Segregation Of Elements Research Articles

Effect of Zr content on microstructure and mechanical properties of MoNbTaTiZrx refractory high-entropy alloy

Abstract The purpose of this paper is to explore how Zr content affects the crystal structure, micro-morphology, and mechanical properties of (MoNbTaTi) 100-xZrx alloys (x = 5,15,25). The results reveal that with the varying Zr contents, the alloy changes from a single-phase solid solution structure of Zr5 to a solid solution structure of Zr15 and Zr25 with a double BCC phase. Higher Zr levels lead to more pronounced elemental segregation, particularly, which makes Zr element enriched in the interdendritic region, and with the increase of segregation degree, the second phase separates between dendrites. In other words, Zr and Ti elements are densely distributed in the BCC2 phase. With the formation of the BCC2 phase, the mechanical properties of the alloy also changed obviously. Notably, as the Zr content rises, the alloy’s hardness and strength improve, while its ductility initially decreases before subsequently increasing. The Zr15 alloy was in a transition period of a two-phase structure, and the two-phase structure was not stable at this time, which led to a decrease in the plasticity of the alloy. The yield strength of Zr25 alloy is 1595 Mpa, the Vickers hardness is 542 HV, and the compressive fracture strain is 29%, showing the best comprehensive properties.

Microstructure evolution and mechanical properties of additively manufactured Ni-based GH4099 superalloy via hot isostatic pressing and heat treatment

In this study, GH4099 alloys with over 99.99 % density were produced by laser powder bed fusion (LPBF) and followed by hot isostatic pressing (HIP) and heat treatment (HT). The effects of HIP and HT on the microstructure evolution and mechanical properties of the additively manufactured GH4099 superalloy were examined systematically. The as-deposited columnar crystals were effectively transformed into equiaxed crystals via HIP and HT. During HIP, the elimination of defects and elemental segregation in the deposited samples occurs. However, uneven precipitation of the γ′ phase within grains causes the emergence of minor gaps in the γ matrix, which adversely affects mechanical properties. The microstructure resulting from HIP + solution treatment (ST) consists entirely of equiaxed recrystallized grains. The presence of twin and long-period stacking-ordered (LPSO) phases at twin boundaries strongly hinders dislocation behavior, and the remelting of precipitates and carbides greatly improves plasticity. Moreover, during the loading process at 900 °C, γ′ phase and carbides were re-precipitated, and the strain concentration was minimized during the precipitation process, resulting in the highest high-temperature strength. Conversely, in the HIP + solution and aging treatment (SAT) process, the progression of γ′ phase precipitation, condensation, annexation, and growth contributes to a reduction in strength. Coupled with an increase in the plasticity of the LPBF GH4099 alloy.

Effect of purity on solidification structure and micro-segregation in a nickel-based single crystal superalloy

The purity of nickel-based single crystal alloys plays an important role in the final service performance of turbine blades as it impacts the solidification structure, elemental segregation, and inclusions of castings. The highest purity of superalloys studied before was of altogether around 10 ppm of contents of N and O produced by the triple purification process (VIM+ESR+VAR). However, the impact mechanism still remains controversial, and meanwhile whether a lower content of N and O still keeps the impacts on castings is not yet clear due to the lack of raw materials. A superhigh purity of second generation of nickel-based single crystal superalloy DD98M with the sum of N and O contents as low as 4 ppm (hitherto the highest purity of the superalloy as published), home-produced by electron beam smelting (EBS), was put on focus in this work. The effect of three levels of purity (N-doped, commercial, and EBS, corresponding to 21, 10, and 4 ppm for the sum of N and O contents, respectively) on the microstructure evolution (including primary dendrite arm spacing (PDAS), eutectic, micropores, and γ′ phase) and the solute segregation behavior at dendritic scale and nano scale (γ/γ′ interfaces) were systematically studied and the influencing mechanisms were elucidated. The results show that the PDAS decreased from 406 μm to 322 μm with the reduction of O and N from 21 ppm to 4 ppm, which was irrelevant to precipitation of the nitride or oxide inclusions. Instead, it was due to the decrease of diffusion coefficient D or the increase of equilibrium coefficient k, or the decrease of the critical nucleation supercooling and the incubation time of dendrites. The micro-segregation, the number and volume fraction of eutectic, and the number and voltage percentage of shrinkage pores and gas pores were all greatly decreased with the increase of purity. These changes were closely related to the reduction of PDAS and the reduction of fluidity of the remained liquid in the interdendrites during solidification. The morphology and the size of the γ′ phase were independent from the purity, while the segregation of alloying elements at the γ/γ′ interface changed remarkably with the variation of the purity.

The Microstructure characteristic and Its influence on the stray grains of Nickel-based single crystal superalloys prepared by Laser directed energy deposition

The microstructure adjustment and the stray grains inhibition are important for the preparation of Nickel-based single crystal (SX) superalloys by laser directed energy deposition (L-DED). In this work, the single channel monolayer and single channel five-layers DD6 SX superalloys have been prepared by L-DED. The macroscopic simulations in the deposition processing and multiscale characterizations of deposition structure were used to analyze the formation and evolution mechanisms of unique precipitations and stray grains. Results shows that the larger laser power and higher powder feed rate have a positive impact on the epitaxial growth of columnar dendrite and the elimination of stray grains. The residual stress caused by the complex thermal cycles is not the direct reason that induce the formation of SGs, but the rapid movement of dislocations result in the formation of sub-grain boundary. According to the columnar transition to equiaxed theory (CET), temperature field simulation and analysis of element segregation behaviors, the element segregation results in the unique microstructure, include petal-shaped γ/γ′ eutectic and demarcation band with a thickness of a single γ/γ′ eutectic. Besides, the geometric size of γ/γ′ eutectic decrease with respect to the deposition height. With the change of height at deposition region, dendritic orientation deviations affect the uniformity of element segregation, resulting in variations in γ′ phase and γ/γ′ eutectic dimensions between dendritic core and the inter-dendrite zone at the microscopic level and manifesting as grain boundaries at the mesoscale. At the same time, the formation mechanisms of carbide and adjacent γ/γ′ eutectic leads to the misorientations between the dendrite core and the inter-dendrite zone, which also appears as stray grains at the mesoscopic scale.

Investigation on microstructural and mechanical integrity of GTAW dissimilar welded joint of IN 718/ASS 304L using Ni-based filler IN 625 using EBSD and DHD techniques

The current study investigates the relationship between the microstructural and structural characteristics of dissimilar gas tungsten arc welding (GTAW) between Inconel 718 (IN 718) and austenitic stainless steel 304L (ASS 304L) using Inconel 625 (IN 625) as a filler material. The microstructural characterization of the dissimilar weld includes the application of an optical microscope (OM), field emission scanning electron microscopy (FE-SEM) including energy dispersive spectroscopy (EDS), and electron backscatter diffraction (EBSD). The optical and FESEM analysis of the base metals (BM) indicates the austenitic nature of the IN 718 BM matrix, which incorporates strengthening precipitates γ′ and γ'' distributed throughout the Nickel matrix. In contrast, the ASS 304L BM exhibits an austenitic microstructure along with twins. Moreover, IN 625 weld metal exhibits austenitic microstructure in the form of cellular, columnar, and equiaxed dendrites. Elemental segregation demonstrates the existence of Nb, and Mo-rich carbides, including the laves phases at the interdendritic regions of the IN 625 weld zone and IN 718 Heat-Affected Zone (HAZ). Ferrite stringers were noticed in the HAZ of ASS 304L. EBSD analysis shows the improved texture of the weld zone exhibiting fine equiaxed recrystallized microstructures. EBSD/Kernel average misorientation (KAM) micrographs reveal the existence of high strain at the weld metal grain boundaries. Vickers microhardness assessment of the dissimilar weld demonstrates the high hardness of 257.5 HV for the IN 625 weld zone because of the occurred NbC, laves phases, and Mo-rich carbides. Room temperature tensile characterization shows the failure of tensile specimens from ASS 304L BM reflecting the high strength of the IN 625 weld metal (662 MPa). Tensile tests at high temperatures were performed at 550 °C, 600 °C, and 650 °C. High-temperature tensile result exhibits a higher tensile strength of IN 625 weld zone than the ASS 304L BM, as the tensile specimens fails from 304L BM. The specimen exposed at 550 °C exhibits the highest tensile strength of 388 MPa. The Charpy impact toughness test was conducted, with notches at the HAZ of ASS 304L, HAZ of IN 718, and the weld center being evaluated. The toughness value of the weld metal decreases (99 J) due to occurrence of the secondary precipitates. To analyze residual stress, the deep hole drilling (DHD) technique was used, which revealed that the peak residual stress (230 MPa) is induced at 6 mm from the weld surface and falls into the tensile stress category.

Compositional regulation in additive manufacturing of precipitation-hardening (CoCrNi)94Ti3Al3 medium-entropy superalloy: Cellular structure stabilization and strength enhancement

High or medium-entropy alloys that feature high thermal stability and excellent oxidation resistance are promising candidates for elevated temperature applications. The rapid softening of monolithic high or medium-entropy alloys with single face-centered cubic structure at elevated temperatures, however, is a main weakness. In this paper, we report new high strength γ′-hardened ((CoCrNi)94Ti3Al3)98Nb2 medium-entropy alloy through laser powder-bed fusion (L-PBF) followed by ageing. In particularly, the tensile strengths of the aged ((CoCrNi)94Ti3Al3)98Nb2 alloy at 20 °C and 700 °C can reach up to 1.93 GPa and 1.11 GPa, respectively, 112 % and 122 % stronger than the as-built CoCrNi alloy tested at the same condition. A new strengthening mechanism, i.e., elemental segregation induced the cellular structure stabilization, in tandem with other hierarchical microstructure features, including ultrafine γ′ precipitates, dense twin boundaries, and other types of crystallized defects, co-contribute to the superb tensile strength at room and elevated temperatures. Such a simple alloy design and processing strategy outlines a guideline for designing novel multicomponent alloys and/or composites with superior microstructural stability and mechanical response at room and elevated temperatures.

On the control of epitaxial growth and stray grains during laser-directed energy deposited Ni-based single crystal superalloy

Laser-directed energy deposition (L-DED) is considered as an effective repair method for damaged single-crystal (SX) superalloy turbine blades. However, controlling stray grains (SGs) and epitaxial growth is still the major problem. This study investigated the influences of pre-solution treatment and intrinsic heat treatment (IHT) on the formation of SGs and epitaxial growth of L-DED René N5 SX superalloy. The γ/γ’ eutectics and coarse γ’ precipitates at the inter-dendrite region can be eliminated after pre-solution treatment procedures before the L-DED experiment. A lower temperature in pre-solution treatment resulted in the retention of residual γ/γ’ eutectics and coarse γ’ precipitates. Thus, the aggravated element segregation within the local melt pool and interface collapse during the L-DED process can result in stray grains (SGs) formation. Improved pre-solution treatment procedures can also help reduce SGs caused by the carbides in the substrate. Besides, the SG formation in the deposited layers can be attributed to the recrystallization as a result of high thermal stress during the IHT in thermal cycles. The optimized pre-solution treatment procedure reduced the elemental segregation of the substrates, resulting in a larger primary dendrite arm spacing (PDAS) from the bottom of the deposited layers. Due to IHT during thermal cycles in the deposited layers, the equivalent heat treatment process promoted the re-precipitation and growth of γ’ phase. Meanwhile, the optimized pre-solution treatment procedure decreased the size of the heat-affected zone (HAZ) caused by thermal cycles. In summary, by optimizing the substrates' pre-solution treatment procedures to eliminate the γ/γ’ eutectics,coarse precipitaes and decrease the carbides in the subsrtates, the formation of SGs resulting from substrate segregation and heterogeneous microstructure can be controlled. This work provides the potential guidance of substrate pre-treatment for L-DED repair of SX superalloys.

A promising strontium and cobalt-free Ba1-xCaxFeO3-δ air electrode for reversible protonic ceramic cells

The air electrode with strontium and cobalt elements has the elemental diffusion or delamination issue on the air electrode/electrolyte interface in reversible protonic ceramic cells (RPCCs). Hence the development of strontium and cobalt-free triple conducting (H+/O2-/e-) air electrodes with high electrochemical activity and stability is urgent. Here, we report a strontium and cobalt-free Ba0.8Ca0.2FeO3-δ (BCF82) air electrode with high catalytic activity and electrochemical stability for oxygen reduction/evolution reactions. A RPCC with the BCF82 air electrode shows a high peak power density of 1.14 W cm−2 in the fuel cell mode and a current density of 3.49 A cm−2 under 1.3 V in the electrolysis mode at 700 °C. Furthermore, the cell demonstrates suitable stability in the fuel cell, electrolysis and reversible modes at 600 °C for hundreds of hours without elemental segregation and delamination issue. This work offers an efficient approach to develop low-cost and durable air electrodes for RPCCs.

Microstructural evolution and spheroidization mechanism of powder metallurgy Ti-6Al-4 V alloys after high-temperature forging

After high-temperature forging and rapidly cooling, the microstructure evolution and spheroidization mechanism of powder metallurgy Ti-6Al-4 V alloy have been clarified. The spheroidization process is divided into two asynchronous stages. The initial stage is primarily characterized by the initial shearing and twisting of GBα grain boundaries, as well as the deformation of lamellar structure. Subsequently, the fragmentation of original GBα grain boundaries and the fracture of intra-granular α lamellae are observed. This process is accompanied by grain twisting and substructure formation, especially the division of lamellae through interface splitting and the segregation of local chemical elements. The differential accumulation of elements around the fractured and twisted grains suggests that element segregation and interfacial energy play a significant role in microstructure evolution. Therefore, the static spheroidization process largely depends on the formation and evolution of dislocation substructures, and the reduction of interfacial energy may be a key factor driving this process. These findings provide a theoretical basis for manufacturing metals with specific anisotropic properties by controlling microstructure evolution.

Research on the novel spinel structure of Cu0.5Ni0.5MnCoO4 and its application in solid oxide fuel cells

In this study, the Cu0.5Ni0.5MnCoO4 (CNMC) material was developed for use in the cathode of solid oxide fuel cells (SOFC). X-ray diffraction (XRD) confirmed the spinel structure and demonstrated compatibility with Yttria-stabilized zirconia (YSZ) electrolyte at elevated temperatures. The conductivity of CNMC was found to be between 28 and 55 S cm−1 at temperatures ranging from 700 to 900 °C. Oxygen-temperature programmed desorption (O2-TPD) revealed that CNMC powder possesses effective oxygen catalytic characteristics. To enhance performance, CNMC was combined with Gd0.1Ce0.9O2-δ (GDC, H2-bank Co. Ltd.) in a mass ratio of 3:7 (CG37). The thermal expansion coefficient (TEC) of this composite was measured at 12.8 × 10−6 K−1, closely matching that of YSZ and avoiding the issue of strontium segregation, eliminating the need for a barrier layer between the electrolyte and the cathode. The peak power densities of CG37 reached 1175 mW cm−2 and 905 mW cm−2 at 800 °C and 750 °C, respectively. CG37 underwent testing for 1000 h under constant-current discharge at 600 mA cm−2 and 750 °C, showing a voltage degradation rate of 2.5 %/kh. The cell's microstructure remained intact without any signs of elemental diffusion or segregation, indicating excellent chemical compatibility and stable structural integrity. This research is expected to further advance the study and utilization of novel solid oxide fuel cells.

Comparative study on microstructure and properties of HR-2 anti-hydrogen steel weld joints with different section shapes by vacuum electron beam welding

The forming, microstructure, mechanical properties and corrosion resistance of three kinds of vacuum electron beam welded joints with different shapes were studied. The results of X-ray inspection of the joints showed that the three shapes of welded joints could meet the requirements of the quality inspection. The results of microstructure characterization show that the worm or bone-like δ-ferrite appears in the upper and lower regions of the funnel-shaped and bell-shaped joints, while only a small amount of δ-ferrite appears in the local regions of the nail-shaped joints. The test results of mechanical properties show that the micro-hardness of the weld center in the three kinds of shaped joints is the lowest. All the specimens fracture in the weld, and the bell-shaped weld presents the highest impact energy and bending load. Funnel-shaped weld shows the worst corrosion resistance due to the element segregation of the weld. Thus, the bell-shaped joint exhibits the best comprehensive performance.

Grain refinement and Laves phase dispersion by high-intensity ultrasonic vibration in laser cladding of Inconel 718

Laser cladding is a promising surface modification and repair technology for fabricating Inconel 718 parts. However, laser cladding may produce coarse grains and brittle Laves phase, leading to a significant decrease in performance. The application of high-intensity ultrasonic vibration in laser cladding is able to refine grain and reduce Laves phase. This study investigates the distribution characteristics and the evolution mechanism of the grains and Laves phase in laser cladding with high-intensity ultrasonic vibration. The effects of high-intensity ultrasonic vibration on alteration of grain characteristics and the reduction of Laves phase were analyzed and discussed through ultrasonic vibration-assisted laser cladding experiments. Results indicate that high-intensity ultrasonic vibration promoted a columnar-to-equiaxed transition, and reduced the grain size from 75.6 μm to 48.8 μm. Furthermore, the Laves phase had a decrease of 47.1% in the volume fraction, and transformed from a long-striped shape into a fine granular shape, leading to a more homogeneous distribution of elements in Laves phase. The change in the grains and the Laves phase is attributed to dendrite fragmentation and inhibition of element segregation by nonlinear effects of ultrasound including cavitation and acoustic streaming. The findings of this study confirm the significant benefits of applying high-intensity ultrasonic vibration in laser cladding and provide insight into the underlying evolution mechanisms of high-intensity ultrasonic vibration for grains and Laves phase.

Improving laser welded joint performance of medium-Mn steel through C and Mn partition by intercritical annealing process

In this paper, the fracture failure mechanism of laser welded (LW) joints of medium-Mn steel is studied. And the mechanical properties of the joints were greatly improved by designated intercritical annealing (IA) process. Experimental results showed that the elongation of the as-welded joint of medium-Mn steel is very low, and the fracture shows typical brittle fracture characteristics. Electron probe micro-analyzer (EPMA) test showed that there were many Mn segregation bands in the joint, and electron backscatter diffraction (EBSD) surface scanning test further demonstrated that many Mn23C6 carbides were produced at the martensite grain boundary (GB) of the fusion zone (FZ), which was the main reason for the occurrence of brittle fracture in the FZ. The IA process improves the segregation of Mn element at the GB of the joint and reduces the intergranular brittleness. At the same time, more austenite was distributed by C and Mn elements, and more Fe3C phases were found near austenite in the EBSD diagram, which provided nucleation centers for the formation of austenite. The product of strength and elongation (PSE) of the IA treated joint was dramatically increased by 2693.65%.

Intrinsic tensile ductility in strain hardening multiprincipal element metallic glass

Traditional metallic glasses (MGs), based on one or two principal elements, are notoriously known for their lack of tensile ductility at room temperature. Here, we developed a multiprincipal element MG (MPEMG), which exhibits a gigapascal yield strength, significant strain hardening that almost doubles its yield strength, and 2% uniform tensile ductility at room temperature. These remarkable properties stem from the heterogeneous amorphous structure of our MPEMG, which is composed of atoms with significant size mismatch but similar atomic fractions. In sharp contrast to traditional MGs, shear banding in our glass triggers local elemental segregation and subsequent ordering, which transforms shear softening to hardening, hence resulting in shear-band self-halting and extensive plastic flows. Our findings reveal a promising pathway to design stronger, more ductile glasses that can be applied in a wide range of technological fields.

Facet-Dependent Ni Segregation in a Micron-Sized Single-Crystal Li1.2Ni0.2Mn0.6O2 Cathode.

Elemental surface segregation in cathode materials is critical for determining the phase and interfacial reaction between the electrode and electrolyte, which consequently affects the electrochemical properties. Single-crystal cathodes of Li1.2Ni0.2Mn0.6O2 and Li1.2Ni0.2Mn0.6O1.95F0.05 with octahedral morphologies of (102)- and (003)-dominated facets have been manifested to show enhanced electrochemical properties. However, the surface structural features of such single crystals have not been investigated. Herein, using scanning transmission electron microscopy, energy dispersive X-ray spectroscopy, and electron energy loss spectroscopy, we probe the elemental surface segregation characteristics in these single-crystal cathodes. We reveal that Ni surface segregation shows dependence on the crystal facet such that it occurs on crystal facets with a mix of cations and anions but not on the facets with only cations or anions. Furthermore, facet-dependent surface reconstructions are observed, featuring a spinel-like structure at the Ni-rich facet but a rock-salt structure at the facet without Ni segregation. The commonly known Mn reduction appears at the single-crystal surfaces and is more pronounced at the facet without Ni segregation. We further reveal that fluorination leads to stabilization of surface oxygens. This study provides detailed structural and chemical information about the facet-dependent Ni surface segregation and the resulting phase formation in the rather less explored micron-sized octahedral Li1.2Ni0.2Mn0.6O2 and Li1.2Ni0.2Mn0.6O1.95F0.05 single crystals, which is key to further exploration of the electrochemical properties of the cathodes in the form of microsized single crystals.

A comparative study on the passive film and SCC behavior of Ti-6Al-3Nb-2Zr-1Mo alloy at various test temperatures in simulated seawater

In this work, the electrochemical and stress corrosion cracking (SCC) behavior of Ti-6Al-3Nb-2Zr-1Mo alloy in simulated seawater at various solution temperatures were systematically studied. Results show rising test temperature increases the point defect density in passive film and deteriorates the stability. Therefore, SCC is promoted by localized anodic dissolution (AD). At 25 °C, SCC initiates in αp phase, and β phase hinders SCC propagation on account of the lower electrochemical activity induced by element segregation. While at 4 °C, the SCC propagation rate is higher than that at 25 °C, as the SCC propagation resistance of β phases decreases.

Homogenous coating of Li+ conductive Li5AlO4 on single-crystalline nonstoichiometric Li1.04Ni0.92Al0.04O2 for rechargeable lithium-ion batteries

Cobalt-free, nickel-rich LiNi1-xAlxO2 (x ≤ 0.1) is an attractive cathode material because of high energy density and low cost but suffers from severe structural degradation and poor rate performance. In this study, we propose a molten salt-assisted synthesis in combination with a Li-refeeding induced aluminum segregation strategy to prepare Li5AlO4-coated single-crystalline slightly Li-rich Li1.04Ni0.92Al0.04O2. The symbiotic formation of Li5AlO4 from reaction between molten lithium hydroxide and doped aluminum in the bulk ensures a high lattice matching between the Ni-rich oxide and the homogenous conductive Li5AlO4 that permits high Li+ conductivity. Benefiting from mitigated undesirable side reactions and phase evolution, the Li5AlO4-coated single-crystalline Li1.04Ni0.92Al0.04O2 delivers a high specific capacity of 220.2 mA h g−1 at 0.1 C and considerable rate capability (182.5 mA h g−1 at 10 C). Besides, superior capacity retention of 90.8% is obtained at 1/3 C after 100 cycles in a 498.1 mA h pouch full cell. Furthermore, the particulate morphology of Li1.04Ni0.92Al0.04O2 remains intact after cycling at a cutoff voltage of 4.3 V, whereas slightly Li-deficient Li0.98Ni0.97Al0.05O2 features intragranular cracks and irreversible lattice distortion. The results highlight the value of molten salt-assisted synthesis and Li-refeeding induced elemental segregation strategy to upgrade Ni-based layered oxide cathode materials for advanced Li-ion batteries.

Reduced Volume Expansion of Micron‐Sized SiOx via Closed‐Nanopore Structure Constructed by Mg‐Induced Elemental Segregation

AbstractThe inherently huge volume expansion during Li uptake has hindered the use of Si‐based anodes in high‐energy lithium‐ion batteries. While some pore‐forming and nano‐architecting strategies show promises to effectively buffer the volume change, other parameters essential for practical electrode fabrication, such as compaction density, are often compromised. Here we propose a new in situ Mg doping strategy to form closed‐nanopore structure into a micron‐sized SiOx particle at a high bulk density. The doped Mg atoms promote the segregation of O, so that high‐density magnesium silicates form to generate closed nanopores. By altering the mass content of Mg dopant, the average radii (ranged from 5.4 to 9.7 nm) and porosities (ranged from 1.4 % to 15.9 %) of the closed pores are precisely adjustable, which accounts for volume expansion of SiOx from 77.8 % to 22.2 % at the minimum. Benefited from the small volume variation, the Mg‐doped micron‐SiOx anode demonstrates improved Li storage performance towards realization of a 700‐(dis)charge‐cycle, 11‐Ah‐pouch‐type cell at a capacity retention of >80 %. This work offers insights into reasonable design of the internal structure of micron‐sized SiOx and other materials that undergo conversion or alloying reactions with drastic volume change, to enable high‐energy batteries with stable electrochemistry.

High temperature embrittlement of Inconel 625 alloy manufactured by laser powder bed fusion

The comprehensive mechanical behavior of Inconel 625 alloy fabricated by laser powder bed fusion (LPBF) and hot isostatic pressing (HIP) was studied. Tensile experiments were performed at six temperatures ranging from room temperature to 1000 °C to explore the effect of temperature on the mechanical properties, and the microstructure and fracture mechanism was investigated by combining electron backscatter diffraction, transmission electron microscopy, and atom probe tomography. In comparison with the properties of conventionally fabricated Inconel 625 alloys, the mechanical properties at room temperature are essentially the same. However, the plasticity of the Inconel 625 alloys fabricated by LPBF is drastically decreased with increasing temperature, especially when the temperature exceeds 700 °C due to the transformation from transgranular ductile fracture to intergranular fracture. Detailed characterization of cracks and grain boundaries (GBs) reveals significant segregation of non-metallic elements at GBs, which impedes the movement of GBs and decreases their strength, thus enhancing the intergranular embrittlement and resulting in the drastic reduction of ductility. Moreover, the irregular grain morphologies result in numerous GBs directional sharp changes and steps, as well as GBs triple junctions, in which the stress concentration is further enlarged, thus promoting the nucleation of voids and cracks and its associated high temperature embrittlement. The underlying mechanism of ductility deterioration of LPBF-fabricated Inconel 625 alloy at elevated temperatures would provide important insights into its performance at high temperatures.

Reduced Volume Expansion of Micron-Sized SiOx via Closed-Nanopore Structure Constructed by Mg-Induced Elemental Segregation.

The inherently huge volume expansion during Li uptake has hindered the use of Si-based anodes in high-energy lithium-ion batteries. While some pore-forming and nano-architecting strategies show promises to effectively buffer the volume change, other parameters essential for practical electrode fabrication, such as compaction density, are often compromised. Here we propose a new in situ Mg doping strategy to form closed-nanopore structure into a micron-sized SiOx particle at a high bulk density. The doped Mg atoms promote the segregation of O, so that high-density magnesium silicates form to generate closed nanopores. By altering the mass content of Mg dopant, the average radii (ranged from 5.4 to 9.7 nm) and porosities (ranged from 1.4 % to 15.9 %) of the closed pores are precisely adjustable, which accounts for volume expansion of SiOx from 77.8 % to 22.2 % at the minimum. Benefited from the small volume variation, the Mg-doped micron-SiOx anode demonstrates improved Li storage performance towards realization of a 700-(dis)charge-cycle, 11-Ah-pouch-type cell at a capacity retention of >80 %. This work offers insights into reasonable design of the internal structure of micron-sized SiOx and other materials that undergo conversion or alloying reactions with drastic volume change, to enable high-energy batteries with stable electrochemistry.