Non-uniform Microstructure Research Articles

Regulation of protonation in aramid nanofiber films for improved mechanical properties

Abstract Aramid nanofibers (ANFs) are a strong and heat resistant nanomaterial that can be isolated from commercial poly(p-phenylene terephthalamide) (PPTA) fibers. These nanofibers allow bottom-up self-assembly to form macroscale structures in various form factors through a simple reprotonation process. However, the mechanical properties of these reassembled ANF structures often fall short of those of PPTA fibers, mainly due to insufficient packing, non-uniform microstructures, and low crystallinity. In this study, we present ANF films with improved mechanical properties prepared by a repeated spin-coating technique combined with a reprotonation process using deionized water and formic acid at concentrations ranging from 20 to 60 wt.%. Extensive analyses were performed on the resulting ANF films to evaluate their surface and cross-sectional morphologies, chemical bonds and compositions, thermal stabilities, and mechanical properties. The fabricated ANF films exhibited remarkable performance, with an elastic modulus of 6.7 GPa, tensile strength of 680 MPa, and toughness of 7.7 MJ m−3, while maintaining the inherent thermal stability of PPTA fibers. These properties significantly exceed those of previously reported ANF films, broadening the potential applications for ANF films in various fields.

Effect of ultrasonic vibrations on mass efficiency and microstructure of laser direct deposition Inconel 718 superalloy

Laser direct deposition (LDD) is widely used to repair and manufacture high-value industrial components. However, it faces various defects, such as porosity, cracks, non-uniform microstructure, lack of fusion, keyhole phenomenon, element segregation, and undesirable secondary phases. A method to manage these defects is to concurrently apply ultrasonic vibrations (USV) during the LDD process. This study investigates the effect of USV on the mass efficiency and microstructure of LDD Inconel 718 superalloy to understand how incorporating USV can change the performance and structural integrity of single passes produced using the LDD process. For this purpose, USV is applied to a substrate during the LDD process. The resulting samples are characterized and analyzed using optical microscopy, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The results indicate that applying USV below a threshold power value increases mass deposition by over 25%, while exceeding this threshold reduces it. Attention to this threshold power value is crucial for determining the process parameters, including laser power and speed. Additionally, USV transforms the microstructure from columnar to equiaxed and increases subgrain formation. This implementation also enhances the cooling rate, significantly decreasing the Laves phase by over 30% in all process parameters.

Quantitative revealing the solute segregation behavior at melt pool boundary in additively manufactured stainless steel using a novel processing method for precise positioning by HAADF-STEM

Laser-powder bed fusion (LPBF) enables the fabrication of complex metallic components by manipulating various laser scan strategies to control microstructure and texture. Multiple thermal cycling and rapid solidification lead to non-equilibrium, non-uniform microstructure, and micro-segregation at the melt pool boundary (MPB), whose accurate location is still invisible by transmission electron microscopy (TEM), and quantitative concentration remains imprecise. In this study, we proposed a novel method to make it clear by controlling the crystallographic texture of 316 L stainless steel through unique LPBF processing parameters to obtain a single-crystal-like microstructure of the cellular structures along the laser scanning direction. The accurate location of the track-track MPB is distinguishable by means of the transverse and longitudinal cellular dislocation structures on both sides. The edge-on state of the track-track MPB makes the quantitative concentration analysis precisely using high-angle annular dark-field scanning TEM with energy-dispersive X-ray spectroscopy, which is in good agreement with the Scheil-Gulliver solidification simulations.

Multiscale topology optimization via dual neural networks and cutting level sets with non-uniform parameterized microstructures

Multiscale topology optimization via dual neural networks and cutting level sets with non-uniform parameterized microstructures

Microstructural Design of PEFC Electrocatalyst Layer Using Mesoporous Carbon

Heavy-duty applications of polymer electrolyte fuel cells (PEFCs) require improved activity and durability of the cathode electrocatalysts. The nanostructure and microstructure of the catalyst layer both significantly affect PEFC performance. Mesoporous carbons (MC) have mesopores which have been shown to suppress ionomer poisoning, when used as a catalyst support, leading to higher catalytic activity. Here, we compare the initial performance of single cells using Ketjen black (KB) and MC catalyst supports. Furthermore, the fuel cell performance is evaluated using Pt-Ta-Co alloy-based catalyst decorated on MC. Pt-Ta-Co/MC electrocatalyst exhibits high cell performance in a low current density range. However, cell performance at high current densities has yet to be improved due to non-uniform microstructure of the Pt-Ta-Co/MC electrocatalyst layer.

Microstructural Design of PEFC Electrocatalyst Layer Using Mesoporous Carbon

Heavy-duty applications of polymer electrolyte fuel cells (PEFCs) require improved activity and durability of the cathode electrocatalysts. The nanostructure and microstructure of the catalyst layer both significantly affect PEFC performance. Mesoporous carbons (MC) have mesopores which have been shown to suppress ionomer poisoning, when used as a catalyst support, leading to higher catalytic activity. Here, we compare the initial performance of single cells using Ketjen black (KB) and MC catalyst supports. Furthermore, the fuel cell performance is evaluated using Pt-Ta-Co alloy-based catalyst decorated on MC. Pt-Ta-Co/MC electrocatalyst exhibits high cell performance in a low current density range. However, cell performance at high current densities has yet to be improved due to non-uniform microstructure of the Pt-Ta-Co/MC electrocatalyst layer.

Microstructure Evolution and Mechanical Properties of In Situ TiB2/Al–Zn–Mg–Cu Composites by Electropulsing‐Assisted Solution Treatment

The traditional solution treatment is not completely applicable for in situ TiB2/Al–Zn–Mg–Cu composite due to the influence of TiB2 particles. This study investigates the impact of the electropulsing‐assisted solution (EAS) process on the microstructure evolution and mechanical properties of TiB2/Al–Zn–Mg–Cu composites. The nonuniform microstructure evolution related to the difference in temperature and current density is supported by simulative and experimental results. EAS treatment significantly enhances the degree of supersaturation, allowing phases surrounding TiB2 particles to dissolve without extensive overburning, unlike traditional solution treatments. This improvement is attributed to the reduced thermodynamic barrier and accelerated atomic diffusion, facilitated by both localized and average Joule heating effects and enhanced thermal electron/phonon scattering. Meanwhile, grain size remains stable during the temperature rise induced by EAS treatment. Furthermore, the mechanical properties of composites increase, among which the increase in strength is mainly ascribed to solid–solution strengthening, and the increase in elongation is related to multiple factors referring to TiB2 particles fracture and interface crack between the undissolved phases and matrix. This study provides an approach to achieve an efficient dissolution of phases aggregated with particles and without widespread overburning in particle‐reinforced Al matrix composites via electropulsing techniques.

Investigation of non-uniform carbonation in strain-hardening magnesia composite (SHMC) and its impacts on fiber-matrix interface and fiber-bridging properties

Unlike Portland cement, the reactive magnesia cement (RMC) develops its strength via carbonation. Non-uniform microstructure and properties due to the varied carbonation degree across cross-section depth have thus been observed. However, the existing micromechanics design theory employs uniform material properties (cementitious matrix and fiber-matrix interface characteristics) to design strain-hardening composites. This research investigated such non-uniform carbonation in a strain-hardening magnesia composite (SHMC) and its impacts on fiber-matrix interface and fiber-bridging properties. Results showed that mineral phase composition (of the cementitious matrix) and fiber-matrix interface properties across cross-section depth are highly non-uniform in SHMC due to varied carbonation degrees. The outer layer exhibited a much higher carbonation degree with significantly stronger fiber-matrix friction, while the inner core showed negligible carbonation with distinct fiber-matrix properties. Insights gained from the micro-scale investigation were used to calculate the fiber-bridging constitutive law of SHMC with non-uniform carbonation across cross-section depth and to assess its strain-hardening performance. This investigation highlights the importance and necessity of considering non-uniform carbonation in the modeling and design of SHMC. The study presents a framework for the consideration of non-uniform micromechanical parameters in the design of strain-hardening cementitious composites.

Solidification-induced nonuniformity in U–Zr–RE metallic nuclear fuel rods

Metallic fuel is being developed for the next generation of sodium-cooled fast reactors due to its safety and fuel cycle economics through spent fuel reprocessing technology. After spent fuel reprocessing, rare earth elements that are immiscible with Uranium and Zirconium are included in the raw material for metallic fuel. Achieving a uniform composition and microstructure of RE inclusions is challenging because phase separation and temperature inhomogeneities during solidification lead to non-uniform composition and microstructure. This study explores the solidification and inclusion formation of U–Zr–RE metallic fuel rods. We show how RE inclusions are formed in the U–Zr matrix and how temperature inhomogeneities during solidification control the inclusion size distribution and edge migration of RE inclusions along the U–Zr–RE rods. Understanding the inhomogeneity of inclusions due to solidification can provide hints for making homogeneous nuclear fuel rods.

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

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

Microstructure, electrical and magnetic properties of MgFe2O4 sintered with (1-x)Bi2O3.xFe2O3 additives

In this research, liquid phase sintering of MgFe2O4 with a Bi2O3-Fe2O3 additive was studied. Initially, MgFe2O4 powder was synthesized at 1150 °C, then 3 wt% additive with (1-x)Bi2O3.xFe2O3 (x=0.00, 0.04, 0.08, 0.12) was added to the powder and sintered at 1050 °C. The x=0.04 sample showed the highest density of ∼4.40 g/cm3. Cubic spinel ferrite and phases containing bismuth oxide were formed in all samples, notably, only x=0.08 and x=0.12 samples consist hematite. Uniform microstructure was achieved for x=0.00 and 0.04 samples while other samples exhibited non-uniform porous microstructures. EDS analysis revealed uniform iron distribution in the grains of x=0.04 sample, unlike the x=0.00 sample. Impedance spectroscopy indicated increased electrical resistivity in x=0.04 compared to x=0.00. Saturation magnetization peaked at 18.5 emu/g for x=0.04, then decreased, while coercive force rose from 13.2 to 30.2 Oe with increasing x. The x=0.04 additive acted as the optimal sintering aid, improving electrical and magnetic properties.

Effect of Annealing after Casting and Cold Rolling on Microstructure and Electrochemical Behavior of High-Entropy Alloy, Cantor

High-entropy alloys (HEAs), a relatively new class of materials, have attracted significant attention in materials science owing to their unique properties and potential applications. High entropy stabilizes the phase of a solid solution over a wide range of chemical compositions, yielding unique properties superior to those of conventional alloys. Therefore, this study analyzed the microstructure and electrochemical behavior of HEAs (Cantor) to evaluate their corrosion resistance, according to their manufacturing process (casting, cold rolling, and annealing). The microstructural morphologies and sizes were analyzed using electron backscatter diffraction. The electrochemical behavior was examined using open circuit potential measurements, electrochemical impedance spectroscopy, potentiodynamic polarization tests, and critical pitting temperature measurements using a potentiostat. The casting process formed a nonuniform microstructure (average grain size = 19 μm). The cold rolling process caused the formation of fine grains (size = 4 μm). A uniform microstructure (grain size > 151 μm) was formed after heat treatment. The corrosion resistance of the HEAs was determined from the passivation layer formed by Cr oxidation. These microstructural differences resulted in variations in the electrochemical behavior. Microstructural and electrochemical analyses are crucial because HEAs have diverse potential applications. Therefore, this study contributes to future improvements in HEA manufacturing processes.

Fatigue crack evaluation of butt weld joints in full-scale aluminum alloy joints: Experimental and numerical study of traction structural stress

In this study, the digital image correlation technique is used to determine the inconsistent mechanical properties and microstructure non-uniformity in different regions of aluminum alloy butt welded joints. A state monitoring method is proposed based on phased-array ultrasonic total focus imaging for crack evolution. A series of surface fatigue crack propagation tests on full-scale aluminum alloy butt welds are investigated, which innovatively revealed the mechanism and evolution law of crack propagation at the surface of the weld. The analytical function for dynamic crack propagation in welded structures is proposed, which provides a new idea and data support for clarifying the state deterioration process of structures. The results show that the traction structural stress can effectively identify the critical fatigue position of the weld and effectively account for the effect of angular misalignment. The phased-array ultrasonic total-focus imaging monitoring analysis method for surface fatigue crack propagation is proposed to improve the completeness of the fatigue crack evolution law.

Metallurgical insight of premature failure of a Blast Furnace copper stave

Present study investigates the premature failure (leakage) of copper (Cu) cooling staves placed at the lower stack region of a Blast Furnace (BF). This failure resulted in an increased frequency of make-up/ reserve water compensation every 10 h instead of average 24hrs. Detailed macro and microstructural analysis were carried out to understand the mechanism of failure in the Cu stave using phenomena observations, dial gauge measurements, metallographic investigation, and chemical analysis. Directional accretion of burden fines and puncture (leakage) profile were observed macroscopically. Puncture occurred from outer surface to inner surface of the channels of the stave. Micrographs of puncture location revealed non-uniform microstructure and grain deformation. Analysis suggested surface wear of the Cu stave due to a combined effect of continuous accretion of burden along with hot gas flow. Wear led to reduction in thickness and subsequent puncture/ leakage took place at the channel locations having a minimum cross-sectional thickness. With the help of this study, a failure mechanism of BF Cu Stave, a process critical component, has been explored. Recommendations such as insert modification, using more wear-resistant material or protective layer and conducting intermittent ultrasonic thickness measurements have been proposed to get an early warning of any untoward damages and process delays.

Faulty machining and micro-segregation assisted fatigue failure of cylinder head stud of a diesel generator

A detailed failure analysis of cylinder head stud bolt of a four-stroke diesel generator has been presented. The study included optical emission analysis, tensile testing, hardness testing, optical microscopy, SEM, and EDX analyses. The investigation showed that the main mechanism of failure was corrosion-fatigue. Fatigue initiation was assisted by pitting corrosion induced by faulty machining, moisture, and presence of tempered martensite and non-metallic inclusions at the surface. Propagation of the fatigue crack was encouraged by localized corrosion within the tempered martensite, non-metallic inclusions, and Mn/Cr/Mo/Si micro-segregation. Both excessive C and Mn/Cr/Mo/Si micro-segregation caused the formation of mixed microstructure of tempered martensite and fresh martensite with retained austenite. The non-uniform microstructure led to non-uniform hardness distribution and caused localized deformation during cyclic loading and promoted fatigue crack propagation.

Non-uniform microstructure evolution rules and mechanisms of Ti55 alloy with initial basket-weave structure during electrically-assisted V bending

Electrically assisted V-bending (EAVB) experiments of Ti55 alloy sheets with initial basketweave structure were carried out at effective current densities of 3–5A/mm2. The history of temperature field, microstructure patterns and mechanical properties were characterized by IR imaging, OM, EBSD and hardness tests. The results show that α lamellae continuously decrease in thickness (from 2.38 μm to 0.64 μm) with increasing current density. The microstructure patterns of the three deformation zones are significantly different due to different deformation mode and electro-thermo-mechanical routes. Due to limited plastic strain, the orientation rotation and shear fracture of the α lamellae are restricted in the neutral layer, while the ones in the inner and outer layers are refined and become more uniform at mild current density. With increasing current density, the main deformation mode of α grains in the inner layer is {1010} prismatic slip and dynamic spheroidization/recrystallization tends to occur at α lamellae with <0110>α//TD orientation. In the neural and outer layer, intense local Joule heat effect induces α→β→α′ phase transformation in “hot spots”, leading to massive growth of 3 variant needle-like α′, intensified heterogeneous micro-deformation and significant strengthening effect. The combined effects of local Joule heat, residual α phase and deformation-induced defect nucleation break the strict Burgers orientation relationship between α/α’ lamellae and β matrix during EAVB and subsequent cooling process.

High elongation heterostructure rare earth magnesium alloy based on rotating backward extrusion process

In this paper, Mg-9.5Gd-4Y–2Zn-0.5Zr cylindrical parts were prepared by the conventional backward extrusion (CBE) process and rotating backward extrusion (RBE) process. The effects of the two processes on the microstructure and mechanical properties of different orientation regions of rare earth magnesium alloy were analyzed and compared. The RBE process introduces a torsional shear quantity based on the CBE process. By changing the direction of plastic flow, has a positive effect on the elongation (EL) of the alloy. It was found that dynamic recrystallization (DRX) occurred in both CBE and RBE processes. With the transition of deformation, the strain continues to accumulate, and the DRX mechanism changes from discontinuous dynamic recrystallization (DDRX) to continuous dynamic recrystallization (CDRX). Compared with the CBE process, the grain refinement of the RBE process is more significant. After deformation, a more significant heterostructure is obtained in the RBE-45° region, and the average grain size reaches 24.7 μm. The ultimate tensile strength (UTS), yield strength (YS), and EL of the alloy in this region are 292.5 ± 7.7 MPa, 226.6 ± 7.4 MPa, and 21.5 ± 1.3 %, respectively. Although the strength is slightly lower than that of CBE alloy, better plasticity is obtained. The excellent strength-toughness synergy is attributed to the synergistic effect between heterogeneous regions of non-uniform microstructure. This study provides some theoretical guidance for the industrial production of large-size magnesium alloy cylindrical parts and subsequent applications.

Material extrusion additive manufacturing of WC-9Co cemented carbide

Additive manufacturing (AM) cemented carbide is primarily challenged by critical issues of difficult-to-eliminate pores, cracks, deleterious phases, and non-uniform microstructure, which result in poor mechanical properties. This study utilizes material extrusion (MEX) AM technology to prepare a WC-9Co cemented carbide. The results show that green body printing and solvent debinding process significantly affect its stacked voids, interlayer bonding defects, and debound cracks. These green body defects are eliminated through liquid phase flow and WC particles flow-rearrangement during sintering, resulting in Co-rich regions or Co pools, abnormal growth of WC grains, and residual pores. A green body free of visible defects is prepared using a feedstock with a powder loading of 54 vol%, a printing temperature of 150 ℃, a microfilament overlap ratio of 30 %, and a printing-layer thickness of 0.1 mm. Followed by a two-step solvent debinding and continuous thermal debinding-vacuum-pressure sintering, a nearly fully dense WC-9Co cemented carbide is fabricated, with a uniform microstructure of two phases and free of pores, cracks, and Co pools. Its Vickers hardness, transverse rupture strength, and fracture toughness reach 1525±3 HV30, 3492±45 MPa, and 20.4±0.5 MPa·m1/2, respectively, which are significantly better than those of similar reports and could be comparable to similar cemented carbides prepared by powder metallurgy. This study could provide a new technological path for developing high-performance cemented carbide complex-structured components.

Manufacturing porous U-10Zr metallic fuels with controllable microstructure by volume control spark plasma sintering

In this paper, the volume control spark plasma sintering tool has been designed and applied to sinter porous U-10Zr metallic fuels, by which the sintered sample volume can be precisely controlled. Ethanol and NH4HCO3 are used to control the powder compact or as pore formers to control the pore size and pore structure. Without pore formers, the fuel pellet displays an inhomogeneous microstructure consisting of highly porous and highly densified areas. Uneven powder stacking in the green body results in a non-uniform microstructure, and in the closed-packed area, Joule heating accelerates the neck formation and densification. The addition of ethanol reduces the friction between the powders, resulting in isolated pores formed by the stacking of powders during the sintering. By adding NH4HCO3, the pore size, and structure can be well controlled, and an interconnected pore structure can be obtained upon the decomposition of the NH4HCO3. A uniform microstructure and pore distributions can be achieved through the U-10Zr fuel pellets by controlling current flow during the volume control SPS sintering. The microstructure and phase characterization of the sintered porous U-10Zr pellets show major phases of α-U and α-Zr for the sample with short dwelling. For the sample with long dwelling (30 min), the ω UZr2 in the Zr-enriched area has been observed. The strategy of volume control SPS sintering with the assistance of pore formers could be used to fabricate porous U-10Zr metallic fuels to mimic the microstructure evolution of irradiated metallic fuels (including porosity) and could enable a possible solution for the design of new sodium-free metallic fuels for high burnup.

Mechanically robust and uniform aramid nanofiber films fabricated using repeated spin-coating and protonation processes

Aramid nanofiber (ANF) films show promise for various industrial applications, but their applicability has been constrained by the low mechanical properties, which are mainly due to their incomplete packing and non-uniform microstructure. This work introduces an efficient method for significantly improving the mechanical properties of ANF films using repeated spin coating and protonation. The method allows for the preparation of ANF films with highly uniform microstructures and adjustable thicknesses while achieving excellent mechanical properties. These ANF films have a Young's modulus of 6.8 GPa, tensile strength of 310 MPa and hardness of 248 MPa, surpassing those produced using previous methods. A comprehensive analysis of the surface and cross-sectional morphologies, chemical composition, thermal stability, and mechanical properties was also carried out to characterize the film properties.