Microstructure Formation Research Articles

Enhanced mechanical properties of the additively manufactured IN738LC superalloy through thermal history management during the laser powder bed fusion process

IN738LC superalloy, as one of the hard-to-weld Ni-based superalloys, is relatively difficult to be produced by laser powder bed fusion (LPBF) due to its high cracking susceptibility. In this study, local heat accumulation based on substrate preheating and chessboard scanning strategy modification was proposed to reduce the thermal stress and promote the dynamic precipitation of IN738LC superalloy during LPBF process, which contributes to the crack inhibition and mechanical property enhancement. The as-built IN738LC superalloy exhibited superior room temperature tensile yield strength (YS) of 1011 ± 7 MPa, ultimate tensile strength (UTS) of 1400 ± 12 MPa, and good ductility of 17.4 ± 2.9 %. The superior mechanical performance was achieved mainly due to the successful elimination of micro-cracks, the formation of hierarchical microstructure composed of columnar γ grains, cellular dislocation network, especially in-situ formation of carbide precipitates. The formation of micro-cracks was fully eliminated due to the reduced temperature gradient and residual stress. In-situ formation of carbide precipitates was enabled by well-controlling the thermal history during the LPBF process. The use of a chessboard scanning strategy and substrate preheating was found to be beneficial for achieving a larger melting pool size, coarser dendrite/cellular arm spacing, and a larger volume of carbide precipitates due to enhanced heat accumulation during the LPBF process, which was verified by finite element analysis. This work provides insights into the effects of thermal profiles inherent to LPBF processes on the performance of LPBF-processed IN738LC superalloy.

Regulation of Osteogenic and Angiogenic Markers in Alkali Treated Titanium for Hard Tissue Engineering Applications.

Titanium (Ti) and Ti alloys are of great interest in bone and dental tissue engineering applications due to their biocompatibility, corrosion resistance, and close mechanical properties to natural bone. However, the formation of fibrous tissue prevents osteointegration and results in implant loosening. Thus, physical and chemical methods are used to improve the surface properties of Ti. This study aimed to understand the role of alkali treatment conditions, including alkali medium concentration, temperature, rotation speed, and post-heat treatment. Our results showed that alkali treatment using 5 and 10 molar sodium hydroxide solution allows the formation of web-like microstructure. However, a higher concentration of 15 molar resulted in cracks along the surface. Interaction between the human fetal osteoblast cells (hfOBs) and Ti samples showed that heat treatment is necessary for increased cellular proliferation, which was not significantly different at later time points compared to the polished Ti. Alkali heat treatment did not induce inflammatory reactions at later time points. It showed an increase in vascular endothelial growth factor, osteoprotegerin/nuclear factor kappa-В ligand ratio, and osteocalcin expression, which is evidence for accelerated osteoblast cell maturation and bone remodeling in surface-modified samples. Together, these data show that alkali treatment using 5 or 10 molar of NaOH followed by heat treatment may have therapeutic effect and assist with bone tissue integration with Ti implant.

Exploring spatial beam shaping in laser powder bed fusion: High-fidelity simulation and in-situ monitoring

Laser beam shaping is a novel and relatively unexplored method for controlling the melt pool conditions during metal additive manufacturing (MAM) processes, but even so it still holds good promise for achieving site-specific tailored properties. In this work, a comprehensive numerical and experimental campaign is carried out to explore this subject within metal laser powder bed fusion (LPBF). More specifically, a multiphysics numerical model is implemented for simulating the heat and fluid flow conditions during LPBF of Ti6Al4V using arbitrary circular beam shapes with various power distributions spanning from a pure Gaussian beam to a pure ring beam profile. The model is subsequently coupled with cellular automata to describe the beam shape effects on the microstructure evolution. Model validation is carried out in a two-fold manner. First, we compare the predicted melt pool cross-section with the one from ex-situ single track experiments, and we find a deviation of less than 9 % in melt pool dimensions. Secondly, advanced in-situ X-ray monitoring is carried out to unravel the melt pool dynamics and we find that the predicted morphology closely matches the in-situ X-ray results. Moreover, it is shown that at lower laser power, a bulge of liquid metal forms at the center of the melt pool when employing ring profiles, and this is ascribed to the absence of recoil pressure at the center of the ring beam. Furthermore, increasing the laser power seems to destabilize the melt pool regime, as the central bulge transforms into a liquid metal jet that periodically collapses and breaks up into hot spatter. Based on the results, we believe that our multiphysics modelling methodology, opens up new pathways for predicting how laser beam shaping influences porosity, surface roughness as well as microstructure formation in LPBF processes.

Investigation of Co-Cr alloy layer prepared by laser metal deposition

Abstract Additive technologies are commonly used for component production and repair. Laser metal deposition is a type of additive technology that can create new bodies or add new components to existing parts. This technology enables continuous modification of the chemical and material properties of the deposited layer to suit the intended purpose. The alloying powder is dissolved and mixed in a small volume molten pool during laser deposition. The laser cladding process is known for its rapid heating and cooling rates. This can result in partial or non-existent dissolution of powder particles in the molten pool, or the formation of non-equilibrium microstructures that cannot be achieved through conventional metallurgical processes. As a result, this method can be used to create materials with unique combinations of properties. In this study, a Co-Cr coating layer was applied to a structural steel base plate. The parameters combination was generated using Taguchi’s experimental design. The relationship between the parameters and the properties of the prepared coating was evaluated using the Taguchi method.

Study on solidification organization and phase formation of Fe-6.5wt.%Si high silicon steel by arc melting and heat treatment

Abstract The solidification microstructure and phase formation behavior of Fe-6.5wt.%Si high silicon steel was investigated using arc melting and heat treatment. The alloy phase composition and microstructure were analyzed by XRD and SEM. The magnetic performance was measured at a high- and low-temperature vibration sample magnetometer. The results show that the temperature gradient causes alloy ingot to be roughly divided into three layers. With the decrease in temperature, from the bottom to the top, the phase morphology is fine crystals, columnar internal dendrites, and isoaxial internal dendrites. In the annealing ring ingot, the inner dendrites disappeared, and from the bottom to the top of the sample, the microstructure changed from fine crystal, columnar crystal, and isoaxial crystal, to micro-cracks, which first increased and then reduced. The hysteresis loop curve width of the alloy is narrow, the slope is large, the hysteresis is 0.126 emu/g, and the magnetic utilization after annealing decreases to 0.0667 emu/g, but the coercive force increases to 2.8 Oe/g, and the annealed alloy is more sensitive to the magnetic field and has a high magnetic conductivity coefficient.

IMAGE-BASED CROSS-SECTIONAL ANALYSIS AND MICROMECHANICAL MODELING OF YARN AND COMPOSITE MATERIALS

This study aims to establish a comprehensive methodology for determining the microstructural properties of hybrid yarns used in composite materials. By developing accurate models of hybrid yarns and composites based on detailed microstructural information such as fibre orientation, fibre diameter and distribution, this approach lays the foundation for future advances. These models, enriched with accurate microstructural data, will facilitate the creation of new modelling techniques that can be used in future research to explore the correlation between microstructural properties and mechanical performance of composite materials.

Corrosion behavior of 2A97 Al−Cu−Li alloys in different thermomechanical conditions by quasi-in-situ analysis

As a promising material in the aircraft industry, 2A97 Al−Cu−Li alloy exhibits high corrosion susceptibility that may limit its application. In the present work, to illustrate the influences of precipitate and grain-stored energy on localized corrosion evolution in 2A97 Al−Cu−Li alloy, cold working and artificial aging were carried out to produce 2A97 Al−Cu−Li alloys under different thermomechanical conditions. Quasi-in-situ analysis, traditional immersion test and electrochemical measurement were then conducted to examine the corrosion behavior of 2A97 alloys. It is revealed that precipitate significantly affects Cu enrichment at corrosion fronts, which determines corrosion susceptibility of alloys, whereas grain-stored energy distribution is closely associated with localized corrosion propagation. It is also indicated that quasi-in-situ analysis exhibits a consistent corrosion evolution with traditional immersion tests, which is regarded as a proper method to explore localized corrosion mechanisms by providing local microstructural information with enhanced time and spatial resolutions.

Study on asymmetric forming and performance strengthening mechanisms of 6061-T6 aluminum alloy joints fabricated by oscillating laser based on keyhole characteristics and molten pool dynamic behaviors

The study intends to unravel the processes behind the particular forming and performance improvement of 6061-T6 aluminum alloy joints by getting a thorough understanding of keyhole features and dynamical characteristics of molten pools during the laser welding with circular oscillation (C-OLW) process. The C-OLW experiments were carried out considering the pivotal parameters, including oscillation frequency (f) and amplitude (A), and their impacts on joint formation, microstructure, and performance were analyzed. Increasing f from 200 Hz to 300 Hz results in a more homogeneous and centered laser energy distribution, reducing weld breadth and the maximum depth. Raising A from 1.2 mm to 1.5 mm concentrated energy along the workpiece surface, increasing weld breadth but decreasing the maximum weld depth. A three-dimensional transient numerical model was established and verified. The simulation results reveal that increasing f considerably improves keyhole stability by virtue of the beam's mixing effect on energy, resulting in a more evenly distributed temperature within the molten pool. The velocity of the beam's motion intensifies, leading to elevated local temperature and subsequently causing an escalation in splattering. When A grows, keyhole stability reduces, as does the intensity of molten pool flow. The major effect of increased frequency is refining the grain size while increasing amplitude primarily promotes the columnar-to-equiaxed transition (CET) process. The extracted results of temperature distribution illustrate that an increase in f leads to an increase in the solidification rate (R), and temperature gradient values (G) are similar or higher along the same isotherm. Therefore, the G/R ratio rises, promoting the formation of finer microstructures. Although increasing A diminishes G, the reduced overall temperature and molten pool volume contribute to the rise in R. Consequently, the G/R ratio declines, fostering equiaxed grain growth, in line with experimental observations. A higher G value on the left side corresponds to finer grain structures, corroborating experimental findings via Electron Backscatter Diffraction (EBSD). The keyhole stability and microstructure characteristics explain why increasing f or A can enhance joint performance. The research reveals that strategically augmenting both oscillation frequency and amplitude enables the achievement of enhanced performance in 6061-T6 aluminum alloy joints.

A novel ultrasonic rolling assisted direct energy deposition method with semi-solid thixo-forming characteristics for AA6061

In order to overcome the defects during the process of additive manufacturing for AA6061, a novel ultrasonic rolling assisted direct energy deposition method with semi-solid thixo-forming characteristics was proposed in this study, which used cold deformed AA6061 wire as raw material, and a corresponding process platform was established. The results showed that under the conditions of laser heating temperature of 750 ℃ and heating plate temperature of 200 ℃, the sample could achieve continuous multi-pass deposition while retaining some of the cold-drawn plastic deformation energy. When the vertical deformation rate was 0.153 and the ultrasonic amplitude was 20 μm, the microstructure of deposition sample after semi-solid heat-treat exhibited typical equiaxed grain characteristics, corresponding to average grain diameter of 95.6 μm and shape coefficient of 1.263. Thin-walled samples with different shapes were formed to verify the capability of process platform. The inference of the formation mechanism of semi-solid microstructure was revealed at last: the introduction of ultrasonic rolling supplemented the plastic deformation energy, and semi-solid heat-treat provided temperature and time for the incubation of equiaxed grains, both of which were crucial for the formation of the semi-solid microstructure.

Revealing the anisotropic response of grain structures in additive manufactured Al-Mn-Sc alloys: Modeling based on experiments

The anisotropy of yield strength of additive manufactured (AM) Al-Mn-Sc alloy is attributed to the diverse distribution characteristics of grain size, aspect ratio and orientation. This work focus on controlling the yield strength and anisotropy of AM aluminum through microstructure design. In this work, microstructures information of laser powder-bed fusion (LPBF) processed Al-Mn-Sc alloys were obtained by electron back scatter diffraction (EBSD) analysis. The impact of grain size, aspect ratio and orientation on strength and anisotropy are quantitatively researched through modeling. Base on quantitative effect of orientation on strength and anisotropy, all microstructure partition schemes are calculated by MATLAB. Microstructure partition schemes of alloy with low anisotropy and high yield strength were predicted and simulation was enforced to certify the credibility of predication. Local stress in grain and orientation variation during deforming were obtained by simulation. It is concluded that the impact of orientation is more obvious than grain size and aspect ratio. Compared with strength and anisotropy obtained by simulation, the prediction of calculation shows fine precision. The impact of microstructures on mechanical properties and the reliability of modeling were verified.

Making 2D Materials Sparkle in Energy Storage via Assembly.

ConspectusTwo-dimensional (2D) materials such as graphene and MXenes offer appealing opportunities in electrochemical energy storage due to their large surface area, tunable surface chemistry, and unique electronic properties. One of the primary challenges in utilizing these materials for practical electrodes, especially those with industrial-level thickness, is developing a highly interconnected and porous conductive network. This network is crucial for supporting continuous electron transport, rapid ion diffusion, and effective participation of all active materials in electrochemical reactions. Moreover, the demand for efficient energy storage in advanced electronic devices and electric vehicles has led to the need for not only thicker but also denser electrodes to achieve compact energy storage. Traditional densification methods often compromise between volumetric capacitance and ion-accessible surface area, which can diminish rate performance. As versatile building blocks, 2D materials can overcome these limitations through the assembly into complex superstructures such as 1D fibers, 2D thin films, and 3D porous networks, a capability less attainable by other nanomaterials.This Account explores the pathways from exfoliated 2D nanosheets to densely packed, yet porous assemblies tailored for compact energy storage. Focusing on graphene and MXenes, we delve into the intricate relationships between surface structure, assembly behaviors, and electrochemical performance. We emphasize the crucial role of surface chemistry and interfacial interactions in forming stable colloidal dispersions and subsequent macroscopic structures. Furthermore, we highlight how solvents, acting as spacers, are instrumental in microstructure formation and how capillary force-driven densification is essential for creating compact assemblies. With precise control over shrinkage, the customized dense assemblies can strike a balance between high packing density and sufficient porosity, ensuring efficient ion transport, mechanical stability, and high volumetric performance across various electrochemical energy storage technologies.Furthermore, we highlight the importance of understanding and manipulating the surface chemistry of 2D materials at the atomic level to optimize their assembly and enhance electrochemical behaviors. Advanced in situ characterizations with high temporal and spatial resolution are necessary to gain deeper insights into the complex assembly process. Moreover, the integration of machine learning and computational chemistry emerges as a promising method to predict and design new materials and assembly strategies, potentially accelerating the development of next-generation energy storage systems. Our insights into the assembly and densification of 2D materials provide a comprehensive foundation for future research and practical applications in compact, high-performance energy storage devices. This exploration sets the stage for a transformative approach to overcoming the challenges of current energy storage technologies, promising significant advancements in 2D materials in the field.

Research Progress on the Microstructure Evolution Mechanisms of Al-Mg Alloys by Severe Plastic Deformation.

Al-Mg alloys are widely used as important engineering structural materials in aerospace engineering, transportation systems, and structural constructions due to their low density, high specific strength, corrosion resistance, welding capability, fatigue strength, and cost-effectiveness. However, the conventional Al-Mg alloys can no longer fully satisfy the demands of practical production due to difficulties caused by many defects. The high strength of Al-Mg alloys as non-heat treatment precipitation-strengthened alloys is achieved primarily by solid solution strengthening along with work hardening rather than precipitation strengthening. Therefore, severe plastic deformation (SPD) techniques can be often used to produce ultrafine-grained structures to fabricate ultra-high strength aluminum alloys. However, this approach often achieves the strengthening of material at the cost of reduced ductility. This paper comprehensively summarizes the various approaches of ultrafine/nanocrystalline materials for enhancing their plasticity, elaborates on the creation of a bimodal microstructure within the alloy, and discusses the formation of a nanotwin microstructure within the alloy and the incorporation of dispersed nanoparticles. The mechanisms underlying both the strengthening and toughening during large plastic deformation in aluminum alloys are summarized, and the future research direction of high-performance ultrafine crystalline and nanocrystalline Al-Mg aluminum alloys is prospected.

Formation of Microstructure and Mechanical Properties of Co-Cr-Mo Alloy by Hot Forging and Subsequent Radial Shear Rolling

Formation of Microstructure and Mechanical Properties of Co-Cr-Mo Alloy by Hot Forging and Subsequent Radial Shear Rolling

Effect of Stöber Nano-SiO2 Particles on the Hydration Properties of Calcined Coal Gangue-Blended Cement.

This study focuses on the calcined coal gangue (CCG)-blended cements containing Stöber nano-SiO2 (SNS) particles. The effects of SNS particles on the workability, hydration behaviour, mechanical properties and microstructure evolution of the blended cements were comprehensively investigated at curing ages ranging from 1 to 28 d. The hydration behaviour was studied via isothermal calorimetry test, X-ray diffraction (XRD) and thermogravimetric (TG) tests. The microstructural evolution was studied using mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM). The results show that the incorporation of SNS led to a significant reduction in fluidity, particularly at an SNS content of 3%. The SNS significantly increased the compressive strength of the CCG-blended cement at all curing ages, and the optimum SNS content was found to be 2%. SNS significantly accelerated not only the early cement hydration but also the pozzolanic reaction of CCG at later curing ages, resulting in a decrease in portlandite, as evidenced by the isothermal calorimetry, XRD and TG analysis. Microstructural analysis shows that the incorporation of SNS effectively refined the pore structure of the CCG-blended cement, resulting in the formation of a dense microstructure. All these beneficial effects of SNS provides advantages in the development of the compressive strength of the CCG-blended cement at all curing ages.

Hydration and microstructure formation of magnesium oxysulfate (MOS) cement regulated by sepiolite with high adsorption ability

Magnesium oxysulfate (MOS) cement is a potential low-carbon cementitious material with its characteristic depending on the reaction between light-burned magnesia (LBM) and MgSO4 solution. This work aimed to elucidate the effect of sepiolite with high adsorption ability on regulating the reaction within MOS cement. Replacement levels of LBM by sepiolite at 2 and 5 wt% were adopted. Hydration kinetics, microstructure, phase composition and compressive strength of MOS cement without and with sepiolite were studied. Results showed that adding sepiolite into MOS cement adjusted the ion distribution at the early hydration stage and promoted the reaction with an early onset of heat flow peaks. The presence of sepiolite refined the morphology of formed needle-like 5 Mg(OH)2·MgSO4·7H2O (517 phase) and strengthened the bond water within its structure. The high adsorption ability of sepiolite enabled the nucleation of 517 phase and amorphous phase onto its surface. Sepiolite also densified the poorly hydrated regions by tightly combining with the incompletely hydrated MgO grains. Consequently, compressive strength of MOS cement under air curing was improved after adding sepiolite.

Infrared microlens formation on chalcogenide polymer surface via femtosecond laser pulse ablation

In this study, we introduced micro-optical surface formation via femtosecond (fs) laser pulse scanning to chalcogenide polymer (ChP), a promising material for cost-effective infrared applications. Employing this method, we successfully fabricated a large-area poly(sulfur-random-(1,3-diisopropenylbenzene)) (S-r-DIB) microlens array (MLA) component. Each micro-concave spherical surface was crafted with a single fs laser pulse, serving as a micro-concave lens surface. We achieved a quasi-periodic MLA sample with over 2 × 105 micro-lenslets within a 10 mm × 10 mm footprint. Additionally, precise locating of laser pulse irradiation enabled us to create a hexagonal MLA with a filling factor over 37 %. Morphological investigations and imaging tests confirmed the adequate surface quality of the fabricated components, with its uniformity revealed by the virtual foci grid in near infrared region. To elucidate the forming conditions and mechanisms, we studied the evolution of surface morphology under various laser irradiation conditions. Laser induced damage thresholds of S70-r-DIB30 were experimentally determined for both 800 nm and 400 nm wavelengths under single- and multi-pulse irradiation scenarios. We identified the optimal fabrication fluence window as 115–205 mJ/cm2 with 800 nm single-pulse irradiation. The bandgap of the S70-r-DIB30 was estimated as 2.06 eV, and energy band analysis confirmed distinctions in ablation morphology. Furthermore, we investigated sub-surface morphology evolution using orthogonal ultrafast pump–probe imaging, revealing diversity compared to traditional inorganic and polymeric optical materials due to differing absorption and etching mechanisms. The elastic wave velocity of 3.2 km/s in this ChP and etching velocity of 0.7 μm/pulse were experimentally determined. These findings deepen our understanding of ChP material interaction with fs lasers, offering insights for potential applications such as surface engineering, substrate cutting, and micro-structure formation.

High performance CaCO3-based composites using sodium tripolyphosphate as phase controlling additive: Bamboo fiber driven high strength development

Due to the limited carbonation degree caused by the surface densification of carbonated products, the development of high-strength carbonated composites remains challenging. In this work, bamboo fiber (BFs) is utilized as a reaction reinforcing agent along with sodium tripolyphosphate (STPP) as a CaCO3 phase controlling additive to prepare high-strength bamboo fiber reinforced carbonated wollastonite composites (BFRCWs). The phase composition and microstructure are systematically investigated by multiscale physicochemical analysis, followed by the determination of macro properties and volume deformation. Results indicate that BF and STPP have a synergistic effect on the microstructural formation and macro performance of BFRCWs. STPP-treated BF (ST-BF) can serve as an internal curing agent and the porous structure of BF provides more channels for ion and CO2 transport, whereas CaCO3 phase composition and cementitious behavior is modified by STPP. The addition of ST-BF, particularly for long fibers, accelerates the carbonation reaction, resulting in an increased ratio of poorly crystalline CaCO3 and a refined pore structure. With increasing ST-BF dosage (0–3 vol%), the cementitious reaction is enhanced, but excessive fibers (3 vol%) incorporation introduces additional porosity, consequently reducing compressive strength. The desired pore structure with the optimal 2 vol% ST-BF (3–6 mm) shows the highest strength of 103.5 MPa at 28 days.

Microstructure and Mechanical Properties of the Powder Metallurgy Nb-16Si-24Ti-2Al-2Cr Alloy.

The Nb-16Si-24Ti-2Al-2Cr alloy was prepared by plasma rotating electrode process (PREP) technology and the hot-pressing (HP) method, and the effects of sintering temperature on the microstructure, mechanical properties and fracture behavior were investigated. The HP alloys sintered at temperatures below 1400 °C are composed of Nbss (Nb solid solution), Nb3Si and Nb5Si3 phases. When the sintering temperature reaches 1450 °C, the Nb3Si phase is completely decomposed into Nbss and Nb5Si3 phases. Meanwhile, the microstructure coarsens significantly. Compared with the cast alloy, the HP alloy shows better mechanical properties. The fracture toughness of the alloy sintered at 1400 °C reaches 20.2 MPa·m1/2, which exceeds the application threshold. The main reason for the highest fracture toughness is attributed to the decomposition of large-sized brittle Nb3Si phase and the formation of a fine microstructure, which greatly increases the number of phase interfaces and improves the chance of crack deflection. In addition, the reduction in the size and content of silicides also reduces their plastic constraints on the ductile Nbss phase.

Microstructure characteristic, formation mechanism and mechanical properties of AZ91D/A356 bimetallic interface with a novel Ni-Cr composite coating

Microstructure characteristic, formation mechanism and mechanical properties of AZ91D/A356 bimetallic interface with a novel Ni-Cr composite coating

Spatiotemporal prediction of surface roughness evolution of C/C composites based on recurrent neural network

Carbon/carbon (C/C) composites are widely used in aerospace applications due to their excellent properties. Their surface roughness is an important factor affecting the material properties and ablation resistance, which is essential for the accurate prediction of the material. Images are often used to summarize and characterize microstructural features, which include information such as fiber microstructure and fiber orientations. An ablation shape evolution model based on optimization of attention mechanism, which combines multi-scale convolutional neural network (MSCNN) and long short-term memory (LSTM) methods for the C/C composites, is proposed. MSCNN encodes the microstructural information of the ablation image, which is fed into the LSTM model to extract the spatiotemporal features and long-term dependencies latent in the temporal law. The attention mechanism is used to assign different weights to the extracted features which makes the model focus more on the important time steps in the sequence. The results show that the proposed model achieves excellent effects in predicting the evolution of ablative morphology, with high agreement with the simulated values. The method saves time and cost, while providing an efficient and reliable method for the design and optimization of thermal protection materials.