Precipitation Of Secondary Phases Research Articles

Effect of Secondary Phase on Passivation Layer of Super Duplex Stainless Steel UNS S 32750: Advanced Safety of Li-Ion Battery Case Materials.

Aluminum, traditionally the primary material for battery casings, is increasingly being replaced by UNS S 30400 for enhanced safety. UNS S 30400 offers superior strength and corrosion resistance compared to aluminum; however, it undergoes a phase transformation owing to stress during processing and a lower high-temperature strength. Duplex stainless steel UNS S 32750, consisting of both austenite and ferrite phases, exhibits excellent strength and corrosion resistance. However, it also precipitates secondary phases at high temperatures, which are known to form through the segregation of Cr and Mo. Various studies have investigated the corrosion resistance of UNS S 32750; however, discrepancies exist regarding the formation and thickness of the passivation layer. This study analyzed the oxygen layer on the surface of UNS S 32750 after secondary-phase precipitation. The microstructure, volume fraction, chemical composition, and depth of O after the precipitation of the secondary phases in UNS S 32750 was examined using FE-SEM, EDS, EPMA and XRD, and the surface chemical composition and passivation layer thickness were analyzed using electron probe microanalysis and glow-discharge spectroscopy. This study demonstrated the segregation of alloy elements and a reduction in the passivation-layer thickness after precipitation from 25 μm to 20 μm. The findings of the analysis aid in elucidating the impact of secondary-phase precipitation on the passivation layer.

Microstructure characteristics and degradation behaviors of medical rare-earth Mg-10.6Gd-0.3Ag-x(Y/Zn) alloys in vitro

Due to excellent biological-functionality, unique/suitable elastic-modulus as well as spontaneous degradation behaviors, Mg alloys acted as medical implants have shown enormous potential in surgical operation and bone-fixation fields. Unfortunately, the extreme mass loss and unmarked-fracture could easily induce the implant failure. In the present study, the microstructure characteristics and degradation behaviors of the Mg-10.6Gd-0.3Ag-x(Y/Zn) alloys were investigated through the XRD, TEM, EPMA, XPS, 3D/CLSM and SECM. Results revealed that with the increment of Y/Zn contents, the amount of Mg24(Gd/Y)5 precipitates increased, which were mainly distributed in grains and on grain boundaries. The addition of Zn and Y increased the undercooling and Y had a large mismatch degree with Mg atoms, which could promote the precipitation of second phases. Additionally, the corrosion rates of Mg-10.6Gd-0.3Ag-x(Y/Zn) increased firstly and then reduced. Also, the best corrosion resistance was achieved in the Mg-10.6Gd-0.3Ag-Y-Zn, with the current intensities of 58.49 μA/cm2, attributed to the formation of continuous reticular structure oxide film, which can act as physical barriers and impede the corrosion process.

Constructing high-density dislocations by primary (Nb,Ti)(C,N) to induce massive secondary precipitations in austenitic heat-resistant cast steel

The microstructural evolution and the high-temperature tensile properties of a novel Nb-Ti-N alloyed austenitic heat-resistant cast steel were investigated during the isothermal aging at 900 °C for up to 1000 h. The mechanisms of enhancing strength-ductility synergy and the high-temperature tensile fracture behaviors after the aging process were analyzed in detail through tensile tests at 900 °C. Obtained results show that the high-density dislocation regions and the Cr segregation, formed around the intragranular primary (Nb,Ti)(C,N), provided numerous nucleation sites for submicron-sized secondary M23C6 precipitates. The density of secondary M23C6 significantly increased, while the coarsening rate was notably reduced during the aging process. Simultaneously, the uniform dispersed precipitation of nano-sized secondary (Nb,Ti)C was promoted by massive dislocations, which exhibited high resistance to coarsening during long-term aging. The improvement of high-temperature strength was attributed to the precipitation strengthening effects induced by the submicron-sized M23C6 and nano-sized (Nb,Ti)C particles. Additionally, the enhancement of ductility during aging was mainly due to the more effective stress transmission and the ameliorated interface relationship between primary (Nb,Ti)(C,N) and austenitic matrix, which was facilitated by the abundant precipitation of secondary phases. The current findings indicate that high-density dislocations constructed by the intragranular primary (Nb,Ti)(C,N) induce the extensive dispersion of secondary strengthening phases, which enhanced both ultimate tensile strength of 158 MPa and elongation of 45.3% at 900 °C after isothermal aging for 1000 h.

Manipulating the mechanical strength and thermal conductivity of a Mg–4Zn-0.6Zr alloy through Ca addition

In this study, the microstructure, mechanical properties, and thermal conductivity of as-extruded Mg–4Zn-0.6Zr-xCa (x = 0, 0.3, 0.6, 0.9 wt%) alloys were investigated. The results revealed a bimodal grain size distribution in all the alloys due to incomplete dynamic recrystallization (DRX), characterized by the coexistence of elongated deformed grains and equiaxed DRX grains. The bimodal grain size distribution enhanced the mechanical properties of the studied alloys. Furthermore, Ca alloying facilitated the formation of Ca2Mg6Zn3 phases, through which the DRX extent was also enhanced. The precipitation of secondary phases, along with the increased DRX induced by Ca addition, was beneficial in eliminating the lattice distortion of the alloys, resulting in improved thermal conductivity compared to the Ca-free Mg–4Zn-0.6Zr alloy. The optimum combination of mechanical properties and thermal conductivity was achieved in the Mg–4Zn-0.6Zr-0.6Ca alloy, with yielding strength, ultimate tensile strength, tensile fracture elongation, and thermal conductivity values of 271 MPa, 318 MPa, 17.6 %, and 123.9 W/(m‧K), respectively. This work demonstrates that Mg–Zn–Zr–Ca-based alloys can be developed with high strength and high thermal conductivity, significantly expanding the industrial application of magnesium alloys.

Study of Precipitated Secondary Phase at 700 °C on the Electrochemical Properties of Super Duplex Stainless Steel AISI2507: Advanced High-Temperature Safety of a Lithium-Ion Battery Case.

Super duplex stainless steel (SDSS) is a suitable structural material for various engineering applications due to its outstanding strength and corrosion resistance. In particular, its high-temperature strength can enhance the safety of electronic products and cars. SDSS AISI2507, known for its excellent strength and high corrosion resistance, was analyzed for its microstructure and electrochemical behavior at the ignition temperature of Li-ion batteries, 700 °C. At 700 °C, AISI2507 exhibited secondary phase precipitation values of 1% and 8% after 5 and 10 h, respectively. Secondary phase precipitation was initiated by the expansion of austenite, forming sigma, chi, and CrN phases. The electrochemical behavior varied with the fraction of secondary phases. Secondary phase precipitation reduced the potential (From -0.25 V to -0.31 V) and increased the current density (From 8 × 10-6 A/cm2 to 3 × 10-6 A/cm2) owing to galvanic corrosion by sigma and chi. As the fraction of secondary phases increased (From 0.0% to 8.1%), the open circuit potential decreased (From -0.25 V to -0.32 V). Secondary phase precipitation is a crucial factor in reducing the corrosion resistance of SDSS AISI2507 and occurs after 1 h of exposure at 700 °C.

Effect of Ce on the Segregation and Secondary-Phase Precipitation During the Solidification of S31254 Super-Austenitic Stainless Steel

Effect of Ce on the Segregation and Secondary-Phase Precipitation During the Solidification of S31254 Super-Austenitic Stainless Steel

Crystallization of Secondary Phase on Super-Duplex Stainless Steel SAF2507: Advanced Li-Ion Battery Case Materials

The demand for Li-ion batteries has increased because of their extensive use in vehicles and portable electronic devices. This increasing demand implies greater interaction between batteries and humans, making safety a paramount concern. Although traditional batteries are fabricated using Al, recent efforts to enhance safety have led to the adoption of AISI304. The strength and corrosion resistance of AISI304 are greater than those of Al; however, issues such as stress-induced phase transformation and low high-temperature strength have been observed during processing. Duplex stainless steel SAF2507, which is characterized by a dual-phase structure consisting of austenite and ferrite, exhibits excellent strength and corrosion resistance. Although SAF2507 demonstrated outstanding high-temperature strength up to 700 °C, it precipitated a secondary phase. The precipitation of this secondary phase, believed to be caused by the precipitation of the carbides of Cr and Mo, has been extensively studied. Research on the precipitation of the secondary phase near 1000 °C has been conducted owing to the annealing temperature (1100 °C) of the SAF2507 solution. The secondary phase precipitates at approximately 1000 °C because of slow cooling rates. However, few studies have been conducted on the precipitation of the secondary phase at approximately 700 °C. This study analyzed the precipitation behavior of the secondary phase at 700 °C when SAF2507 was applied and assessed its safety during heat generation in Li-ion batteries. The precipitation behavior was analyzed using field emission scanning electron microscopy for morphology, energy-dispersive X-ray spectroscopy for composition, and X-ray diffraction for phase identification.

Study on Microstructure and Properties of Cold Metal Transfer and Pulse Hybrid Welded Super Duplex Stainless Steel

The investigation focuses on the microstructure, impact toughness, and pitting corrosion resistance of cold metal transfer and pulse hybrid welded joints of unified numbering system (UNS) S32750 duplex stainless steel. The results show that the filler pass exhibits the highest austenite ratio (47.9%), whereas the heat‐affected zone (HAZ) shows the lowest (32.3%). Notably, secondary austenite (γ2) is present in both the backing pass and HAZ, but conspicuously absent in the filler pass, indicating that reheating from subsequent weld pass is a prerequisite for the precipitation of γ2. Additionally, chromium nitride (Cr2N) also precipitates in the HAZ and backing pass. Comparative analysis with the weld metal (WM) and base metal (BM) indicates that the HAZ displays lower impact toughness, primarily attributing to imbalanced phase ratio, coarse ferrite grains and the brittle Cr2N. Owing to the lower austenite content and Cr2N precipitation in the backing pass, its toughness (122.6 J cm−2) is found to be inferior to that of the filler pass (130.1 J cm−2). Furthermore, the HAZ with a lower critical pitting temperature compared to the WM (79.1 °C) and BM (87 °C), and exhibits the worst pitting corrosion resistance due to the abundant precipitation of secondary phases and excessive ferrite with low pitting resistance equivalent number.

Failure analysis of an AISI 310 stainless steel beam reinforcement fracture during service in a rolling beam furnace

This work investigated the premature failure of a beam reinforcement made of austenitic stainless steel AISI 310 used in the entrance of a rolling beam furnace working continuously at cycles from 650 to 850 °C. Fracture surface and microstructural investigations allowed to identify the fracture mechanism as fatigue failure. The fracture was probably initiated at the oxidized grain boundaries at an early stage of service life, when no microstructure degradation was present, while most of the fatigue crack propagation occurred after the precipitation of secondary phases. The microstructure investigation revealed severe microstructure degradation with the presence of intermetallic sigma (σ) phase (area fraction = 19 %) and M23C6 carbides (area fraction = 1 %), which were formed during the high-temperature exposure. Cracking of σ phases and decohesion at σ /austenite matrix interfaces were observed near the fracture and in the small punch test samples. Such discontinuities provide an easy path for crack propagation.

Thermal Mechanical Behavior and Microstructure Characteristics of As‐Cast FeCrNiAl Steel

To find the suitable deformation temperature range for the as‐cast Fe–5.5Cr–5.5Ni–3.0Al–0.27C high‐strength lightweight steel, the thermal mechanical behavior and the dependent microstructure characteristics are studied to investigate the high‐temperature mechanical response of the steel. In the results, it is shown that the microstructure of the steel owns a dendrite framework consisting of the martensite dendrite and the interdendritic austenite, among which precipitations of NiAl, Ni3Al, and δ‐Fe are induced by high‐temperature deformation. The flow stress dependence of deformation temperature shows two different variation tendencies, corresponding to the varied deformation mechanisms of strain‐induced precipitation of second phases and δ‐Fe nucleation, and then resulting in different variation of dislocation density. It is found that a periodical fluctuation of flow stress appears as the alternative occurrence of first rise and then drop followed by drop and rise, and the phenomenon is inferred to be caused by local dynamic recrystallization in the dendrites and the neighboring interdendritic spacings.

Study of Electroless Nickel Plating on Super Duplex Stainless Steel for Lithium-Ion Battery Cases: Electrochemical Behaviour and Effects of Plating Time

With increasing demand for Li-ion batteries, studies are focusing on enhancing battery performance and safety. However, studies on battery cases remain scarce. Herein, we propose the use of super duplex stainless steel SAF2507, which is a two-phase (austenite + ferrite) steel, for battery casings. Unlike conventional AISI304, SAF2507 maintains its corrosion resistance and strength at high temperatures and precipitates a secondary phase at approximately 975 °C. However, the effects of Ni plating on this secondary phase are not well documented. Therefore, the electroless Ni plating of SAF2507 after secondary-phase precipitation was studied. Briefly, heat treatment at 1000 °C was used to induce precipitation, and the electroless Ni plating behaviour over varying plating periods was analysed using open-circuit potential, potentiodynamic polarisation, and electrochemical impedance spectroscopy measurements. The plating state and corrosion behaviour were examined using scanning electron microscopy. Heat-treated SAF2507 steel with a secondary phase exhibited excellent electroless Ni plating behaviour, which enhances the safety and durability of Li-ion batteries. Furthermore, uniform plating and electrochemical behaviour were achieved after 180 s, suggesting that SAF2507 is superior to AISI304. These findings contribute to the development of safer and more efficient batteries and address the growing demand for Li-ion battery case materials.

Nanostructuring of Ferritic Steel: A Review on Enhanced Surface Properties Using Ultrasonic Shot Peening

Nanostructuring of ferritic stainless steel refers to the process of intentionally reducing the grain size of the material at the nanoscale level. By manipulating the microstructure of the steel, it is possible to enhance its mechanical, physical, and chemical properties. Nanostructuring can significantly improve the strength, hardness, and wear resistance of ferritic stainless steel, while still maintaining its corrosion resistance. The increased density of grain boundaries and the complex dislocation network within the nanostructured material contribute to these improved properties. Moreover, the nanostructured ferritic stainless steel exhibits enhanced thermal stability, leading to better high-temperature performance and resistance to creep deformation. The small grain size also allows for increased precipitation of secondary phases, such as carbides, nitrides, or intermetallic compounds, which can further improve the material's properties. There are several methods to achieve nanostructuring in ferritic stainless steel, such as severe plastic deformation (SPD) techniques like high-pressure torsion, equal channel angular pressing, and accumulative roll bonding. These techniques impose extreme plastic deformation on the material. Leading to grain refinement below the micrometre range. Also, a novel method of surface nanostructuring ultrasonic shot peening (USP) is discussed in detail. Shot peening is a process in which small, spherical media, typically made of steel or ceramic, called "shots," are propelled onto the surface of a material at high velocities. Ultrasonic shot peening enhances the traditional shot peening process by introducing high-frequency vibrations to the shots. These vibrations are generated by an ultrasonic transducer, which is immersed in a bath of shots and liquid. The vibrations are transmitted through the liquid to the shots, causing them to collide with the surface of the ferritic steel at even higher velocities and energy levels than in traditional shot peening. In summary, nanostructuring of ferritic stainless steel offers great potential for tailoring the material's properties to meet specific application requirements, including improved strength, hardness, wear resistance, corrosion resistance, and high-temperature performance. USP is an effective surface treatment method for ferritic steel, offering advantages in terms of fatigue life, stress corrosion cracking resistance, surface hardness, and wear resistance.

Temperature field simulation and microstructure study of WAAM fabricated Mg-Gd-Y-Zn-Zr alloy

A new combined heat source model was established to more accurately simulate the shape and temperature distribution of the molten pool in additive manufacturing. The model was verified by comparing experimental and simulated results. Experimental and simulation studies have ascertained that the cooling rate of the liquid phase directly impacts the microstructure, thereby significantly affecting the performance of the fabricated parts. When the inter-layer cooling time is controlled at 400 seconds to maintain a thermal accumulation temperature below 246°C, the liquid phase cooling rate is between 2295 °C/s and 1395 °C/s. Under these manufacturing conditions, a profusion of networked secondary phases precipitate along the grain boundaries, primarily composed of rod-like LPSO structures and Mg5(Gd,Y,Zn). Employing this process can notably enhance the performance across different regions of the formed parts, with the hardness reaching up to 110.4 HV, yield strength up to 223 MPa, and compressive strength up to 498 MPa.

Microstructural damage assessment in alloy 617M near high cycle fatigue threshold at elevated temperature

AbstractHigh cycle fatigue (HCF) behavior of Ni superalloy 617M is investigated at 973 K and R‐ratio −1 on a resonance‐based fatigue testing system at 85 Hz frequency. The alloy experiences an abrupt drop in fatigue life within a narrow domain of 2.5–5 MPa near its fatigue strength at 320 MPa. Electron microscopy and diffraction techniques were employed to thoroughly analyze the nominal fatigue damage. The characterization revealed the significance of precipitation of secondary phases M23C6, Ti (C, N), and γ′ phase in dictating the HCF strength of the alloy. Cyclic loading at high temperature causes γ‐matrix hardening and secondary phase precipitation synergistically strengthening the material beyond its yield strength. Conjunctively, dynamic strain aging was also seen to play a major role in the evolution of fatigue damage. The work highlights the collective contribution of γ′‐phase precipitation, carbides, and dynamic strain aging and their influence on the HCF behavior of alloy 617M.

Secondary Phase Precipitation in Fe-22Mn-9Al-0.6C Low-Density Steel during Continuous Cooling Process.

Secondary phase precipitation in Fe-22Mn-9Al-0.6C low-density steel was investigated during a continuous cooling process with different cooling rates through a DIL805A thermal expansion dilatometer, and the changes in microstructures and hardness by different cooling rates were discussed. The results showed that the matrix of the Fe-22Mn-9Al-0.6C was composed of austenite and δ-ferrite; moreover, the secondary phases included κ-carbide, β-Mn and DO3 at room temperature. The precipitation temperatures of 858 °C, 709 °C and 495 °C corresponded to the secondary phases B2, κ-carbide and β-Mn, respectively, which were obtained from the thermal expansion curve by the tangent method. When the cooling rate was slow, it had enough time to accommodate C-poor and Al-rich regions in the austenite due to amplitude modulation decomposition. Furthermore, the Al enrichment promoted δ-ferrite formation. Meanwhile, the subsequent formation of κ-carbide and β-Mn occurred through the continuous diffusion of C and Mn into austenite. In addition, the hardness of austenite was high at 0.03 °C/s due to the κ-carbide and β-Mn production and C enrichment, and it was inversely proportional to the cooling rate. It can be concluded that the presence of κ-carbide, DO3 and β-Mn produced at the austenitic/ferrite interface when the cooling rate was below 0.1 °C/s resulted in κ-carbide and β-Mn precipitating hardly at cooling rates exceeding 0.1 °C/s, which provides a guideline for the industrial production of Fe-Mn-Al-C low-density steel in the design of the hot working process.

The role of secondary phase precipitates in zircaloy corrosion: From point defects to local percolation

A thin oxide film on NZ alloy (Zr-1Sn-0.3Nb-0.3Fe-0.1Cr) was formed to investigate the correlation of microstructure and corrosion behavior at the initial stage by directly identifying defect-enriched sites. The sites of high conductivity are revealed and labelled by silver deposition, and in the further investigation of microstructure secondary phase precipitates (SPPs) interconnected with micro cracks are found below. Enrichment of oxygen-18 and deuterium in SPPs after isotopic tracing by secondary corrosion highlights their influence on carrier diffusion. Thus, the percolation for corrosion media transportation is reached locally by SPPs interconnected with micro cracks.

Aging temperature effect on the phase composition, microstructure, and selected mechanical properties of non-equiatomic TiZrNbTaMo/Mn HEAs targeted for biomedical implants

High entropy alloys (HEAs) have been developed for many applications and recognized for their superior strength, ductility, and corrosion resistance, attracting the attention for biomedical applications. This study aims to evaluate the effect of aging treatment at distinct temperatures on the phase composition, microstructure, and selected mechanical properties of non-equiatomic TiZrNbTaMo and TiZrMoNbTaMn HEAs for potential use as biomedical implants. The TiZrNbTaMn sample exhibited a single BCC phase, while the TiZrNbTaMo a major BCC and minor HCP phases. The microstructure of the TiZrNbTaMo sample was composed of BCC grains with some acicular precipitations of the HCP phase in the grain boundaries, having the aging temperature acted in the grain growth and secondary phase precipitation. Contrarily, the TiZrNbTaMn sample exhibited larger BCC grains permeated with a minor amount of acicular structures, which were entirely decomposed with the aging treatments. The semi-quantitative chemical analysis indicated that the phase composition was a result of elemental chemical segregation, having the refractory metals (Mo, Ta, and Nb) preferentially located in the inner region of the grains, while the other ones (Ti, Zr, and Mn) in the grain boundary. The aging treatment acted in the phase precipitation/dissolution oppositely on the samples through the atomic diffusion mechanism induced by the temperature. The elastic modulus and Vickers microhardness were sensitive to the chemical and phase composition of the samples, having the TiZrNbTaMo aged at 773 K achieved better performance than the commercial Ti-6Al-4 V alloy for use as biomedical implants.

Effect of CaF2 on the preparation and optical property of MgAl2O4 transparent ceramics

To achieve optimal light transparency in MgAl2O4 transparent ceramics, a higher sintering temperature is required to eliminate pores. However, inevitable rapid grain growth occurs, leading to lower mechanical properties. To address this problem, calcium fluoride (CaF2) is utilized as a sintering additive to enhance the transparency of MgAl2O4 ceramics. The influence of CaF2 on the densification process and microstructure evolution is investigated. CaF2 demonstrates notable abilities in facilitating densification and lowering the sintering temperature. Moreover, it inhibits grain growth during the final sintering stage. However, the sintering temperature must be controlled because the secondary phases (calcium aluminate) precipitate at a higher temperature, thereby affecting the homogeneity of the ceramic microstructure. After optimizing the sintering process, ceramics (with a thickness of 5 mm) containing 0.05 wt% CaF2 exhibited the highest in-line transmittance of 81 % and 87 % in the visible and near-infrared wavelengths, respectively, after pre-sintering at 1505 °C for 3 h and subsequent hot isostatic pressing (HIPing) at 1550 °C for 3 h.

Strengthening and control of second-phase particle precipitation in ferritic/austenitic/martensitic heat-resistant alloys: a review

Strengthening and control of second-phase particle precipitation in ferritic/austenitic/martensitic heat-resistant alloys: a review

Reactive transport modelling of tailings hydrogeochemistry under a composite cover

Quantitative forecasts of acid mine drainage (AMD) production are important for remediation planning. Reactive transport simulations corresponding to a detailed sampling location at a covered legacy tailings impoundment in northern Ontario, Canada, were conducted to quantitatively assess the predominant hydrogeochemical reactions. The simulations span the period from the end of tailings deposition (circa 1970) to early 2020, 12 years after remediation by a five-layer composite cover. The conceptual model of uncovered tailings weathering and subsequent geochemistry of the covered tailings system was implemented in 1D using the multi-component reactive transport code MIN3P. Transient monthly infiltration, post-cover boundary condition changes, and a dynamic temperature regime were incorporated. The shrinking core model, including parallel O2(aq) and Fe3+ oxidation reactions for the waste rock in the cover and the underlying tailings, was implemented to simulate the oxidation of As-bearing pyrite, chalcopyrite, and sphalerite. Primary carbonate and aluminosilicate host minerals promoted acid-neutralization reactions. Precipitation of secondary phases and sorption/desorption of Cu, Zn, and arsenite were incorporated into the model. The overall agreement between key simulated and field-measured post-cover aqueous geochemical parameters suggests that the conceptual model captured the primary hydrogeochemical processes in the covered tailings. A lack of reliable data on initial tailings mineralogy and pre-cover hydrogeochemistry increased simulation uncertainty. Simulated reaction rates indicate that where intact, the cover decreased sulfide oxidation rates by both O2(aq) and Fe3+ and improved pore-water quality over time. Simulation results indicate that elevated concentrations of Zn and As are likely to persist in the tailings regardless of cover performance, whereas concentrations of Cu and Al are the parameters most sensitive to cover effectiveness.