Microstructural Analysis Research Articles

Sol-Gel Derived Alumina Particles for the Reinforcement of Copper Films on Brass Substrates.

The aim of this study is to provide tailored alumina particles suitable for reinforcing the metal matrix film. The sol-gel method was chosen to prepare particles of submicron size and to control crystal structure by calcination. In this study, copper-based metal matrix composite (MMC) films are developed on brass substrates with different electrodeposition times and alumina concentrations. Scanning electron microscopy (FE-SEM) with energy-dispersive spectroscopy (EDS), TEM, and X-ray diffraction (XRD) were used to characterize the reinforcing phase. The MMC Cu-Al2O3 films were synthesized electrochemically using the co-electrodeposition method. Microstructural and topographical analyses of pure (alumina-free) Cu films and the Cu films with incorporated Al2O3 particles were performed using FE-SEM/EDS and AFM, respectively. Hardness and adhesion resistance were investigated using the Vickers microindentation test and evaluated by applying the Chen-Gao (C-G) mathematical model. The sessile drop method was used for measuring contact angles for water. The microhardness and adhesion of the MMC Cu-Al2O3 films are improved when Al2O3 is added. The concentration of alumina particles in the electrolyte correlates with an increase in absolute film hardness in the way that 1.0 wt.% of alumina in electrolytes results in a 9.96% increase compared to the pure copper film, and the improvement is maximal in the film obtained from electrolytes containing 3.0 wt.% alumina giving the film 2.128 GPa, a 134% hardness value of that of the pure copper film. The surface roughness of the MMC film increased from 2.8 to 6.9 times compared to the Cu film without particles. The decrease in the water contact angle of Cu films with incorporated alumina particles relative to the pure Cu films was from 84.94° to 58.78°.

Development of Cost-Effective Sn-Free Al-Bi-Fe Alloys for Efficient Onboard Hydrogen Production through Al–Water Reaction

Leveraging the liquid-phase immiscibility effect and phase diagram calculations, a sequence of alloy powders with varying Fe content was designed and fabricated utilizing the gas atomization method. Microstructural characterizations, employing SEM, EDS, and XRD analyses, revealed the successful formation of an incomplete shell on the surfaces of Al-Bi-Fe powders, obviating the need for Sn doping. This study systematically investigated the microstructure, hydrolysis performance, and hydrolysis process of these alloys in deionized water. Notably, Al-10Bi-7Fe exhibited the highest hydrogen production, reaching 961.0 NmL/g, while Al-10Bi-10Fe demonstrated the peak conversion rate at 92.99%. The hydrolysis activation energy of each Al-Bi-Fe alloy powder was calculated using the Arrhenius equation, indicating that a reduction in activation energy was achieved through Fe doping.

Corrosion resistance analysis of Al2O3-TiO2 composite ceramic coatings on carbon steel pipe surfaces

This study investigates the corrosion resistance of Al2O3-TiO2 composite coatings reinforced with multi-walled carbon nanotubes (MWCNTs) on carbon steel pipe surfaces. Coatings were deposited using atmospheric plasma spraying (APS) and high velocity oxy-fuel (HVOF) techniques. Microstructural analysis revealed that HVOF-sprayed coatings exhibited denser and more homogeneous structures compared to APS-sprayed coatings. Electrochemical tests in 3.5 wt% NaCl solution showed that the HVOF-sprayed Al2O3-13 wt% TiO2-1.5 wt% MWCNT coating demonstrated the lowest corrosion current density of 7.6 × 10−9 A/cm2 and the most positive corrosion potential. Hot corrosion tests in a simulated boiler environment (500°C, 1000 h) revealed that this coating also exhibited minimal weight gain (0.9 mg/cm2) and thickness loss (2 μm). The corrosion rate of the optimal coating was 0.05 mm/year, significantly lower than the bare carbon steel (2.45 mm/year). XRD analysis of corroded samples showed that HVOF-sprayed coatings maintained their original phase composition without detectable substrate corrosion products. The superior corrosion resistance of the HVOF-sprayed Al2O3-13 wt% TiO2-1.5 wt% MWCNT coating is attributed to its optimized composition, dense microstructure, and the reinforcing effect of MWCNTs. These findings provide valuable insights for developing advanced coating solutions to mitigate corrosion-related challenges in the oil and gas industry and other harsh industrial environments.

Effect of multidirectional forging on grain structure and mechanical properties of hypereutectic Al–20%Si alloys with added refiners and modifiers

ABSTRACT The present work is focused on the multidirectional forging (MDF) of Al–20 wt-% Si alloys with the addition of refiners and modifiers. The MDF process was performed at 200°C with a cumulative strain of 0.63. Microstructural characterization and mechanical performance were evaluated on the Al–20Si, Al–20Si–4.5Cu, Al–20Si–4.5Cu–1(Al–Ti–B), Al–20Si–4.5Cu–1(Al–Ti–B)–10(Al–Sr). The microstructure analysis revealed significant changes in the eutectic and primary phase refinement. The micro-Vickers hardness confirmed that the MDF process resulted in increased hardness (125 ± 1.9 VHN) compared to the homogenized samples (96 ± 2.7 VHN). Tensile test results showed that with the accumulation of strain, ultimate tensile strength increased to 435 MPa from 302 MPa with reduction in the percentage of elongation from 7.8 to 5.6. The grains were more uniformly distributed with addition of modifiers, and refiners further reduced the nucleation number of eutectic grains. The wear study demonstrated that the wear resistance is more in the Al–Si-Cu-Sr sample due to the increased level of hardness. The combination of multidirectional forging techniques with judicious incorporation of refiners and modifiers engenders a synergistic enhancement of microstructural integrity, hardness profiles, and wear-resistant properties in hypereutectic Al-20Si alloys.

Manufacturing and mechanical performance of lightened gypsum reinforced by hemp/epoxy composites

In recent years, the construction industry has increasingly focused on reducing its environmental impact, addressing research efforts towards innovative materials and technological solutions. In this context, gypsum-based materials and natural fibers represent some of the most promising alternatives in terms of sustainability. This paper aims to propose a new gypsum structure reinforced with a composite hemp fabric impregnated with epoxy resin, investigating its manufacturing process and the mechanical properties, specifically in terms of flexural, impact and bearing strength. To achieve lightweight structures, lightened gypsum was also considered in addition to conventional gypsum. Both the lightened gypsum matrix and the hemp/epoxy reinforcement were produced using specific techniques able to obtain lightweight gypsum composites. Beneficial effects in the use of lightened gypsum matrix were found indeed, the reinforced lightweight samples exhibited higher values of flexural strength coupled with a density reduction of about 18%. Additionally, a significant change in post-cracking behavior was observed, with a gradual failure rather than a brittle one. The same trend was observed for the impact, while for bearing strength, the presence of porosity affected negatively the resistance of the composites, prevailing over the benefits of density reduction. Experimental results demonstrated the presence of a good interaction between the hemp fabric and the gypsum matrix, which was further confirmed by the microstructure analysis. The interesting mechanical properties showed by these lightweight gypsum/hemp composites, suggested their possible use for different and unconventional applications of gypsum-based walls and components.

Prediction of Mechanical Properties of Rare-Earth Magnesium Alloys Based on Convolutional Neural Networks.

Rare-earth magnesium alloys exhibit higher comprehensive mechanical properties compared to other series of magnesium alloys, effectively expanding their applications in aerospace, weapons, and other fields. In this work, the tensile strength, yield strength, and elongation of a Mg-Gd-Y-Zn-Zr rare-earth magnesium alloy under different process conditions were determined, and a large number of microstructure observations and analyses were carried out for the tensile specimens; a prediction model of the corresponding mechanical properties was established by using a convolutional neural network (CNN), in which the metallographic diagram of the rare-earth magnesium alloy was taken as the input, and the corresponding tensile strength, yield strength, elongation, and three mechanical properties were taken as the output. The stochastic gradient descent (SGD) algorithm was used for parameter optimization and experimental validation, and the results showed that the average relative errors of the tensile strength and yield strength prediction results were 1.90% and 3.14%, respectively, which were smaller than the expected error of 5%.

Static and dynamic mechanical properties of aluminum nitride-silicon carbide whisker composites

AlN composites reinforced with SiC whiskers and Y2O3 sintering aids were fabricated using the hot-pressing technique to investigate static and dynamic mechanical properties. Microstructure analysis revealed that increasing SiC whisker content yielded grain refinement and decreasing relative density. The Vickers hardness increased from 10.29 to 14.47 GPa, while the fracture toughness improved from 3.03 to 4.39 MPa·m1/2 with 30 wt% SiC whiskers. A numerical approach for evaluating the dynamic modulus and loss factor is presented utilizing the wave propagation characteristics. The dynamic properties showed decreasing dynamic modulus and increasing loss factor with higher SiC content, attributed to increased porosity and interphase boundaries. Thermal conductivity, however, decreased from 139.53 to 49.95 W/m·K as SiC whisker content increased, primarily due to enhanced phonon scattering at grain and interphase boundaries. These findings suggest that AlN-SiCw composites are promising candidates for heat dissipation ceramic substrates, which offer superior mechanical strength and reliable thermal management.

TECHNO-FUNCTIONAL PROPERTIES OF CHICKPEA PROTEIN ISOLATE-TREATED ACIDIC AND BASIC PH-CYCLING

This study examined the impact of extreme pH-cycling treatments on chickpea protein isolate (CPI). Untreated CPI, along with samples shifted to pH 2 (pH2) and pH 12 (pH12), displayed solubilities of 60.25%, 25.01%, and 75.48%, respectively. Both treatments significantly improved water and oil absorption capacities. Emulsion activity and stability for CPI at pH2 and pH12 were 125 m2/g and 110 m2/g, respectively, versus 75 m2/g for the untreated sample. Notably, the foaming capacity and stability of pH12-treated CPI increased by 3.5 and 8.8 times, respectively, compared to the untreated protein. pH12-treated CPI also demonstrated the lowest gelling concentration at 10%, compared to 14% and 18% for untreated and pH2-treated CPI, respectively. Microstructural analysis revealed partial disintegration of CPI under pH-cycling, underscoring that alkaline pH12-shifting notably enhances functional properties of CPI.

Ultrastructural evaluation of adverse effects on dentine formation from systemic fluoride application in an experimental mouse model.

Fluoride is widely used in dentistry for its caries prevention. To reduce dental caries, the optimal fluoride concentration of public water supplies in the United States is 0.7 ppm. However, excessive systemic fluoride consumption can lead to dental/enamel fluorosis. Numerous studies have explored the effects of fluoride on enamel and enamel-forming cells. However, research on systemic fluoride's impact on dentine is limited, particularly the effect of fluoride on the structure of the dentine-pulp complex. Therefore, this study aimed to identify how excessive fluoride affects dentine microstructure using an experimental mouse model. C57BL6/J male mice (6-9 weeks old) were randomized into four groups (Fluoride at 0, 50, 100, or 125 ppm in drinking water) (n = 4/group). Mice were provided water adlibitum for 6 weeks along with fluoride-free food. Thereafter, mandibular incisors were analysed. Enamel phenotypes were evaluated using light microscopy and quantitative light-induced fluorescence (QLF) to measure fluorosis levels. Dentine morphology was evaluated using micro-CT, scanning electron microscopy (SEM), SEM-EDX (energy-dispersive X-ray), microhardness test and histological imaging. Data were analysed using one-way ANOVA with Dunnett's multiple comparisons as a post hoc test and the Kruskal-Wallis test with Dunn's multiple comparisons post hoc test (p < .05). Mice treated with fluoride at 50-125 ppm developed enamel hypoplasia in their erupting incisors and micro-CT imaging revealed that fluoride 125 ppm caused external resorption of the growing incisor. Dentine mineral density, dentine volume decreased compared with the 0 ppm control, while pulp volume increased compared with the 0 ppm control group. SEM showed wider predentine layer and abnormalities in calcified matrix vesicles derived from odontoblasts in fluoride 100 and 125 ppm groups. Vickers microhardness of dentine significantly decreased in the high-dose group. Fluoride-induced dentine hypoplasia in a dose-dependent manner. Histological evaluation showed excessive fluoride 125 ppm induced micro abscess formation and inflammatory cell infiltration. Fluoride induced dentine dysplasia with a dentine microstructure resembling hypophosphatasia. High doses of systemic fluoride can cause dentine dysplasia. Both three-dimensional and microstructural analyses showed the structural, chemical and mechanical changes in the dentine and the mineralized tissue components, along with external resorption and pulp inflammation.

Modulating the rejuvenation in a Al75Mg25 metallic glass by multiple recovery annealing treatment

Rejuvenation presents a promising way to improve the plasticity of metallic glasses. How modulating the degree of rejuvenation of metallic glasses remains a challenging issue. Here, based on the molecular dynamics simulation, we investigate the evolution of the structural and mechanical properties of a binary Al75Mg25 metallic glass and successfully realized the rejuvenation modulation through the multiple recovery annealing treatment. A range of samples with different degrees of rejuvenation were obtained by successive multiple recovery annealing process. According to our calculations, we found that the degree of rejuvenation is highly correlated with the Al-centered clusters. Microstructural analyses show that a higher degree of rejuvenation is concomitant with less 1551 index of Honeycutt-Andersen indices and a lower content of <0,0,12,0 > in terms of Voronoi Tessellation analysis. Moreover, our calculated results demonstrate that the samples with the aging initial state show a higher degree of rejuvenation as compared to the samples with the rejuvenated initial state. This can be attributed to that there are more icosahedral clusters, which are more likely to change to other types of clusters with low local fivefold symmetry in the aged samples during the subsequent high-temperature annealing process. Our work confirms that proper multiple (no more than three times) recovery annealing treatment can increase the degree of rejuvenation of metallic glasses and can offer a better understanding of the effect of rejuvenation on the microstructures and mechanical properties of metallic glasses.

Investigation of Mechanical Properties and Microstructure Analysis of 5356 Al Alloy Thin Plate and Block Fabricated by Directed Energy Deposition-Arc

Investigation of Mechanical Properties and Microstructure Analysis of 5356 Al Alloy Thin Plate and Block Fabricated by Directed Energy Deposition-Arc

Temperature dependence of the deformation behavior and mechanical properties of a Fe–Mn–Al–C low-density steel for cryogenic application

The temperature dependence of the deformation behavior and mechanical properties of a Fe–20Mn–6Al-0.6C-0.15Si austenitic low-density steel was studied by tensile test and Charpy impact test at −196 °C, −77 °C and room temperature (RT), followed by microstructure analyses. The results indicate that the decreased tensile temperature, which is corresponding to reduced stacking fault energy (SFE), promotes the planar glide of dislocations. This led to larger fraction of low-angle grain boundaries (LAGBs) at lower tensile temperature. Consequently, both the tensile strength and elongation were improved as temperature decreased. At lower impact test temperature, the load and energy of crack initiation were larger, indicating a higher resistance to crack initiation. However, the transition from stable to unstable crack propagation occurred more rapidly at lower temperature, resulting in lower crack propagation energy and reduced resistance to crack propagation. This is because less region experienced planar glide. Due to the rapid unstable crack propagation, the Charpy absorbed energy at −196 °C was the lowest. The smaller fracture surface area, larger fibrous zone and more obvious ductile fracture characteristics in radial zone suggest that the toughness is better at higher temperature. Additionally, the presence of secondary cracks at RT delayed fracture, therefore benefitting toughness.

Macro-micro deformation mechanism of tantalum‑tungsten alloy flyer under explosive loading

This study investigates the macro-micro deformation mechanism of tantalum and tantalum‑tungsten alloys under extreme rate loading. Flyers with varying tungsten contents (0 wt%, 2.5 wt%, 5 wt%, 7.5 wt%, 10 wt%) and different texture were subjected to explosive loading tests. Molding and penetration capabilities of the flyers were comprehensively assessed by the mild-steel witness plate, recovered penetrator and plug. Tantalum‑tungsten alloys with 10 wt% tungsten were crushed, forming discrete holes on witness plate, while those flyers with 0 wt%, 2.5 wt%, 5 wt%, and 7.5 wt% tungsten content formed complete circular perforations on the witness plate. Recovered penetrators and plugs indicated partial fracture of pure tantalum. The increased tungsten content in the alloy enhances the penetration stability and recovery integrity of the penetrator, while simultaneously reducing dynamic plastic deformation. Microstructural analysis via Electron Back Scatter Diffraction (EBSD) revealed a robust {111}//Z axial texture at impact side of the penetrator, which weakened with increasing tungsten content; While un-impacted side showed a {110}//Z axial texture. And uniform equiaxial crystalline structures outperformed long strip grain structures subjected. Therefore, the alloys' molding abilities and penetration stabilities ranked as Ta2.5 W > Ta5W > Ta&Ta7.5 W > Ta10W. These findings provide a foundation for the application of tantalum and tantalum‑tungsten alloys under explosive loading.

Correlation of microstructure and magnetic softness of Si-microalloying FeNiBCuSi nanocrystalline alloy revealed by nanoindentation

Abstract Compared to the commercial soft-magnetic alloys, the high saturation magnetic flux density (B s) and low coercivity (H c) of post-developed novel nanocrystalline alloys tend to realize the miniaturization and lightweight of electronic products, thus attracting great attention. In this work, we designed a new FeNiBCuSi formulation with a novel atomic ratio, and the microstructure evolution and magnetic softness were investigated. Microstructure analysis revealed that the amount of Si prompted the differential chemical fluctuations of Cu element, favoring the different nucleation and growth processes of α-Fe nanocrystals. Furthermore, microstructural defects associated with chemical heterogeneities were unveiled using the Maxwell-Voigt model with two Kelvin units and one Maxwell unit based on creeping analysis by nanoindentation. The defect, with respect to a long relaxation time in relaxation spectra, was more likely to induce the formation of crystal nucleus that ultimately evolved into the α-Fe nanocrystals. As a result, Fe84Ni2B12.5Cu1Si0.5 alloy with refined uniform nanocrystalline microstructure exhibited excellent magnetic softness, including a high B s of 1.79 T and very low H c of 2.8 A/m. Our finding offers new insight into the influence of activated defects associated with chemical heterogeneities on microstructures of nanocrystalline alloy with excellent magnetic softness.

Synchrotron X-ray radiation study of retained austenite stability and the effect on fatigue behavior of bainitic railway steels

The effect of retained austenite stability on the fatigue performance was studied in bainitic rail steel subjected to different heat treatments, including normalizing at 900 °C and normalizing at 900 °C combined with tempering at 320 °C. The normalized steel had yield strength of 851 MPa, tensile strength of 1131 MPa, uniform elongation 7.0 %, and total elongation 17.5 %. Tempering the steel at 320 °C resulted in similar strength and plasticity compared to the normalized condition. However, the fatigue performance of steel was improved significantly after tempering. The ultimate fatigue stress (endurance limit) after 1 × 107 cycles was 671 MPa, which was 38 MPa greater than the normalized steel. Microstructural analysis revealed similarities between normalized and tempered matrices at crystallographic interfaces and grain boundaries. Synchrotron X-ray radiation indicated that the initial retained austenite content was ∼15.5 % in both normalized and tempered conditions. However, at tensile stress of 800 MPa, the amount of retained austenite transformed in the normalized steel was ∼4 %, which was twice that of the tempered steel. The enhancement of retained austenite stability was an important aspect in improving the fatigue performance. The analysis of interphase spacing showed that the strain in the normalized matrix synchronized with the retained austenite, and the stress was concentrated in the retained austenite, which promoted transformation of retained austenite. The matrix of tempered steel was strained first, which prevented stress concentration in the retained austenite and rendered the retained austenite stable.

High-silicon spring steel transformation to carbide-free bainitic (CFB) steel: a mechanical and tribological approach under rolling/sliding conditions

The present study concentrates on the development of carbide-free bainite steel and explores its tribological and mechanical characteristics using a newly devised disk-on-disk tribometer. The microstructure of the treated samples was examined through heat treatment at various holding temperatures (300, 350, and 400 °C) and durations (10, 20, and 30 min), along with isothermal transformation. The wear rate demonstrated significant sensitivity to holding duration, transformation temperature, phase fraction, and the stability of retained austenite. The microstructural analysis encompassed atomic force microscopy (AFM), FE-SEM, x-ray diffraction (XRD), and energy-dispersive x-ray spectroscopy (EDS). The study extensively investigated the robust correlation among mechanical properties, microstructure, wear behavior, and the presence of retained austenite (RA) and bainite volume fraction. The findings indicate that carbide-free bainite steel holds promise for replacing conventional railway wheel track steel in the steel industry. The structural property correlations have developed of high silicon steel, hardness reduced with increasing temperature and isothermal preserving time; resulting in a gradual increase in the wear rate of CFB steel. The salt bath soaking temperature of 350 °C with a period of 30 min was found to be the preeminent wear properties condition for CBF steel.

Effect of heat treatment on the microstructure and mechanical properties of AZ91D magnesium alloy fabricated via GTA wire arc additive manufacturing

This study aims to address elemental segregation and poor mechanical properties in as-deposited AZ91D magnesium alloy fabricated via wire arc additive manufacturing through heat treatment. Three distinct heat treatments are investigated: solution treatment (T4), artificial aging treatment (T5), and a combination of solution and aging treatment (T6). Microstructural analysis reveals equiaxed grains in all samples. In the T4 state, the eutectic phase along grain boundaries dissolvs into the matrix, reducing elemental segregation but increasing grain size. In the T5 state, elemental segregation is further reduced; however, due to the relatively low aging temperature, the microstructural features of the as-deposited state are largely retained. In the T6 state, solution treatment increases grain sizes, and the uneven distribution of the reprecipitated β phase leads variations in mechanical properties between vertical and horizontal directions. Compared to the as-deposited state, the T6 treatment achieves a synergistic improvement in both strength and ductility. The ultimate tensile strength increases to 262.3 MPa, and the elongation rises to 13.8%, representing improvements of 12.5% and 32.7%, respectively, compared to the as-deposited values of 233.2 MPa and 10.4%.

Microstructural Analysis, Tribological, and Corrosion Behavior of Nix-Tiy Alloys Deposited Using µ-Plasma Additive Manufacturing Process

Microstructural Analysis, Tribological, and Corrosion Behavior of Nix-Tiy Alloys Deposited Using µ-Plasma Additive Manufacturing Process

Effect of Pressure on the Linear Friction Welding of a Tool Steel and a Low‐Alloy Carbon Steel

This study investigates the effect of pressure (burn‐off and forging) on the mechanical properties of the joint between a wear‐resistant tool steel and a low‐alloy steel using linear friction welding. The authors have previously demonstrated the feasibility of joining these dissimilar materials, but the impact of pressure on the mechanical properties of the bimaterial joint remains unclear. To address this, weld samples are prepared using different pressures and are characterized through microstructural analysis, microhardness, tensile testing, and fractography. The results show that the strength of the joint between the wear‐resistant tool steel and the low‐alloy carbon steel increases as the pressure increases up to a certain point, after which a decrease is observed. The highest joint strength is achieved at a pressure of 360 MPa. The microhardness profile measurement reveals a distinct transition zone at the interface between the two materials, with varying hardness values. The hardness of the low‐alloy carbon steel increases near the interface, while that of the wear‐resistant tool steel decreases. This transition zone is found to be narrower at higher pressures. Microstructural characterization shows that the grain structure near the interface differs from that of the starting base materials.

Comparative Microstructure Characteristics of Synthesized PbS Nanocrystals and Galena

Lead sulfide (PbS) on the nanoscale was synthesized via a chemical route at room temperature using lead nitrate {Pb(NO3)2} and sodium sulfide (Na2S). The Na2S was prepared at ~105 °C using sodium hydroxide (NaOH) and sulfur (S) powder. The produced PbS, denoted as Lab-PbS, was compared with a high-concentration PbS phase of galena. The produced Na2S and Lab-PbS were examined using scanning electron microscopy and energy dispersive X-ray spectroscopy for microstructural and chemical analysis. The results confirmed a high-purity PbS compound (&gt;99%) with a nanoscale particle size. The results showed that ultrasonic agitation was vital for obtaining the nanoparticle size of the Lab-PbS. Furthermore, thin films from the synthesized Lab-PbS and galena were successfully thermally evaporated on glass, quartz, and silicon substrates. The formation of nanometric grains was confirmed by scanning electron microscopy (SEM). XRD and FTIR spectroscopy were carried out for the Lab-PbS, galena fine powders, and galena thin films. The average crystal diameter was calculated for the galena thin films and was found to be approximately 26.6 nm. Moreover, the UV–Visible transmission curve was measured for the thin films in the wavelength range of 200–1100 nm in order to calculate the bandgap energy (Eg) for the thin films. The values of Eg were approximately 2.65 eV and 2.85 eV for the galena and Lab-PbS thin films, respectively. Finally, the sintering of the Lab-PbS and galena powders was carried out at ~700 °C for 1 h under vacuum, achieving relative densities of ~98.1% and ~99.2% for the Lab-PbS and galena, respectively.