PDMS to assess the impact of AP addition, and finally, AP/AL/MWCNT/PDMS to evaluate the impact of adding conductive aluminum grains. Compression samples (ASTM D695) were fabricated and subjected to monotonic compression. Electrical resistance is recorded in conjunction with the mechanical test via an LCR meter. Gauge factors relating to the change in normalized resistance to applied strain are calculated to quantify the electromechanical response. MWCNT dispersions and mechanical failure modes are analyzed via scanning electron microscopy imaging of the fracture surfaces. Correlations between the electrical behavior in response to the mechanical behavior are presented, and possible mechanisms that influence the electromechanical behavior are discussed. The results presented herein demonstrate the successful ability of MWCNT networks as SHM sensors capable of real-time strain and damage assessment of PBEs.

Optimized pyrolytic synthesis and physicochemical characterization of date palm seed biochar: unveiling a sustainable adsorbent for environmental remediation applications.

This study focuses on the optimization and comprehensive characterization of biochar synthesized from date palm seeds (DPS), a prevalent agricultural waste in arid regions. Using response surface methodology (RSM) with a central composite design (CCD), we optimized the pyrolysis process by investigating the effects of time (1-3 h) and temperature (600-900 °C) on critical properties such as specific surface area, pore volume, and yield. The optimized biochar, produced at 828 °C for 1.7 h, demonstrated a high specific surface area of 654.8 m2/g and well-developed microporosity. Characterization techniques, including XRD, FTIR, SEM-EDS, and BET analyses, revealed an amorphous carbon structure with graphitic domains, diverse surface functionalities, and a heterogeneous porous microstructure. The biochar's point of zero charge at pH 7.58 indicates its potential for selective adsorption of charged contaminants. The close agreement between RSM-predicted and experimental values for specific surface area (652.1 m2/g vs. 654.8 m2/g) and micropore volume (0.191 cm3/g vs. 0.190 cm3/g) validates the effectiveness of the model in optimizing biochar properties. This research highlights the potential of DPS-derived biochar as a sustainable adsorbent for environmental remediation, opening avenues for valorizing agricultural wastes and contributing to circular economy principles.

On the heterogeneous microstructure and strengthening mechanisms in a laser welding AZ80 magnesium alloy

This study investigates the microstructural characteristics and mechanical properties of a laser welded AZ80 magnesium alloy. The welding process led to the formation of coarse-grained fusion zone (FZ), where a secondary phase formed continuous network. Mg17Al12 precipitation and coarsening of grain boundaries occurred in the heat affected zone. The welded joint exhibited excellent mechanical properties with a yield strength of 202 MPa and a joint efficiency of 92%. The microstructure analysis via EPMA and EBSD in conjunction with synchrotron X-ray diffraction analysis reveals that precipitates and increased dislocation density in the fusion zone are primary strengthening mechanisms for the laser welded AZ80 Mg alloy.

Nanoscale heterogeneities dictate corrosion pathways in a high-strength aluminum alloy

Micro-segregation and resulting nanoscale microstructural heterogeneities are unavoidable in wrought 7xxx aluminum alloys produced using current casting and thermomechanical processes. This study demonstrates that these nanoscale heterogeneities significantly impact pit growth in an extruded, age-hardened aluminum alloy 7075-T651. The alloy exhibits a complex microstructure with heterogeneously distributed E-Al18Mg3Cr2 dispersoids, which promote the precipitation of coarse ƞ-Mg(ZnAlCu)2 nanoparticles resulting in the formation of solute-depleted regions both within the grain interior and along the grain boundaries in dispersoid-rich areas. These alterations affect resistance to pit growth at the nanoscale, governing the transition of micro-galvanic sites into large pits with potential for crack initiation. This work underscores the necessity for modifying alloy composition and casting processes to develop superior aluminum alloys for critical applications.

Effect of Microstructure Heterogeneity on Shale Strength: Insights from Micro-CT Imaging and Numerical Simulations

Effect of Microstructure Heterogeneity on Shale Strength: Insights from Micro-CT Imaging and Numerical Simulations

Achieving high strength in Mg-Gd-Ag-Zr alloy through heterogeneous microstructure with multimodal grain structure and hierarchical precipitates

The development of high-strength Magnesium (Mg) alloys is a key research focus due to their relatively low strength compared to other structural metals. In this paper, a high-strength Mg-13.4Gd-2.2Ag-0.4Zr wt% alloy is achieved by carefully designing a multimodal grain structure combined with hierarchical precipitates, using a processing route of hot rolling followed by aging. The multimodal grain structure, characterized by three distinct grain size distributions and a strong basal texture, arises from partial dynamic recrystallization during hot rolling. The hierarchical precipitates include microscale rod-like and particle-like β phase at grain boundaries, twins, and deformation bands, as well as nanoscale β phase precipitates (~63nm) dispersed within the grain interiors. The fully β precipitates also demonstrate a modified precipitation pathway, differing from the β' and γ'' nanoprecipitates observed in conventional Mg-Gd-Ag alloys. This unique microstructure results in an ultimate tensile strength of 447MPa, primarily attributable to the strong basal texture, hierarchical precipitates, hetero-deformation-induced (HDI) strengthening, and high dislocation density.

Unleashing the elastocaloric cooling potential of 3D-printed NiTi alloy with heterogeneous microstructures and Ni4Ti3 nanoparticles

Toward the development of elastocaloric (eC) refrigeration applications, this study examines how Ni4Ti3 nanoparticles improve the eC properties of laser powder bed-fused (LPBF) NiTi alloys, with a focus on the formation of a NiTi/Ni4Ti3 nanocomposite. The LPBF-produced microstructure offers significant advantages: i) a heterogeneous grain structure that provides complementary benefits—fine grains offer higher deformation resistance while coarse grains initiate phase transformation (PT) earlier, releasing more latent heat; ii) a strong <001>//building direction texture that enhances recoverability. However, these benefits are partially limited by grain boundary slip during PT, leading to lower cooling efficiency and increased energy dissipation in as-built NiTi alloys. To address these issues, Ni4Ti3 nanoparticles are introduced through aging treatment, forming a composite structure that strengthens grain boundaries. Given the challenges of applying severe plastic deformation to 3D-printed components, this approach may offer a more practical solution. The study also reveals that Ni4Ti3 nanoparticles contribute to: 1) reducing Ni content in the matrix, increasing lattice size and enthalpy, which enhances the temperature drop (ΔTad); and 2) promoting R phase formation, which hinders the B2↔B19' PT, reducing energy dissipation and improving the coefficient of performance (COPmat). The balance of these effects depends on nanoparticle size, with smaller particles (∼5–12 nm) amplifying the second effect, while larger particles (∼130 nm) increase the first effect. At 350°C aging, the optimized nanocomposite exhibits a maximum COPmat of 15 and ΔTad of 14K, representing a 163% improvement over the as-built alloy. This work highlights the potential of NiTi composites in 3D-printed eC components.

Additive manufacturing of sustainable and heat-resistant Al-Fe-Mo-Si-Zr alloys

Improving the sustainability of metals and alloys is essential for slowing down global warming. The reason is that their extraction and production stand for about 40% of all greenhouse gas emissions in the industrial sector. This motivates new alloy design and processing criteria such as the (1) preferred use of abundant and sustainable alloying elements and (2) improved material tolerance against impurity intrusion from recycling. In this context, additive manufacturing (AM) is attractive, through rapid solidification, capable of quenching impurities into a solid solution state, avoiding formation of large intermetallics and introduction of metastable phases. Here, by using this approach we show how iron, an important scrap-related contaminant in aluminum alloys, can be turned from a harmful into a valuable ingredient. Specifically, the addition of Mo and Si facilitates the formation of beneficial metastable body-centred cubic (BCC) Al12(Fe, Mo)3Si phase, instead of more stable but detrimental intermetallic variants commonly observed in Al-Fe alloys. The as-built microstructures have excellent thermal stability, tested up to 200hours at 300 °C, because of low diffusivity of Fe and the formation of Zr shell. We find that for such supersaturated alloys, two issues are important, namely (a) the heterogeneous microstructures in the as-built condition, (b) the evolution of metastable precipitates during heating. We suggest that this type of approach help to guide sustainable alloy design via AM and other rapid solidification processes.

Coupled effect of microstructure heterogeneity and hydrogen on local embrittlement of CGHAZ and IC-CGHAZ in X65 pipeline steel

The local embrittlement of the coarse-grained heat-affected zone (CGHAZ) and intercritically reheated CGHAZ (IC-CGHAZ) in X65 pipeline steel was investigated using an in situ crack-tip opening displacement test in air and H2S, combined with microstructure-based simulation. The IC-CGHAZ exhibited significantly lower cracking resistance, with the fracture toughness reduced by 50% compared to CGHAZ in both environments (0.160 mm in air and 0.017 mm in H₂S for IC-CGHAZ, compared to 0.307 mm in air and 0.034 mm in H₂S for CGHAZ). The martensite/austenite (M/A) constituents showed exceptionally higher intrinsic hardness than the ferrite matrix. The continuous distribution of M/As along the prior austenite grain boundaries resulted in local hardening and the formation of heterogeneous hard zones in IC-CGHAZ. Such microstructure heterogeneity resulted in the unique partitioning of plastic strain localization and stress triaxiality that promotes premature fracture, particularly with the coupled effect of hydrogen. This study provides a novel perspective on the fracture mechanisms and the typical fracture morphology of IC-CGHAZs in pipeline steel under the coupled effect of microstructure heterogeneity and hydrogen.