Microstructural Variations Research Articles

Microstructural evolution in laser powder bed fusion of water-atomized high-carbon low-alloy steel: Analysis of melting mode effects

Medium/High‑carbon steels are considered susceptible to cracking during rapid cooling in laser powder bed fusion (LPBF) applications. Also, water-atomized (WA) steel powders, containing oxides, have been associated with porosity defects during this process. In this study, LPBF was employed to process WA high‑carbon low-alloy steel powders under three operational regimes – conduction, transition, and keyhole modes. Analyses based on the scaling law of keyhole stability, melt pool dimensions, and x-ray computed tomography (XCT) suggested that processing under the transition mode closely resembled a stable keyhole, enabling the successfully printing of water-atomized powders to a density of 99.93 %. Subsequent heat treatment, hardness, and residual stress assessments presented a prominent structural softening and relief of compressive stress under the transition mode. This was attributed to the intense in-situ tempering and re-austenitization that occurred within each layer. Under this condition, with no post heat treatment, an ultimate tensile strength of 1250 MPa with >2.6 % elongation was achieved. Finally, the ball-on-disk test showed that wear performance of the printed steels was primarily governed by the tribo-oxides, with a limited influence from the microstructural variation.

Conceptual design and properties of ultra-high residual strength geopolymer after 1000 ℃ thermal exposure

A novel geopolymer concrete is developed, incorporating waste ceramic aggregates, with ultra-high residual strength after exposure to elevated temperatures. Different aggregate volume fractions and particle size gradations are designed, and the variations in mass loss, volume shrinkage, compressive strength, mineral composition, and microstructure of geopolymer mortar after exposure to high temperatures ranging from 20 ℃ to 1000 ℃ are investigated by testing mass loss, volume change, strength, XRD and SEM. The results show that the waste ceramic aggregates (WCA) applied in the preparation of geopolymer mortars improve the mechanical properties and high-temperature resistance. By optimizing aggregate particle size gradation, the microstructure of the geopolymer mortar becomes denser and more homogeneous, and the high-temperature resistance is further improved. The residual compressive strength at 1000 °C is 115.2 MPa, 476 % higher than that of reference. These findings demonstrate the great potential of geopolymer mortars using ceramic aggregates with optimized gradation for high temperature resistant applications.

Comprehensive regulation of mechanical properties and thermal conductivity of Al-Si-Fe alloys through the mixed-additive (Sr and TiB2) strategy

It is of both scientific and technical significance to adjust the balance between the thermal conductivity and mechanical performance of Al-Si alloys. In this work, we proposed a strategy of using mixed-additive to perform such tuning. A permanent mold casting (PMC) was used to optimize the as-cast properties based on the orthogonal combination of Sr and TiB2. It is anticipated that the addition of Sr addition can modify the eutectic Si, while the addition of TiB2 can refine the primary α-Al dendrites, with uncertainty of its effects on the modification efficiency of Sr. The results showed that addition of TiB2 does not impair the modification efficiency of Sr. The optimized composition contained 200 ppm Sr and 300 ppm Ti. Casting specimens were then prepared using high-pressure die casting (HPDC) process. The results demonstrated that significant reduction in the size of β-AlFeSi, eutectic Si, and α-Al grains can be achieved by HPDC process. As a result, the tensile properties have been improved. The natural effects of HPDC process on the alloy, however, such as microstructure refinement and variation in porosity, leading to deduction in the thermal conductivity to 148.5 W/(m·K). This value still exceeds conventional alloys nevertheless.

Insight into the changes in active metabolite profiles of noni (Morinda citrifolia L.) fruit subjected to different drying treatments

Noni fruit is renowned for its abundance of bioactive compounds. Drying is an important method for processing functional products derived from noni. However, limited information exists on how drying methods affect the active metabolite profiles of noni fruit. This study investigated the impact of four common drying methods, including hot-air drying (HAD), vacuum freeze drying (VFD), microwave drying (MWD), and far infrared drying (FID), on the physicochemical indexes, bioactive components, and functional properties of dried noni fruit slices using targeted and untargeted metabonomics analysis. The results showed significant variations in appearance, water migration, and microstructure of dried noni fruit slices subjected to the four drying methods. VFD treatment yielded better dried noni fruit products when compared to other drying methods. The superiority of VFD treatment was due to its uniform stratification, reduced collapse, better retention of bioactive components and antioxidants, and higher enzyme inhibitory rates. These findings suggest that VFD method is ideal for obtaining premium bioactive profiles and maintaining the biological activity of noni fruit.

Quantifying the Impact of Microstructure Variation on Charging Capability in Lithium-Ion Batteries

Through the use of electrochemical simulations, variation in the local onset of lithium plating can be predicted and used to set charging guidelines to reduce the risk of lithium plating. The pseudo-two-dimensional (P2D) model is typically used for capturing this behavior; however, it only provides a global lithium plating onset estimate and does not consider the local variation. With material properties translated to an average continuum value, the P2D model can simulate rapid charge and capture global onset of lithium plating. However, this model lacks the ability to resolve localized behaviors across individual components due to local non-uniformities. Our three-dimensional microstructure-based (3DMS) modeling method that we employ to simulate rapid charge and capture local performance across the electrochemical components while agreeing with P2D model. Using the 3DMS model, we predict the onset of local lithium plating to design more conservative charging conditions to delay the onset of lithium plating and improve the performance of these electrochemical systems. In this work, several similar microstructures are evaluated for the lithium plating onset time during fast charge operation. A small normal distribution for particle sizes are explored to drive variation in performance and are compared to a uniform particle size structure.

Anisotropy of microstructure features and tensile properties of Ti–48Al–2Cr–2Nb alloy produced by electron beam powder bed fusion

A Ti–48Al–2Cr–2Nb alloy was produced by electron beam powder bed fusion. The effect of the volume energy density parameter on the forming quality was investigated, and the tissue characteristics, hardness distribution, and mechanical properties of the alloy were analyzed. The results showed that the quality was better when the volume energy density parameter was 21.5–22.5 J/mm3. The microstructure of the alloy has the phenomenon of changing with the forming height: with an increase in the forming height, the forming part produces the phenomenon of strip microstructure along the construction direction, and the regional microstructure variability occurs under the cross section of the same height. The average hardness of the alloy reached 375.2 HV at the bottom, 381.8 HV in the middle, and 389.6 HV at the top, and the standard errors of the hardness values were 12.40, 10.49, and 7.12 HV, respectively, with the microhardness showing a gradual increase along the molding direction, and the homogeneity was gradually better. The transverse tensile strength at room temperature reached 526 MPa, the yield strength reached 461 MPa, and the elongation at break reached 1.24%, while the longitudinal tensile strength reached 486 MPa, the yield strength reached 414 MPa, and the elongation at break reached 1.02%.

Gas tungsten arc welding of a multiphase CoCuxFeMnNi (x=20,30) high entropy alloy system: Microstructural differences and their consequences on mechanical performance

With the current advancements in materials science, the development of high entropy alloys (HEAs) is progressively increasing. Hence, research on their processability is essential to make them competitive alternatives to common engineering alloys that are widely used in structural applications. One manufacturing technique commonly employed in this sector is gas tungsten arc welding (GTAW). This technique allows to obtain single monolithic parts from separate components, often at the cost of local microstructural and mechanical properties variation across the joint. As such, GTAW processing is capable of supplying relevant knowledge regarding the feasibility of joining new materials and their potential industry uptake. In this study, we present a comparative analysis on the use of GTAW on two distinct multiphase high entropy alloys: CoCu20FeMnNi and the CoCu30FeMnNi. Firstly, microstructural observations coupled with CalPhaD-based calculations and synchrotron X-ray diffraction analysis, allowed to delve, and compare, the microstructural evolution across both welds. It was possible to observe the dual phase nature of the microstructure throughout the welded joint alongside the nucleation of a B2 BCC phase in the heat affected zone (HAZ) of both HEAs. Considering the mechanical properties of the welded materials, results evidenced a poorer, yet still acceptable mechanical performance. The observed decrease in mechanical strength is attributed to the residual stress conditions and large grain size that developed owing to the process thermal cycle, which contrasted deeply with the microstructure of each base material.

Investigating the low velocity impact response of additively manufactured tri-material composite structure with application on helmet

Additively manufactured composite structures can be utilized in the production of engineering materials with enhanced mechanical properties. In this work, mono-, bi-, and tri-material structures (MMS, BMS, and TMS, respectively) were fabricated using additively manufactured PLA (poly-lactic acid) lattice frames embedded with Polyurethane (PU) foam and milled glass fibers (MGFs). TMS samples were reinforced with MGFs at 1.25, 2.5, 3.75, and 5.0 vol%, indicated as TMS-1, TMS-2, TMS-3, and TMS-4, respectively. The mechanical response of these composite structures was tested by applying a low-velocity impact load. The effects of MGF content and variations in applied impact energy, and variation in microstructure on the composite samples were investigated. Results revealed an enhanced mechanical response of TMS samples compared to MMS and BMS. Additionally, with increasing applied impact energy, the TMS samples showed an improved corresponding response, with a peak absorbed energy of 96.03% of the applied 60 J energy. Furthermore, to study the applicability of the composite structures in real-life applications, helmet prototypes made of MMS, BMS, and TMS were designed and tested under the applied low-velocity load, showing an improved response of TMS helmet samples compared to the other composite structures.

Laser-based directed energy deposition and characterisation of cBN-reinforced NiAl-based coatings

Within this study, the alloy NiAl–2.5Ta–7.5Cr is investigated as a new matrix material for cBN-reinforced abrasive turbine blade tip coatings as currently used NiCoCrAlY matrix alloys suffer from insufficient strength at the high operating temperatures. Laser-based directed energy deposition with blown powder was applied to produce cBN reinforced NiAl-based coatings on monocrystalline CMSX-4 substrates. For this, powdery titanium-coated cBN and NiAl–2.5Ta–7.5Cr material were co-injected into the process zone to achieve an in situ formation of a NiAl–2.5Ta–7.5Cr/cBN composite. In order to overcome challenges such as cracking susceptibility, inductive preheating of the substrate up to 800 °C was used. Optical and scanning electron microscopy, energy dispersive X-ray spectroscopy, as well as electron backscatter diffraction were applied to analyse the fabricated samples’ microstructure. Additionally, the mechanical properties were evaluated by means of microhardness mappings. This work demonstrates the feasibility of in situ forming a metal matrix composite with a homogeneous distribution of cBN particles. The results show the beneficial effect of high-temperature preheating on the crack formation. However, the study also reveals challenges such as cracking induced by the injected cBN particles as well as severe intermixing of substrate and coating, which yields spatially resolved deviations in the chemical composition and resulting variations in microstructure and hardness.Graphical abstract

Evolution of microstructure, texture and formability of Al–Mg–Si alloys at different hot rolling finish temperatures

The impact of hot rolling finish temperature (HRFT) on the evolution of microstructure, texture, as well as formability—including deep drawability and bendability—of Al–Mg–Si alloy was studied in present work. The obtained results reveal that HRFT has a notable influence on the dynamic softening and dynamic precipitation behaviors during the hot rolling process of the investigated alloy. This leads to the volume fraction and number density of micro-sized Mg2Si particles increase as the increase of HRFT, those of nano-sized particles decrease, and the dislocation density decrease, in the hot-rolled sheets. These microstructural variations persist in the cold-rolled sheets, subsequently affecting the ultimate microstructure, texture, as well as formability of T4P sheets. The deep drawability improves as the HRFT rises, as indicated by the increase in normal anisotropy (r‾) and decrease in planar anisotropy (Δr). This is attributed to the weakening of texture intensity. The bendability, quantified by the minimum hemming factor (Rmin/t), deteriorates as the HRFT rises from 260 °C to 390 °C, attributed to the strengthening of P component along with the weakening of Cube component. Conversely, with the HRFT rises from 390 °C to 420 °C, the bendability improves dramatically due to the significant reduction in the average grain size. A combination of excellent deep drawability and bendability could be obtained by elevating the HRFT to 420 °C, attributed to the combined effect of weakened texture intensity and fine grains.

In-situ analysis of the effect of residual fcc phase and special grain boundaries on the deformation dynamics in pure cobalt

Polycrystalline hcp metals – an important class of engineering materials – typically exhibit complex plasticity because of a limited number of slip systems. Among these metals, deformation is even more complicated in cobalt as it commonly contains residual fcc phase due to the incomplete martensitic fcc→hcp transformation upon cooling. In this work, we employ a combination of in-situ (acoustic emission, AE) and ex-situ (scanning electron microscopy, SEM) techniques in order to examine deformation dynamics in pure polycrystalline cobalt varying in grain size and the content of residual fcc phase prepared using systematic thermal treatment and cycling. We reveal that the presence of the fcc phase and special ∼71∘ grain boundaries between different hcp martensite variants brings about higher deformability and strength. The fcc phase provides additional slip systems and also accommodates deformation via the stress-induced fcc→hcp transformation during loading. On the other hand, special boundaries enhance structural integrity and suppress the formation of critical defects. Both these non-trivial effects can dominate over the influence of grain size, being a traditional microstructural variable. The ex-situ SEM experiments further reveal that the stress-induced fcc→hcp transformation is sluggish and only partial even at high strains, and it does not give rise to detectable AE signals, unlike in other materials exhibiting martensitic transformation. In turn, these insights into cobalt plasticity provide new avenues for the microstructure and performance optimization towards the desired applications through the modern concept of grain boundary engineering.

Sex-related variability of white matter tracts in the whole HCP cohort

Behavioral differences between men and women have been studied extensively, as have differences in brain anatomy. However, most studies have focused on differences in gray matter, while white matter has been much less studied. We conducted a comprehensive study of 77 deep white matter tracts to analyze their volumetric and microstructural variability between men and women in the full Human Connectome Project (HCP) cohort of 1065 healthy individuals aged 22–35 years. We found a significant difference in total brain volume between men and women (+ 12.6% in men), consistent with the literature. 16 tracts showed significant volumetric differences between men and women, one of which stood out due to a larger effect size: the corpus callosum genu, which was larger in women (+ 7.3% in women, p = 5.76 × 10–19). In addition, we found several differences in microstructural parameters between men and women, both using standard Diffusion Tensor Imaging (DTI) parameters and more complex microstructural parameters from the Neurite Orientation Dispersion and Density Imaging (NODDI) model, with the tracts showing the greatest differences belonging to motor (cortico-spinal tracts, cortico-cerebellar tracts) or limbic (cingulum, fornix, thalamo-temporal radiations) systems. These microstructural differences may be related to known behavioral differences between the sexes in timed motor performance, aggressiveness/impulsivity, and social cognition.

The use of nonlinear guided-wave features for detection and assessment of intermetallic compounds within dissimilar joints – an experimental investigation

Abstract Welding dissimilar materials is widely employed in industrial construction and manufacturing to enhance cost-effectiveness and performance, often utilizing non-fusion methods like solid-state and high-energy beam welding. However, a significant challenge is the formation of intermetallic compounds (IMCs) at the joint interface, which can weaken the bond and increase brittleness, leading to hidden internal cracks. Nonlinear ultrasound detection methods are employed as advanced, non-destructive testing techniques for early damage inspection in various materials. This research investigates the assessment of the thickness of the intermetallic layer within dissimilar joints using non-linear ultrasound-wave features. Numerical and experimental investigations were performed using four friction stir welding (FSW) lap joints, between AA5052-H32 aluminum and ASTM 516-70 steel, with various intermetallic thicknesses. The methodology involved examining the generation of second-order harmonic frequency by exciting Lamb waves (LW) at specific frequencies. To determine the necessary LWs' excitation frequency, synchronism, and non-zero power flux conditions were employed. The collected signals were measured and analyzed in the time and frequency domains to understand the behavior of the non-linear parameter β′ with the thickness of the intermetallic layer. The results show that β′ changes in a linear manner with the thickness of the intermetallic compound layer (several micrometers in thickness). This provides strong evidence that nonlinear LW features are sensitive to microstructural variations in the FSW joints, which enables them to effectively evaluate their strength.

Characterization of the microstructural, magnetic, and thermal behaviors of boron-doped Fe–Co–Ni alloys produced via mechanical alloying

FeCoNi alloys, both doped and undoped, were synthesized into nanocrystalline forms using a high-energy mechanical milling technique. The study used the x-ray diffraction technique to examine the microstructure characteristics of powder materials. The identified patterns were examined using Maud software. It was found that mechanical alloying produced solid solutions with BCC and FCC structures and crystallite sizes in the range of 25 nm after 100h of milling. The BCC-Fe(Co,Ni,B) and orthorhombic-Fe3B phases were refined for the alloy doped with amorphous boron, while only the bcc-Fe(Co,Ni,B) phase was identified for the alloy doped with crystalline boron. Meanwhile, the FeCoNi alloy revealed a mixture of FCC-Co and BCC-FeCoNi phases. This sample has a soft ferromagnetic behavior, whereas the doped ones have hard ferromagnetic behaviors. The squareness ratios (Mr/Ms) are typically low. The microstructural variations were associated with magnetic characteristics. The thermal stability of the alloyed powder mixtures was investigated by the DSC technique from 25 to 700 °C for 2h. The alloyed samples were first annealed at selected temperatures and then analyzed using x-ray diffraction. The obtained x-ray diffraction results proved that at temperatures below 230 °C, the initial heavy deformed structure’s structural relaxation followed by the recrystallization of the fcc-Co phase and, at higher temperatures, the recrystallization of new phases, such as α-FeCo, fcc-FeNi, fcc-Ni3Fe, and borides of the (FeNi)23B6, -(FeCo)23B6 types. The stability of the crystalline phases that are formed and their magnetic characteristics can be regulated through a carefully calibrated annealing process.

Comparative analysis of experimental techniques for microstructural characterization of novel nanostructured aluminium alloys

Precipitation holds a pivotal role in comprehending the intrinsic behavior of materials. In the design of nanostructured metallic alloys, precipitates have found to increase the alloys' stability and response under extreme environmental conditions. Studies on precipitation often rely on conventional and ex situ electron-microscopy methods, but a systematic investigation that compares different sample conditions during heat treatment and its microstructural implications are rarely available. In this context, we employed a novel ultrafine-grained AlMgZnCuAg crossover alloy to compare three distinct conditions for investigating the precipitation sequence: (i) ex situ transmission electron microscopy (TEM) from bulk heating, (ii) ex situ TEM from TEM foil heating, and (iii) in situ TEM with microelectromechanical-system (MEMS) heating. Although the heat treatment procedure was consistent across all cases studied, the application of these three different experimental conditions in the same alloy system resulted in significant and non-negligible differences in the final precipitation behavior. Ultimately, it resulted in observable microstructural variations and precipitates with distinctively different shape and sizes and, as a result, we outline herein the major similarities and differences among these techniques to achieve comparable results. This knowledge will help to compare and assess results of precipitation sequences obtained in different conditions.

A two-scale approach for assessing the role of defects in fatigue crack nucleation in metallic structures

Metal structures often exhibit macroscopic defects from which cracks can nucleate during cyclic loading. The current work presents a two-scale approach to enable the prediction of crack nucleation from such defects by taking into account local microstructure features. The geometrical description of the defect and associated non-homogeneous strain fields are modeled using a macroscale model which employs a continuum elastoplastic material model for cyclic deformation. The cyclic deformation of the microstructure near the defect is modeled using a mesoscale model which employs a crystal plasticity material model and uses multiple realizations to address the statistical microstructure variability. The boundary conditions of the mesoscale model are extracted from the macroscale model. By simulating the deformation of the microstructure using the strain fields near the defect and by introducing a fatigue indicator parameter for crack nucleation, along with the weakest-link based upscaling methodology, the developed approach enables the prediction of the distribution of crack nucleation life. The approach is used for analyzing different defects for crack nucleation by considering local grain orientations. The predictions are shown to not only capture phenomena such as scatter, size effects, etc. qualitatively, but also agree with a classical engineering approach and experimentally reported data sets quantitatively.

An approach for identifying the deformation-induced strain from tensile tests and x-ray diffraction measurements

ABSTRACT Non-uniform plastic deformation and phase transformation introduce residual stress (RS) in a material. The present study focuses on the influence of tensile strain on RS development in 304L austenitic stainless steel, wherein strain-induced martensite (SIM) transformation influences deformation behaviour. Room temperature tensile tests were interrupted at various tensile strains between the material yield and ultimate tensile strength at 5.21 × 10−4 and 1.3 × 10−2 s−1 strain rates. Microstructural characterisation of as-received and deformed samples by electron backscatter diffraction provides evidence of SIM formation and shear bands. Analysis of tensile flow and work hardening behaviour is discussed in correlation to the microstructural and dislocation density variations. In addition, RS in the austenite and martensite phases was measured using the x-ray diffraction method, and the RS balance that occurs between the longitudinal and transverse components and the two phases after tensile deformation is presented. It is shown that a combined analysis of RS and x-ray diffraction peak width could be utilised to find the deformation level in tensile fractured, press brake bent, and roll bent samples.

Multi deep learning-based stochastic microstructure reconstruction and high-fidelity micromechanics simulation of time-dependent ceramic matrix composite response

A multi deep learning-based framework is developed for efficient, automated microstructure reconstruction and generation of stochastic representative volume elements (SRVEs) with periodic boundary conditions (PBCs) for accurate modeling of ceramic matrix composite (CMC) response. The methodology comprises a convolutional neural network coupled with regression layers to act as a vanilla regression network for semantic segmentation of the microstructure, allowing accurate characterization of the phases and their distributions at the microscale. Scanning electron microscope and confocal microscope are used to obtain C/SiNC and SiC/SiNC CMCs micrographs for vanilla regression testing. Microstructure variability in terms of fiber volume fraction and porosity are quantified through the output regression layer, ensuring accurate representation of material variability in SRVE construction. Generative adversarial network (GAN) and its variants are designed to produce high-fidelity SRVE, spanning CMCs microstructure variability space. A circular padding algorithm is developed to generate SRVEs with PBCs during training of GANs. The accuracy of the generated SRVEs is established through micromechanics simulations, where an efficient formulation of the high-fidelity generalized methods of cells (HFGMC) approach is used to compute the effective mechanical properties. An iterative algorithm is implemented in the HFGMC solver to simulate time-dependent deformation of SiC/SiNC subjected to creep loading conditions.

Microstructural and optoelectronic properties of sputtered Al:ZnO films and Al:ZnO/Cu bilayer structures: Effects of substrate and Cu thickness

In this study, using a multi-source confocal radio frequency magnetron sputtering system, we synthesized aluminum doped zinc oxide (AZO) single layers and AZO/Cu bilayers on glass and crystalline quartz substrates with a constant AZO thickness of 65 nm and variable Cu bottom layers with a thickness of 4–13 nm. The microstructural, morphological, optical, and electrical characteristics of all samples were investigated using a variety of spectroscopic techniques. The X-ray diffraction results show that all films prepared on both substrates have a hexagonal wurtzite crystal structure and exhibit the preferred orientation along the (002) plane with some microstructural variations. The atomic force microscopy images revealed that the thickness of the Cu layer and substrate type greatly affect the films' topography and surface roughness. The transmittance spectra indicate that the single AZO layer on both substrates possess the highest average visible transmission; however, all the samples deposited on glass substrates show greater transmittance than that on quartz. Photoluminescence analysis put into evidence a decrease in ultraviolet emission with Cu thickness for both substrates, with intensities varying according to substrate type. Hall Effect measurements reveal that all samples have n-type conductivity as well as that Cu thickness has a significant impact on their electrical characteristics. Moreover, a higher value of the figure of merit is achieved with the AZO/Cu bilayer structure grown on a glass substrate with 13 nm of Cu layer thickness.

Prediction of martensitic transformation and residual stress field on 17–4 PH stainless steel fabricated by laser powder bed fusion

The 17–4 precipitation-hardened (PH) alloy can be printed into diverse microstructures. Existing reports on the alloy have focused on the effect of Creq/Nieq ratios and the processing parameters of laser powder bed fusion (LPBF) on the final microstructures of the δ-ferrite and α’-martensite phases in the alloy. However, the effect of microstructural variations on the residual stress field of LPBFed 17–4 PH stainless steel has not yet been investigated. This study bridges the gap between what is known about the microstructure and residual stresses by proposing an alloy-equivalent phase prediction diagram for the additive manufacturing of the 17–4 PH alloy by varying the Creq/Nieq ratio and volumetric energy density to control residual stresses via microstructure manipulation. Dilatometry and Satoh tests were performed to elucidate the mechanism of the offset effect in martensite transformation. To control the microstructures, samples were fabricated with various Creq/Nieq ratios (2.05, 2.15, 2.30, and 2.49) and laser powers (130, 150, 170, and 190 W). The 17–4 PH alloy exhibited a low Ms temperature and approximately net zero residual stresses in the Satoh test. The study confirmed that martensitic transformation, which occurs more readily at lower Creq/Nieq ratios and higher laser powers, effectively offsets tensile residual stresses during the LPBF process.