Microstructural stability of long-term aged wrought Ni–Fe-based superalloys

The influence of long-term thermal exposure on the microstructure and microhardness of a new Ni–Fe-based superalloy, for advanced ultra-supercritical coal-fired power plants, was studied. Spherical γ′ particles were coarsened with the increase of aging time, while the volume fraction of γ′ was decreased. The amount of M₂₃C₆ carbides was increased with aging time at 750°C, and the coarsening rate of the width of M₂₃C₆ was consistent with that of the LSW model. The microhardness of the alloy was maintained following 935?h of aging time and then was slightly decreased. It was found that the transition from the strongly coupled dislocations model to the Orowan model was dependent on the size and volume fraction of γ′.     

Effects of heat treatments on the microstructure and mechanical properties of Rene 80

Effects of heat treatments on room temperature mechanical properties and stress-rupture properties of Rene 80 have been investigated. The microstructures were analyzed by optical microscope and scanning electron microscope after each step of heat treatments. With the decrease of aging temperature, the average size of γ′ phase decreases, but the volume fraction of γ′ phase increases. The lower aging temperature suppresses the growing of the coarse γ′ particles, but facilitates the growth of the fine γ′ particles. After the optimum heat treatment, the ultimate tensile strength and yield strength are respectively higher than 1040 MPa and 950 MPa, the stress-rupture life at 871 °C/310 MPa is higher than 170 h with excellent ductility. The improved tensile strength and stress-rupture life are primarily due to the increased volume fraction of γ′ phase. The borides precipitate at grain boundaries at about 913 °C. The primary MC is found to decompose into M₆C at about 873 °C and M₂₃C₆ at 840–873 °C at grain boundaries. The precipitate of the carbides may partly contribute to the improved mechanical properties.     

Precipitation hardening in Inconel* 625

Abstract

The hardness of the nickel based superalloy Inconel 625, aged at 625, 700, and 760°C for different intervals of time ranging from 1 to 335 h, has been measured. Peak hardening is found to occur much earlier at 760°C than at 700°C. Also the peak hardness is higher at 700°C than at 760°C. The results have been discussed in terms of precipitation. Scanning electron microscopy revealed the presence of precipitates in specimens aged at 760°C for a longer time. Electron probe microanalysis results show these precipitates to be rich in Ni, Nb, and Mo indicating that these are γ″ precipitates of Ni₃ (Nb, Mo) type. Transmission electron microscopy confirmed that these are γ″ precipitates. It also suggests that nucleation takes place heterogeneously on dislocations and stacking faults. Longer aging causes somewhat uniform nucleation but still preferentially on the secondary defects. At 700°C γ′ precipitates have been observed in addition to γ″ precipitates. The orientation relationship between the precipitates and the matrix has also been determined.     

Phase evolution and crystallography of precipitates during decomposition of new “tungsten-free” Co(Ni)–Mo–Al–Nb γ–γ′ superalloys at elevated temperatures

This article reports the microstructural stability and consequent phase decomposition including the appearance of topologically close-packed (TCP) phases at high temperature of recently discovered tungsten-free γ–γ′ alloys of base composition Co–10Al–5Mo–2Nb with or without the addition of Ni and Ti. On prolonged aging at 800 °C of the Co–10Al–5Mo–2Nb alloy, needle-shaped DO₁₉-ordered precipitates with stoichiometry of Co₃(Mo, Nb) start appearing in the microstructure. In addition, growth of cellular domains from the grain boundaries featuring a three-phase composite lamellar structure could be observed. These phases are fcc γ-Co with composition different from the original matrix, CoAl with B2 ordering and Co₃(Mo, Nb) with DO₁₉ ordering. All the phases exhibit well-defined crystallographic orientation relationships. The decomposition of the alloys depends on the solvus temperature of the γ′ phase. The Ni-containing alloy exhibits no phase decomposition until 100 h of aging at 800 °C without any significant effect on γ′ volume fraction (76 %). However, at 950 °C, the alloy decomposes leading to the appearance of four different phases including TCP phases: a Cr₃Si-type cubic phase, a hexagonal Laves phase, rhombohedral μ phase, and solid solution of Co phase. The γ–γ′ microstructure in the Co–10Al–5Mo–2Nb and Co–30Ni–10Al–5Mo–2Ta alloys is not stable at 800 and 950 °C, respectively, on long-term aging. This shows that the measured solvus temperatures (i.e., 866 and 990 °C) are metastable solvus temperatures. We also report that the Ti-containing alloy exhibits superior stability with no evidence of either TCP phase formation or any other decomposition of γ′ precipitates, even after aging at 950 °C for 100 h.     

Isothermal aging–microstructure–property relationship of SmCo 2:17 magnets

Abstract

The isothermal aging–microstructure–magnetic property relationship of a SmCo 2:17 alloy was investigated in the present study. The alloy also contained Fe, Cu and Zr as major addition. Its magnetic properties, including intrinsic coecivity H _ci, remanence B _r and maximum energy product (BH)_max, were obtained from the measured second quadrant M–H hysteresis curves. The microstructure of the alloy was characterised using X-ray diffraction (XRD) and TEM. It was found that, as the one step aging temperature was increased from 850 to 900°C, the remanence of the SmCo 2:17 alloy magnet was increased while its coercivity was reduced. The maximum energy product (HB)_max of the magnet was significantly improved by applying a two step aging, consisting of aging first at 900°C followed by aging at 850°C. Based on XRD and TEM analyses, effects of the aging condition on the microstructure and magnetic properties were discussed. The microstructural change observed in the current work included cell size of the cellular structure and the degree of Cu segregation at the cell boundaries. Change in the degree of Cu segregation at the cell boundaries might be the major cause for the change in coercivity of the alloy aged in different aging conditions. The effect of aging condition on the remanence could be attributed to the effect of aging condition on cell size of the cellular structure, which affects the volume fraction of SmCo 2:17 phase in the alloy.     

Precipitation of second phases in aged Ni rich NiTiRe shape memory alloy

Abstract

This study investigated the effect of aging on the structure and precipitation of second phases of Ni₅₂Ti_47·7Re_0·3 shape memory alloys. The alloy was solutionised at 1000°C for 24 h before aging at various temperatures ranging from 300 to 600°C for 3 h. The matrix phase in both solutionised and aged specimens was martensite. Ti₂Ni phase was also present in the microstructure of both solutionised and aged specimens and its volume fraction decreased as the aging temperature increased. Ni₄Ti₃ phase began in appearance by increasing aging temperature to 400°C. Ni₄Ti₃ precipitates had lenticular and non-geometry shapes. Aging at 600°C led to precipitation of Ni₃Ti phase in the microstructure. This precipitated phase formed in white blocky shapes. Ti/Ni ratio increased and/or Ni content decreased in the matrix with increasing in aging temperature.     

Influence of thermal exposure on γ′ precipitation and tensile properties of DZ951 alloy

The effect of long-term exposure on the γ′ phase and the tensile behavior of a directionally solidified nickel-base superalloy DZ951 was investigated. Alloys after standard heat treatment (SHT) were isothermally aged at 900 °C up to 2000 h and tensile tests were performed in both SHT and aged conditions at various temperatures. The morphology of the γ′ phase changes from cuboid to rafting and the size increases from 300 nm at SHT to 930 nm, and the volume fraction of the γ′ phase decreases from 70% at SHT to 65% during aging at 900 °C for 2000 h. The changing trend of yield stress at different test temperatures is similar. The yield stress decreases slightly at 600 °C. This arises from few dislocations shearing the γ′ precipitates. There is a peak yield stress value at 760 °C, which is attributed to the high strength of the γ′ phase, the homogeneous deformation structure, and dislocation-γ′ precipitate and dislocation–dislocation interactions. The yield stress then decreases rapidly with increased temperature. The low strength of the γ′ phase and γ′ rafting at high temperature contribute to the drop of yield stress. The change of tensile elongation is inverse to that of yield stress. The yield stress continuously decreases with the increase of aging time at 900 °C. This arises from the coarsening of γ′ and a decrease in the γ′ volume fraction.     

Precipitation behaviour of β and γ′ in high Al low thermal expansion superalloy

Abstract

The precipitation behaviour of β and γ′ in a low thermal expansion superalloy IN783 was investigated. It was demonstrated that coarse γ′ precipitates do form during β aging at 845°C. During aging at lower temperatures, not only fine γ′ particles are formed, the coarse γ′ particles also change from spherical to cuboidal. Therefore, a bimodal distribution of γ′ is formed in the matrix after standard aging treatment. The formation of β consumes Al atoms, which constrains the formation of coarse γ′ in the zone around β during aging at 845°C. During γ′ aging, a fine γ′ precipitating zone is formed around β. Prolonging the β aging duration markedly promotes the formation of β at grain boundaries and in the matrix, significantly enlarges the fine γ′ precipitating zone and influences the precipitation of coarse γ′.     

Correlation between ultrasonic velocity and solutionising time in Rene 80 superalloy

Abstract

Ultrasonic measurements have been used to characterise the solutionising phenomenon in Rene 80, a Ni based superalloy. Starting material was solutionised at 1204°C for 30–120 min on identical samples. The microstructures of these samples were evaluated by ultrasonic immersion technique, X-ray diffraction and scanning electron microscopy. It was observed that the area fractions and, consequently, the γ′ volume fractions were decreased by increasing the solutionising time. A direct correlation was observed between ultrasonic wave velocity and solutionising time at 1204°C. The ultrasonic compression wave velocity followed a descending pattern similar to that of γ′ area fraction with the increase in solutionising time. The observed variation in ultrasonic velocity has been attributed to the effect of the γ′ dissolution on the elastic constants of the material.     

Dissolution and precipitation kinetics of γ' in nickel base superalloy Udimet 520

Abstract

The influence of various solution andaging heat treatments on the dissolution and precipitation kinetics of γ' in wrought nickel base Udimet 520 superalloy was investigated, with the aim of determining optimum preforge and post-forge heat treatment schedules. Solution heat treatments at 1070, 1100, 1110, and 1120°C for 1, 2, and 4 h followed by water quenching were applied. Examination by SEM showed that in specimens solution treated at 1070°C the necklace type microstructure remained and partialagglomeration of γ' precipitates was observed even after 4 h holding. By contrast, after solutionising at 1100°C for 4 h, the γ' volume fraction decreased from 28 to 5% and when solution treated at 1140°C, abnormal grain growth was observed. The optimum solution treatment leading to an almost complete dissolution of γ' particles was determined to be 1120°C/4 h. Double aging treatments were carried out at 925°C/4 h/ AC (air cooled) followed by aging at 700 or 800°C for times ranging from 1 to 100 h. The results indicated that the precipitates have almost spherical shapes at the beginning and as the aging time is increased a partial change to a cuboidal shape is observed. This behaviour was more pronounced when aging at 800°C was employed. Microhardness measurements under both aging conditions showed that at 700°C hardness values increase about 60 HV when γ' particles grow 70 nm. On the other hand, in the samples aged at 800°C, hardness values increase with the particle size until a certain value and then drop. The precipitate growth process was followed by image analysis and the activation energy for γ' growth was evaluated to be 104 kJ mol ^-1. The results obtained are discussed in the framework of classic nucleation theory and compared with other workers' results.     

Analysis of Ostwald ripening in Ni-rich Ni-Ti alloys by diffusion couples

The coarsening kinetics of γ′ precipitates in Ni-rich Ni-Ti alloys are studied using a Ni-11.5 wt% Ti and pure Ni diffusion couple. The formed concentration gradient allowed to study the aging process at 1023 K (750 °C) in Ni-rich Ni-Ti alloys with Ti content from 8.62 to 11.15 wt% Ti. In general, during the coarsening of γ′ precipitates, the experimental coarsening kinetics do not fit well to the LSW or TIDC theoretical models and anomalous behaviour of coarsening rate constant (k _r) associated with γ′ volume-fraction is confirmed at high values.     

Effect of hot working variables on microstructure and brittle to ductile transition in Ti–46.5Al–3Nb–2Cr–0.2W gamma titanium aluminide

Abstract

The microstructure and mechanical properties of a γ-TiAl alloy (Ti–46.5Al–3Nb–2Cr–0.2W, in at.-%) were studied in two conditions: (a) after conventional forging in the +γ phase field and (b) after subsequent isothermal forging in the ₂+γ phase field. Tensile tests were conducted in the temperature range 800–1000°C and strain rate range of 10^-3–10^-1 s^-1. The microstructure of the alloy in condition 1 was non-homogeneous consisting of about 90 vol.-% of small γ grains (grain size of 3 to 20 µm) and 10 vol.-% of coarse grains or lamellar regions. The alloy in this condition showed a brittle to ductile transition at about 950°C and extensive cavitation during deformation above the transition temperature. The microstructure in condition 2 was much more uniform and finer, and the transition temperature was decreased to 850°C. The alloy in condition 2 showed better deformability and cavitation resistance than that in condition 1 and superplastic behaviour at temperatures 900–1000°C.     

Effect of cooling rate on microstructure,microsegregation and mechanical properties of cast Ni-based superalloy K417G

The effects of different solidification rates after pouring on the microstructures,microsegregation and mechanical properties of cast superalloy K417 G were investigated.Scheil-model was applied to calculate the temperature range of solidification.The casting mould with different casting runners was designed to obtain three different cooling rates.The microstructures were observed and the microsegregation was investigated.Also,high temperature tensile test was performed at 900?C and stress rupture test was performed at 950?C with the stress of 235 MPa.The results showed that the secondary dendrite arm spacing,microsegregation,the size and volume fraction of γ'phase and the size of γ/γ'eutectic increased with decreasing cooling rate,but the volume fraction of γ/γ' eutectic decreased.In the cooling rate range of 1.42?C s~(-1)–0.84?C s~(-1),the cast micro-porosities and carbides varied little,while the volume fraction and size of phase and γ/γ' eutectic played a decisive role on mechanical properties.The specimen with the slowest cooling rate of 0.84?C s~(-1) showed the best comprehensive mechanical properties.     

Oxygen-enrichment of YBa2Cu3 YBa2Cu3O7-δ using the fluidization techniqueusing the fluidization technique

The oxygen-deficient phase of the highT _c superconductor, YBa₂Cu₃O₇, was oxygen-enriched using the fluidization technique to give good superconducting properties. The normal method of oxygen treatment at 900°C for 24 h and at 600°C for 24 h has been reduced to just one treatment at 600°C for 12 h by the fluidization technique to achieve almost the same strength of superconducting signal for the YBa₂Cu₃O₇ powder, which establishes the attractiveness of the latter route for the large-scale preparation of superconducting material. The particle sizes were in the range 0–90, 90–180 and 180–420 μm. The fluidized particles were crystalline with orthorhombic distortion.T _c ^onset , estimated using the a.c. magnetic susceptibility method, was 91·3 K. The volume fraction of superconducting material in the product was 83·7–85·3%, one of the highest values reported so far for YBa₂Cu₃O₇.     

Microstructure and mechanical properties of as aged Mg–3Sn–1Al and Mg–3Sn–2Zn–1Al alloy

Effect of Zn on the microstructure, age hardening response and mechanical properties of Mg–3Sn–1Al alloy which is immediately aged at 180°C after extrusion process (T5) was investigated. It was found that the Zn can refine the microstructure, remarkably improve the aging response with the peak hardness increases to 75 HV and the time to peak hardness reduces from ～110 to ～60 h, which is attributed to the solid solution hardening of Al, Zn and an amount of finer Mg₂Sn precipitates. The as aged Mg–3Sn–2Zn–1Al alloy exhibits better mechanical property at room temperature or 150°C than that of Mg–3Sn–1Al alloy, which is ascribed to the fine grained microstructure and thermally stable Mg₂Sn particles dispersed at grain boundaries and in the matrix.     

Formation and characteristics of coarsening resistant cubic sigma phase in AI-4.2Cu-1.6Mg-0.2Si

Abstract

The precipitation and coarsening characteristics of an alloy of nominal composition (wt-%) AI-4.2Cu-l.6Mg-0.2Si were investigated at 200, 265, and 305°C for times up to 650 h. All aging conditions produced a mixture of homogeneously nucleated S′ and the cubic phase σ. The quench rate did not alter appreciably the volume fraction of cubic phase. The lattice parameter of the σ phase was 0.831 ± 0.005 nm and the aspect ratio of the σ precipitates was 1.4 ± 0.1 for treatments at 200 and 265°C, increasing to 1.8 for the specimens aged at 305°C for 24 h. The precipitated σ phase exhibited better resistance to coarsening and dissolution in long term aging treatments at 265°C than the concurrently precipitated S′, although the S′ was a more effective precipitation. hardener.     

Precipitation hardening of Cu – Ti – Zr alloys

Abstract

The influence of age hardening temperature and time on the hardness, tensile properties, electrical conductivity, and microstructure of Cu – 4Ti – 0.1Zr and Cu – 3Ti – 0.1Zr alloys has been investigated. The resulting microstructure of these alloys suggests that zirconium addition prohibited the formation of compositional modulations in the solution treated condition. These alloys exhibited maximum hardness and strength on peak aging at 450°C for 24 h by the formation of a coherent and metastable Cu₄Ti phase (β') in modulated structure while overaging occurred by the formation of equilibrium phase β-Cu₃Ti. The electrical conductivity of both the alloys increased moderately on aging. Unlike in an earlier study of binary Cu – Ti and some ternary Cu – Ti – X alloys, overaging did not cause any discontinuous precipitation in the Cu – Ti – Zr alloys investigated. Modulated structure formed on peak aging persisted on prolonged aging at 450°C for 80 h or at 500°C for 8 h.     

Effect of cooling rate on electrical properties, impulse surge and dc-accelerated aging behaviors of ZPCCD-based varistors

The effect of cooling rate on nonlinear electrical properties, and stability against impulse surge and dc-accelerated aging stress of ZPCCD-based varistors was investigated. The cooling rate relatively slightly affects the microstructure, whereas it did not significantly modify the densification process. The nonlinear coefficient increased with the increase of cooling rate up to 240 °C/h, whereas the further fast cooling rate caused it to decrease. The samples cooled at 240 °C/h exhibited the highest nonlinearity, in which the nonlinear coefficient is 61.6 and the leakage current density is 6.8 μA/cm². The aging was not significantly affected by the specified impulse surge stress, whereas it was greatly affected by dc-accelerated aging stress. The samples cooled at 120 °C/h exhibited the highest stability, in which the variation rate of breakdown field is −5.5% and the variation rate of nonlinear coefficient is −29.1% under continuous stress composed of the specified impulse surge and dc-accelerated aging stress of 0.95 E _B/150 °C/24 h.     

Density and Volume Fraction of Supercritical CO<Subscript>2</Subscript> in Pores of Native and Oxidized Aerogels

The density and volume fraction of an adsorbed phase of carbon dioxide (CO₂) in aerogels was investigated using a formalism based on independent measurements of neutron transmission and small-angle neutron scattering from fluid-saturated absorbers (Rother et al. J. Phys. Chem. C 111, 15736 (2007)). The range of excess fluid pressures (0 <  P <  8 MPa) and temperatures (T = 35°C and 80°C) corresponded to the supercritical regime above the critical temperature T _C = 31.1°C and critical density ρ _C = 0.468 g · cm⁻³ of the bulk fluid. The results demonstrate that a porous aerogel matrix works to create an adsorbed phase with liquid-like fluid densities reaching ~1.1 g · cm⁻³ and ~0.8 g · cm⁻³ at T = 35°C and 80°C, respectively. Thus, despite the fact that the density and volume fraction of the adsorbed fluid both decrease with temperature, the dense adsorbed phase is still present in the aerogel at temperatures far exceeding the T _C. Heat treatment (“oxidation”) of the aerogel at 500°C for 2 h, which removes a significant fraction of the alkyl groups from the aerogel surface, has little effect on the adsorption properties. The observed reduction of the density and volume fraction of the adsorbed CO₂ with temperature and its minor dependence on the surface modification are consistent with predictions of the pore-filling model.     

Effect of thermal ageing on microstructure,mechanical properties,and fracture behaviour of 50 % cold rolled duplex stainless steel (alloy 2507)

The paper deals with cold rolling and ageing on microstructure and mechanical properties of 2507 duplex stainless steel. Microstructure depicts acicular/Widmanstätten austenite and δ-ferrite with dissimilar volume fraction (∼0.55 for ferrite and ∼0.45 for austenite). Cold rolling and ageing at 950 °C, 1000 °C and 1050 °C result in equiaxed austenite for samples solution treated at 1040 °C and elongated at 1300 °C. By lowering ageing temperature from 1050 °C to 950 °C, structure becomes finer from ∼20 μm to <10 μm grain size. The sigma (σ) phase appears after ageing at 950 °C. Micro-hardness reveals maximum hardness for the hot rolled, solutionized (1040 °C) water quenched, and cold rolled (50 %) sample (380 HV_δF 100 and 430 HV_γ 100), whereas the tensile results reveal the hot rolled, solution treated (1300 °C, 1040 °C), cold rolled and aged at 950 °C samples show higher strength (yield strength=625 MPa, 567 MPa and ultimate tensile strength=892 MPa, 826 MPa) and lower ductility (23 %, 32 %) due to the σ-phase. The solution treated (1040 °C), cold rolled, aged at 1050 °C sample exhibits attractive strength and ductility combination (∼30 GPa %). Fractography supports the tensile results.