Reverse Martensitic Transformation and Resulting Microstructure in a Cold Rolled Metastable Austenitic Stainless Steel

The reverse martensitic transformation in cold‐rolled metastable austenitic stainless steel has been investigated via heat treatments performed for various temperatures and times. The microstructural evolution was evaluated by differential scanning calorimetry, X‐ray diffraction and microscopy. Upon heat treatment, both diffusionless and diffusion‐controlled mechanisms determine the final microstructure. The diffusion reversion from α′‐martensite to austenite was found to be activated at about 450°C and the shear reversion is activated at higher temperatures with A_f′ ~600°C. The resulting microstructure for isothermal heat treatment at 650°C was austenitic, which inherits the α′‐martensite lath morphology and is highly faulted. For isothermal heat treatments at temperatures above 700°C the faulted austenite was able to recrystallize and new austenite grains with a low defect density were formed. In addition, carbo‐nitride precipitation was observed for samples heat treated at these temperatures, which leads to an increasing M_s‐temperature and new α′‐martensite formation upon cooling.     

Influence of thermomechanical treatments on the microstructure and mechanical properties of HSLA-100 steel plates

The influence of thermomechanical treatment (TMT), i.e., controlled rolling and direct quenching, as a function of rolling temperature and deformation on the microstructure and mechanical properties of HSLA-100 steel have been studied. The optical microstructure of the direct quenched (DQ) and tempered steel rooled at lower temperatures (800 °C and 900 °C) showed elongated and deformed grains, whereas complete equiaxed grains were visible after rolling at 1000 °C. The transmission electron microscope (TEM) microstructure of the 800 °C rooled DQ steel showed shorter, irregular, and closer martensite laths with extremely fine Cu and Nb(C,N) precipitates after tempering at 450 °C. The precipitates coarsened somewhat after tempering at 650 °C; the degree of coarsening was, however, less compared to that of the reheat-quenched (RQ) and tempered steel, indicating that the DQ steel was slightly more resistant to tempering. Similar to the RQ steel, at a 450 °C tempering condition, the DQ steel exhibited peak strength with extremely poor impact toughness. After tempering at 650 °C, the toughness of the DQ steel improved significantly, but at the expense of its strength. In general, the strength of the DQ and tempered steel was good and comparable to that of the RQ and tempered steel, although, its impact toughness was marginally less than the latter. The optimum combination of strength and toughness in the DQ steels was achieved after 900 °C rolling with 50 pct deformation, followed by direct quenching and tempering at 650 °C (yield strength (YS)=903 MPa, ultimate tensile strength (UTS)=928 MPa, and Charpy V-notch (CVN) strength=143 J at −85 °C).     

Analysis of Particle and Crystallite Size in Tungsten Nanopowder Synthesis

Tungsten nanopowders were synthesized by a low-temperature technique and then heat treated in a gaseous reductive atmosphere in order to study the phase evolution, crystallite size, and particle size of the powders as the heat treatment temperature was modified. Synthesis of the powders was carried out in aqueous media using NaBH₄ as a reducing agent using careful control of the pH of the solutions. The XRD patterns of the as-synthesized powders showed an amorphous phase. After washing, energy dispersive spectroscopy showed that the powders had peaks for oxygen and tungsten. In order to promote crystallization and eliminate the oxygen, the powders were heat treated at 773 K, 923 K, and 1073 K (500 °C, 650 °C, and 800 °C) in a H₂/CH₄ reducing atmosphere for 2 hours. XRD after heat treatment showed α-W peaks for the powders treated at 1073 K and 923 K (800 °C and 650 °C) and a mixture of β-W and α-W for the powders treated at 773 K (500 °C). The crystallite sizes determined from X-ray peak broadening were 12, 16, and 20 nm, whereas the average particle sizes from dynamic light scattering were 260, 450, and 750 nm, for heat treatment temperatures of 773 K, 923 K, and 1073 K (500 °C, 650 °C, and 800 °C), respectively. The average crystallite size and particle sizes increased proportionally with the treatment temperature, in contrast to what has been found for some ceramics, in which as the heat treatment temperature is increased, the crystallite size increases, but the particle size stays constant.     

Structure Homogeneity and Thermal Stability of Austempered Ductile Iron

Solid-state transformation during heat treatment is of great practical importance because it significantly affects the final structure, properties, and thermal stability of cast components. The present study highlights the issue of structure formation and its effect on the thermal stability of high-quality cast iron, namely, austempered ductile iron (ADI). In this study, experiments were carried out for castings with a 25-mm-walled thickness and under variable heat treatment conditions, i.e., austenitization and austempering within ranges of 850 °C to 925 °C and 250 °C to 380 °C, respectively. The X-ray diffraction (XRD) investigations were carried out within a range of − 260 °C to + 450 °C to study the structure parameters related to the XRD tests, which provided information related to the phase participation, lattice parameters, and stresses in the microstructure as well as with an expansion of the crystal lattice. The results also provide insight into the role of the structure and its homogeneity on the thermal stability of ADI cast iron. The present work also aims to develop strategies to suppress the formation of blocky-shaped austenite in the ADI structure to maintain a homogeneous microstructure and high thermal stability.

     

Structure and Properties of High-Temperature Multilayer Hybrid Material Based on Vanadium Alloy and Stainless Steel

The present work is devoted to the development of new structural composite material having the unique complex of properties for operating in ultrahard conditions that combine high temperatures, radiation, and aggressive environments. A new three-layer composite tube material based on vanadium alloy (V-4Ti-4Cr) protected by stainless steel (Fe-0.2C-13Cr) has been obtained by co-extrusion. Mechanism and kinetics of formation as well as structure, composition, and mechanical properties of “transition” area between vanadium alloy and stainless steel have been studied. The transition area (13- to 22-µm thick) of the diffusion interaction between vanadium alloy and steel was formed after co-extrusion. The microstructure in the transition area was rather complicated comprising different grain sizes in components, but having no defects or brittle phases. Tensile strength of the composite was an average 493 ± 22 MPa, and the elongation was 26 ± 3 pct. Annealing at 1073 K (800 °C) increased the thickness of transition area up to 1.2 times, homogenized microstructure, and slightly changed mechanical properties. Annealing at 1273 K (1000 °C) further increased the thickness of transition area and also lead to intensive grain growth in steel and sometimes to separation between composite components during tensile tests. Annealing at 1073 K (800 °C) is proposed as appropriate heat treatment after co-extrusion of composite providing balance between diffusion interaction thickness and microstructure and monolithic-like behavior of composite during tensile tests.

     

Effect of Thermomechanical Treatment on Functional Properties of Biodegradable Fe-30Mn-5Si Shape Memory Alloy

The structure, martensitic γ ↔ ε transformation temperatures, Young’s modulus, mechanical properties, and electrochemical behavior of Fe-30Mn-5Si (wt pct) biodegradable shape memory alloy subjected to various thermomechanical treatments (TMT) comprising hot rolling or cold rolling with post-deformation annealing were characterized by optical microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, differential scanning calorimetry, tensile testing, open circuit potential, and polarization curves measurements in Hanks’ solution, as compared to reference heat treatment. The optimum combination of mechanical properties (low Young’s modulus, high tensile strength, and appropriate ductility) for biomechanical compatibility was obtained after TMT with hot rolling at 600 and 800 °C due to the formation of favorable dynamically polygonized and recrystallized structures and decrease in the γ↔ε transformation starting temperature down to the human body temperature. The TMT did not show a significant effect on the corrosion rate as compared to the appropriate corrosion rate after the reference heat treatment. It is concluded that the TMT with hot rolling at 600 or 800 °C, which provides an optimum combination of the required corrosion rate in the simulation body fluid with high biomechanical compatibility, can be considered a promising treatment of Fe-30Mn-5Si biodegradable alloy for bone implants.

     

Mechanical Properties and Microstructural Characterization of Cu-4.3 Pct Sn Fabricated by Selective Laser Melting

Components were fabricated via selective laser melting (SLM) of prealloyed Cu-4.3 pct Sn powder and heat treated at 873 K and 1173 K (600 °C and 900 °C) for 1 hour. Tensile testing, conductivity measurement, and detailed microstructural characterization were carried out on samples in the as-printed and heat-treated conditions. Optimization of build parameters resulted in samples with around 97 pct density with a yield strength of 274 MPa, an electrical conductivity of 24.1 pct IACS, and an elongation of 5.6 pct. Heat treatment resulted in lower yield strength with significant increases in ductility due to recrystallization and a decrease in dislocation density. Tensile sample geometry and surface finish also showed a significant effect on measured yield strength but a negligible change in measured ductility. Microstructural characterization indicated that grains primarily grow epitaxially with a submicron cellular solidification substructure. Nanometer scale tin dioxide particles identified via X-ray diffraction were found throughout the structure in the tin-rich intercellular regions.

     

Microstructure,Mechanical and Abrasive Wear Behavior of 8.0 wt pct Cr White Iron Subjected to Continuous and Cyclic Annealing Treatment

Continuous annealing treatment (austenitization for 4 hours followed by furnace cooling) and cyclic annealing treatment (four cycles of austenitization, each of 0.66 hours duration followed by forced air cooling) of 8.0 wt pct Cr white iron samples are undertaken at 1173 K, 1223 K, 1273 K, 1323 K, and 1373 K (900 °C, 950 °C, 1000 °C, 1050 °C, and 1100 °C) as steps of destabilizing the as-cast structure. Continuous annealing results in precipitation of secondary carbides on a matrix containing mainly pearlite, while cyclic annealing treatment causes similar precipitation of secondary carbides on a matrix containing martensite plus retained austenite. On continuous annealing, the hardness falls below the as-cast value (HV 556), while after cyclic annealing treatment there is about 70 pct increase in hardness, i.e., up to HV 960. Decrease in hardness with increasing annealing temperature is quite common after both heat treatments. The as-cast notched impact toughness (4.0 J) is nearly doubled by increasing to 7.0 J after both continuous and cyclic annealing treatment at 1173 K and 1223 K (900 °C and 950 °C). Cyclic annealing treatment gives rise to a maximum notched impact toughness of 10.0 J at 1373 K (1100 °C). Abrasive wear resistance after continuous annealing treatment degrades exhibiting wear loss greater than that of the as-cast alloy. In contrast, samples with cyclic annealing treatment show reasonably good wear resistance, thereby superseding the wear performance of Ni-Hard IV.

     

Transformation and Precipitation Kinetics in 30Cr10Ni Duplex Stainless Steel

To improve the microstructure during casting, hot forming, and heat treatment of 30Cr10Ni duplex stainless steel, accurate data on the precipitation and transformation processes at high temperatures are needed. In this article, the precipitation and transformation processes at various aging times in the temperature range 873 K to 1573 K (600 °C to 1300 °C) were studied. The 30Cr10Ni ferrous alloy contains a relatively large amount of Cr, Ni, and C, which results in a complex microstructure. In addition to the ferrite, austenite, and sigma phase, the M₂₃C₆ and MC carbides were also observed in the microstructure. The precipitation of the sigma phase was observed after just 3 minutes of aging, and after 30 minutes of aging at approximately 1053 K (780 °C), its fraction exceeded 40 pct. An intensive austenite-to-ferrite transformation was observed above 1423 K (1150 °C). Optical microscopy, energy-dispersive X-ray spectroscopy (EDS), electron backscattered diffraction (EBSD), and X-ray diffraction (XRD), as well as micro-indentation hardness, hardness, impact toughness, and tensile tests, were carried out to evaluate the obtained microstructures of aged samples.     

Overview no. 63 Non-equilibrium grain boundary segregation of boron in austenitic stainless steel-II. Fine scale segregation behaviour

A combination of TEM, FIM, AP and IAP has been used to study boron grain boundary segregation in austenitic stainless steels of the types 316L (with 40 ppm or with <1 ppm boron) and “Mo-free 316L” (23 ppm boron). High resolution segregation profiles were determined for cooling rates from 0.29 to 530°C/s for three starting temperatures: 800, 1075 and 1250°C. Boron grain boundary segregation was found after all heat treatments. The segregation behaviour was mainly of the nonequilibrium type after cooling from 1075 or 1250°C whereas equilibrium segregation dominated after rapid cooling from 800°C. The influence of the relative grain orientation on the amount of non-equilibrium segregation was small for general boundaries. However, no segregation was detected at coherent twin boundaries. The binding energy of boron to austenite grain boundaries was estimated at 0.65 ± 0.04 eV for both types of steels. The influence of the composition and boron content of the steels on the segregation behaviour is discussed and the experimental techniques used are presented.     

The Effect of Surface Preparation on the Precipitation of Sigma During High Temperature Exposure of S32205 Duplex Stainless Steel

Although the formation of sigma phase in duplex stainless steels is reasonably well documented, the effect of surface finish on its formation rate in surface regions has not been previously noted. The growth of the sigma phase precipitated in the subsurface region (to a maximum depth of 120 μm) has been quantified after heat treatment of S32205 duplex stainless steel at 1073 K (800 °C) and 1173 K (900 °C) after preparation to two surface finishes. Here, results are presented that show that there is a change in the rate of sigma phase formation in the surface region of the material, with a coarser surface finish leading to a greater depth of precipitation at a given time and temperature of heat treatment. The growth rate and morphology of the precipitated sigma has been examined and explored in conjunction with thermodynamic equilibrium phase calculations.

     

Modeling Creep Strength of Welded 9 to 12 Pct Cr Steels

The influence of weld-simulated heat treatments of 9 to 12 pct steels is evaluated by a fundamental model for creep. The heat-affected microstructure is predicted by considering particle coarsening, particle dissolution, and subgrain coarsening. Particle coarsening is predicted for a multicomponent system, showing significant M₂₃C₆ coarsening in the bcc matrix. Dissolution simulations of MX and M₂₃C₆ are performed by considering a size distribution of particles, indicating that the smallest particles can be dissolved already at relatively low welding temperatures. Recovery in dislocation networks will take place due to the coarser particles. Creep rate modeling is performed based on the heat-affected microstructure, showing strength reduction of weld-simulated material by 12 pct at 1123 K (850 °C) and 30 pct at 1173 K (900 °C). The main cause of this degradation is believed to be the loss of the smallest carbonitrides.     

High Strength and High Ductility of Ultrafine-Grained,Interstitial-Free Steel Produced by ECAE and Annealing

Interstitial-free steel (IF steel) underwent severe plastic deformation by equal-channel angular extrusion/pressing (ECAE/P) to improve its strength, and then it was annealed to achieve a good strength-ductility balance. The coarse-grained microstructure of IF steel was refined down to the submicron level after eight-pass ECAE. The ultrafine-grained (UFG) microstructure with high dislocation density brought about substantially improved strength but limited tensile ductility. The limited ductility was attributed to the small, uniform elongation caused by early plastic instability. The annealing at temperatures below 723 K (450 °C) for 1 hour did not lead to remarkable softening, whereas annealing at temperatures up to 923 K (650 °C) resulted in complete softening depending on the development of recrystallization. Therefore, the temperature of approximately 923 K (650 °C) can be considered as a critical recrystallization temperature for UFG IF steel. The annealing at 873 K (600 °C) for different time intervals resulted in different stress–strain response. Uniform tensile elongation increased at the expense of strength with annealing time intervals. After annealing at 873 K (600 °C) for 60 minutes, the yield strength, tensile strength, uniform elongation, and total elongation were found to be 320 MPa, 485 MPa, 15.1 pct, and 33.7 pct, respectively, showing the better combination of strength and ductility compared with cold-rolled samples.     

Kinetics and Grain Boundary Selectivity of Discontinuous Precipitation in Binary Ni-Cr Alloy

A supersaturated Ni-Cr alloy (42 wt pct Cr) was subjected to a series of aging heat treatments in the two-phase region in the temperature range of 923 K to 1123 K (650 °C to 850 °C) for different time periods. The resultant microstructures were seen to be composed of varying volume fractions of continuous (CP) and discontinuous precipitation (DP). The DP dominated at lower temperatures, while CP dominated at higher temperatures and the expected DP termination temperature was estimated to be 1138 K (865 °C). The kinetics of DP followed the Turnbull model at lower temperatures and the Aaronson–Liu model at higher temperatures. The nucleation and growth of DP cells, which occurred via the ‘precipitate driven grain boundary migration,’ was seen to be a strong function of the nature of the participating grain boundaries.

     

A Study of Submicron Grain Boundary Precipitates in Ultralow Carbon 316LN Steels

This article reports our efforts in characterization of an ultralow carbon 316LN-type stainless steel. The carbon content in the material is one-third that in a conventional 316LN, which further inhibits the formation of grain boundary carbides and therefore sensitizations. Our primary effort is focused on characterization of submicron size precipitates in the materials with the electron backscatter diffraction (EBSD) technique complemented by Auger electron spectroscopy (AES). Thermodynamic calculations suggested that several precipitates, such as M₂₃C₆, Chi, Sigma, and Cr₂N, can form in a low carbon 316LN. In the steels heat treated at 973 K (700 °C) for 100 hours, a combination of EBSD and AES conclusively identified the grain boundary precipitates (≥100 nm) as Cr₂N, which has a hexagonal closed-packed crystallographic structure. Increases of the nitrogen content promote formation of large size Cr₂N precipitates. Therefore, prolonged heat treatment at relatively high temperatures of ultralow carbon 316LN steels may result in a sensitization.     

Influence of Grain Boundary Character on Creep Void Formation in Alloy 617

Alloy 617, a high-temperature creep-resistant, nickel-based alloy, is being considered for the primary heat exchanger for the Next Generation Nuclear Plant (NGNP), which will operate at temperatures exceeding 760 °C and a helium pressure of approximately 7 MPa. Observations of the crept microstructure using optical microscopy indicate creep stress does not significantly influence the creep void fraction at a given creep strain over the relatively narrow set of creep conditions studied. Void formation was found to occur only after significant creep in the tertiary regime (>5 pct total creep strain) had occurred. Also, orientation imaging microscopy (OIM) was used to characterize the grain boundaries in the vicinity of creep voids that develop during high-temperature creep tests (900 °C to 1000 °C at creep stresses ranging from 20 to 40 MPa) terminated at creep strains ranging from 5 to 40 pct. Preliminary analysis of the OIM data indicates voids tend to form on grain boundaries parallel, perpendicular, or 45 deg to the tensile axis, while few voids are found at intermediate inclinations to the tensile axis. Random grain boundaries intersect most voids, while coincident site lattice (CSL)–related grain boundaries did not appear to be consistently associated with void development. Similar results were found in oxygen-free, high-conductivity (OFHC) copper, severely deformed using equal channel angular extrusion, and creep tested at 450 °C and 14 MPa.