On Phase Equilibria in Duplex Stainless Steels

The equilibrium conditions of four duplex stainless steels; Fe‐23Cr‐4.5Ni‐0.1N, Fe‐22Cr‐5.5Ni‐3Mo‐0.17N, Fe‐25Cr‐7Ni‐4Mo‐0.27N and Fe‐25Cr‐7Ni‐4Mo‐1W‐1.5Cu‐0.27N were studied in the temperature region from 700 to 1000 °C. Phase compositions were determined with SEM EDS and the phase fractions using image analysis on backscattered SEM images. The results showed that below 1000 °C the steels develop an inverse duplex structure with austenite and sigma phase, of which the former is the matrix phase. With decreasing temperature, the microstructure will be more and more complex and finely dispersed. The ferrite is, for the higher alloyed steels, only stable above 1000 °C and at lower temperatures disappears in favour of intermetallic phases. The major intermetallic phase is sigma phase with small amounts of chi phase, the latter primarily in high Mo and W grades. Nitrides, not a focus in this investigation, were present as rounded particles and acicular precipitates at lower temperatures. The results were compared to theoretical predictions using the TCFE5 and TCFE6 databases.     

Influence of annealing treatment on the formation of nano/submicron grain size AISI 301 Austenitic stainless steels

Nano/submicron austenitic stainless steels have attracted increasing attention over the past few years due to fine structural control for tailoring engineering properties. At the nano/submicron grain scales, grain boundary strengthening can be significant, while ductility remains attractive. To achieve a nano/submicron grain size, metastable austenitic stainless steels are heavily cold-worked, and annealed to convert the deformation-induced martensite formed during cold rolling into austenite. The amount of reverted austenite is a function of annealing temperature. In this work, an AISI 301 metastable austenitic stainless steel is 90 pct cold-rolled and subsequently annealed at temperatures varying from 600 °C to 900 °C for a dwelling time of 30 minutes. The effects of annealing on the microstructure, average austenite grain size, martensite-to-austenite ratio, and carbide formation are determined. Analysis of the as-cold-rolled microstructure reveals that a 90 pct cold reduction produces a combination of lath type and dislocation cell-type martensitic structure. For the annealed samples, the average austenite grain size increases from 0.28 μm at 600 °C to 5.85 μm at 900 °C. On the other hand, the amount of reverted austenite exhibits a maximum at 750 °C, where austenite grains with an average grain size of 1.7 μm compose approximately 95 pct of the microstructure. Annealing temperatures above 750 °C show an increase in the amount of martensite. Upon annealing, (Fe, Cr, Mo)₂₃C₆ carbides form within the grains and at the grain boundaries.     

Mechanical properties of new stainless steels based on the system Fe‐30Mn‐5A1‐XCr‐0.5C

New stainless steels based on the system Fe‐30Mn‐5AI‐XCr‐0.5C (Cr mass contents of ≤ 9 %) were developed and evaluated as a replacement of conventional AISI 304 steel. The alloys were produced by induction melting and thermomechanically processed to obtain a fine equiaxed microstructure. A typical thermomechanical processing for AISI 300 austenitic stainless steels was used and included forging at 1200°C, rolling at 850 °C and final recrystallization at 1050 °C. A final fully austenitic microstructure with grains of about 150 μm in size was obtained in all the steels. Tensile tests at temperatures ranging from ‐196 to 400 °C showed similar results for the various alloys tested. In accordance with the values for the elongation to fracture, this temperature range was subdivided into three regions. In the temperature range of ‐196 °C to room temperature, elongation to fracture increases with decreasing temperature. At temperatures ranging from 100 to 300 °C, elongation to fracture increases with testing temperature and serrations on the stress‐strain curve were observed. Finally, higher testing temperatures were accompanied by a decrease in ductility. Examination of the microstructures after deformation led to the conclusion that mechanical twinning was the dominant mechanism of deformation at the tested temperatures.     

Contribution to the investigation of microsegregation processes in 13% Cr 4% Ni steel during long-term annealing at 400°C

The present paper deals with the study of the development of microsegregation processes in the 13% Cr 4% Ni martensiteaustenite stainless steel during long-term annealing. The long-term annealing of 13% Cr 4% Ni steel at 400°C is accompanied by the decrease in notch impact toughness values, which is associated with an increasing tendency to the occurrence of the brittle failures. The conditions for the transition from the transcrystalline brittle failure to the intercrystalline brittle failure depend on the initial heat treatment affecting the achieved microstructure of investigated steel. The higher frequency occurrence of intercrystalline failure on the fracture surfaces of notch impact toughness specimens is accompanied by an enrichment of the prior austenite grain boundaries by phosphorus and nitrogen. At the same time the enrichment of intercrystalline fracture surfaces by nickel, or chromium was also observed. The application of an additional intercritical annealing after quenching accelerates the formation of intercrystalline failure towards shorter times during the isothermal annealing at 400°C.     

High temperature phase chemistries and solidification mode prediction in nitrogen-strengthened austenitic stainless steels

Nitronic 50 and Nitronic 50W, two nitrogen-strengthened stainless steels, were heat treated over a wide range of temperatures, and the compositions of the ferrite and austenite at each temperature were measured with analytical electron microscopy techniques. The compositional data were used to generate the (γ + δ phase field on a 58 pct Fe vertical section. Volume fractions of ferrite and austenite were calculated from phase chemistries and compared with volume fractions determined from optical micrographs. Weld solidification modes were predicted by reference to the Cr and Ni contents of each alloy, and the results were compared with predictions based on the ratios of calculated Cr and Ni equivalents for the alloys. Nitronic 50, which contained ferrite and austenite at the solidus temperature of 1370 °C, solidified through the eutectic triangle, and the weld microstructure was similar to that of austenitic-ferritic solidification. Nitronic 50W was totally ferritic at 1340 °C and solidified as primary delta ferrite. During heat treatments, Nitronic 50 and Nitronic 50W precipitated secondary phases, notably Z-phase (NbCrN), sigma phase, and stringered phases rich in Mn and Cr.     

Stress‐Temperature‐Transformation and Deformation‐Temperature‐Transformation Diagrams for an Austenitic CrMnNi as‐cast Steel

Stress‐Temperature‐Transformation (STT) and Deformation‐Temperature‐Transformation (DTT) diagrams are well‐suited to characterize the TRIP (transformation‐induced plasticity) and TWIP (twinning‐induced plasticity) effect in steels. The triggering stresses for the deformation‐induced microstructure transformation processes, the characteristic temperatures, the yield stress and the strength of the steel are plotted in the STT diagram as functions of temperature. The elongation values of the austenite, the strain‐induced twins and martensite formations are shown in the DTT diagram. The microstructure evolution of a novel austenitic Cr‐Mn‐Ni (16%Cr, 6% Mn, 6% Ni) as‐cast steel during deformation was investigated at various temperatures using static tensile tests, optical microscopy and the magnetic scale for the detection of ferromagnetic phase fraction. At the temperatures above 250 °C the steel only deforms by glide deformation of the austenite. Strain‐induced twinning replaces the glide deformation at temperatures below 250 °C with increasing strain. Below 100 °C, the strain‐induced martensite formation becomes more pronounced. The kinetics of the α'‐martensite formation is described according to stress and deformation temperatures. The STT and DTT diagrams, enhanced with the kinetics of the martensite formation, are presented in this paper.     

Austenitic Nickel- and Manganese-Free Fe-15Cr-1Mo-0.4N-0.3C Steel: Tensile Behavior and Deformation-Induced Processes between 298 K and 503 K (25 °C and 230 °C)

The high-temperature austenite phase of a high-interstitial Mn- and Ni-free stainless steel was stabilized at room temperature by the full dissolution of precipitates after solution annealing at 1523 K (1250 °C). The austenitic steel was subsequently tensile-tested in the temperature range of 298 K to 503 K (25 °C to 230 °C). Tensile elongation progressively enhanced at higher tensile test temperatures and reached 79 pct at 503 K (230 °C). The enhancement at higher temperatures of tensile ductility was attributed to the increased mechanical stability of austenite and the delayed formation of deformation-induced martensite. Microstructural examinations after tensile deformation at 433 K (160 °C) and 503 K (230 °C) revealed the presence of a high density of planar glide features, most noticeably deformation twins. Furthermore, the deformation twin to deformation-induced martensite transformation was observed at these temperatures. The results confirm that the high tensile ductility of conventional Fe-Cr-Ni and Fe-Cr-Ni-Mn austenitic stainless steels may be similarly reproduced in Ni- and Mn-free high-interstitial stainless steels solution annealed at sufficiently high temperatures. The tensile ductility of the alloy was found to deteriorate with decarburization and denitriding processes during heat treatment which contributed to the formation of martensite in an outermost rim of tensile specimens.     

Hot Ductility of DSS and Its Microstructure Observation During Hot Deformation

By selecting several typical duplex stainless steels (DSS), i. e., 00Cr22Ni5Mo3N, 00Cr21Ni2Mn5N and 00Cr25Ni7Mo4N, as research materials, hot ductility characteristic of DSS was studied by thermal simulation method and microstructure evolution during hot compression was observed through TEM. The results show that the optimum hot ductility temperature range of DSS is 1050–1200°C. 00Cr25Ni7Mo4N exhibits the worst hot ductility and 00Cr21Ni2Mn5N has similar hot ductility to 00Cr22Ni5Mo3N. During hot compression, the dynamic recovery of austenite occurs in DSS while the dynamic recovery and reerystallization of ferrite take place in 00Cr22NioMo3N and 00Cr21Ni2Mn5N, but only the dynamic recovery of ferrite can be observed in 00Cr25Ni7Mo4N.     

Formation of Austenite During Intercritical Annealing of Dual-Phase Steels

The formation of austenite during intercritical annealing at temperatures between 740 and 900 °C was studied in a series of 1.5 pct manganese steels containing 0.06 to 0.20 pct carbon and with a ferrite-pearlite starting microstructure, typical of most dual-phase steels. Austenite formation was separated into three stages: (1) very rapid growth of austenite into pearlite until pearlite dissolution is complete; (2) slower growth of austenite into ferrite at a rate that is controlled by carbon diffusion in austenite at high temperatures (~85O °C), and by manganese diffusion in ferrite (or along grain boundaries) at low temperatures (~750 °C); and (3) very slow final equilibration of ferrite and austenite at a rate that is controlled by manganese diffusion in austenite. Diffusion models for the various steps were analyzed and compared with experimental results.     

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.     

铌对00Cr12Ni不锈钢组织和性能的影响

 分别冶炼了3种不同铌含量的00Cr12Ni不锈钢,用光学显微镜和透射电镜观察了热轧退火态的显微组织,测量了试验钢的拉伸性能和不同温度的冲击功。试验结果表明：铌的添加显著抑制了退火时铁素体再结晶的发生。未添加稳定化元素铌的钢中析出相为Cr23C6,w(Nb)为0.28%的试验钢中析出相为Nb(C,N)和Fe3Nb3C,w(Nb)为0.49%的试验钢中析出相为Nb(C,N)和Fe2Nb,而且其析出相总体积分数明显高于其他2种试验钢。铌的添加提高了试验钢的强度,降低了试验钢的塑性和韧性,w(Nb)为0.49%的试验钢冲击功最低,但其韧脆转变温度也最低。     

Evolution of Microstructure and Texture During Warm Rolling of a Duplex Steel

The effect of warm rolling on the evolution of microstructure and texture in a duplex stainless steel (DSS) was investigated. For this purpose, a DSS steel was warm rolled up to 90 pct reduction in thickness at 498 K, 698 K, and 898 K (225 °C, 425 °C, and 625 °C). The microstructure with an alternate arrangement of deformed ferrite and austenite bands was observed after warm rolling; however, the microstructure after 90 pct warm rolling at 498 K and 898 K (225 °C and 625 °C) was more lamellar and uniform as compared to the rather fragmented and inhomogeneous structure observed after 90 pct warm rolling at 698 K (425 °C). The texture of ferrite in warm-rolled DSS was characterized by the presence of the RD (〈011〉//RD) and ND (〈111〉//ND) fibers. However, the texture of ferrite in DSS warm rolled at 698 K (425 °C) was distinctly different having much higher fraction of the RD-fiber components than that of the ND-fiber components. The texture and microstructural differences in ferrite in DSS warm rolled at different temperatures could be explained by the interaction of carbon atoms with dislocations. In contrast, the austenite in DSS warm rolled at different temperatures consistently showed pure metal- or copper-type deformation texture which was attributed to the increase in stacking fault energy at the warm-rolling temperatures. It was concluded that the evolution of microstructure and texture of the two constituent phases in DSS was greatly affected by the temperature of warm rolling, but not significantly by the presence of the other phase.     

Spontaneous and Deformation‐Induced Martensite in Austenitic Stainless Steels with Different Stability

The fraction and microstructure of spontaneous and deformation‐induced martensite in three austenitic stainless steels with different austenite stability have been investigated. Samples were quenched in brine followed by cooling in liquid nitrogen or plastically deformed by uniaxial tensile testing at different initial temperatures. In‐situ ferritescope measurements of the martensite fraction was conducted during tensile testing and complemented with ex‐situ X‐ray diffractometry. The microstructures of quenched and deformed samples were examined using light optical microscopy and electron backscattered diffraction. It was found that annealing twins in austenite are effective nucleation sites for spontaneous α'‐martensite, while deformation‐induced α'‐martensite mainly formed within parallel shear‐bands. The α'‐martensite formed has an orientation relationship near the Kurdjumov‐Sachs (K‐S) relation with the parent austenite phase even at high plastic strains, and adjacent α'‐martensite variants were mainly twin related (<111> 60° or Σ3).     

Microstructure evolution during isothermal annealing of a standard duplex stainless steel type 1.4462

Small alterations in chemical composition, even within the boundaries of the international standards, can drastically alter the formation kinetics of intermetallic phases in a stainless steel. Therefore, by means of isothermal annealing experiments, the time‐temperature‐precipitation (TTP) diagram was constructed for an industrially cold rolled and annealed standard duplex stainless steel of type 1.4462 (X2CrNiMoN22‐5‐3), having a distinct composition. Temperature was varied from 600 to 1050 °C, with annealing times from 10 to 3·10⁵ s Two intermetallic phases were observed with scanning electron microscopy (SEM): σ phase and χ phase. σ precipitation occurred in a slightly higher temperature range than χ precipitation. In addition, at high temperatures σ was the first phase to appear, while at lower temperatures χ was the first. This could be explained by the driving force for transformation, which is larger for σ at high temperatures and larger for χ at low temperatures. The microstructural changes during the heat treatment were studied in detail in order to provide a complete overview of all the phenomena that occur during annealing. At temperatures between 750 and 900 °C precipitation was fastest and all the α was replaced by γ and σ after prolonged times. The presence of neighbouring ferrite seems to be a necessary condition for the χ phase to be stable. The appearance of large volume fractions of σ above 700 °C was accompanied by a strong growth of the austenitic phase resulting in a more isotropic microstructure. Beneath 700 °C, the precipitated volume fractions of σ were relatively small and consequently the original banded structure remained clearly visible. At these lower temperatures the mobility of alloying elements is limited and a Widmannstätten like austenite was observed to grow into the ferrite in a needle‐like manner.     

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.     

Nanoscale Analyses of High-Nickel Concentration Martensitic High-Strength Steels

Austenite reversion in martensitic steels is known to improve fracture toughness. This research focuses on characterizing mechanical properties and the microstructure of low-carbon, high-nickel steels containing 4.5 and 10 wt pct Ni after a QLT-type austenite reversion heat treatment: first, martensite is formed by quenching (Q) from a temperature in the single-phase austenite field, then austenite is precipitated by annealing in the upper part of the intercritical region in a lamellarization step (L), followed by a tempering (T) step at lower temperatures. For the 10 wt pct Ni steel, the tensile strength after the QLT heat treatment is 910 MPa (132 ksi) at 293 K (20 °C), and the Charpy V-notch impact toughness is 144 J (106 ft-lb) at 188.8 K (?84.4 °C, ?120 °F). For the 4.5 wt pct Ni steel, the tensile strength is 731 MPa (106 ksi) at 293 K (20 °C) and the impact toughness is 209 J (154 ft-lb) at 188.8 K (?84.4 °C, ?120 °F). Light optical microscopy, scanning electron and transmission electron microscopies, synchrotron X-ray diffraction, and local-electrode atom-probe tomography (APT) are utilized to determine the morphologies, volume fractions, and local chemical compositions of the precipitated phases with sub-nanometer spatial resolution. The austenite lamellae are up to 200 nm in thickness, and up to several micrometers in length. In addition to the expected partitioning of Ni to austenite, APT reveals a substantial segregation of Ni at the austenite/martensite interface with concentration maxima of 10 and 23 wt pct Ni for the austenite lamellae in the 4.5 and 10 wt pct Ni steels, respectively. Copper-rich and M₂C-type metal carbide precipitates were detected both at the austenite/martensite interface and within the bulk of the austenite lamellae. Thermodynamic phase stability, equilibrium compositions, and volume fractions are discussed in the context of Thermo-Calc calculations.     

Microstructure-strength relations in a hardenable stainless steel with 16 pct Cr, 1.5 pct Mo,and 5 pct Ni

Metallographic studies have been conducted on a 0.024 pct C-16 pct Cr-1.5 pct Mo-5 pct Ni stainless steel to study the phase reactions associated with heat treatments and investigate the strengthening mechanisms of the steel. In the normalized condition, air cooled from 1010 °C, the microstructure consists of 20 pct ferrite and 80 pct martensite. Tempering in a temperature range between 500 and 600 °C results in a gradual transformation of martensite to a fine mixture of ferrite and austenite. At higher tempering temperatures, between 600 and 800 °C, progressively larger quantities of austenite form and are converted during cooling to proportionally increasing amounts of fresh martensite. The amount of retained austenite in the microstructure is reduced to zero at 800 °C, and the microstructure contains 65 pct re-formed martensite and 35 pct total ferrite. Chromium rich M₂₃C₆ carbides precipitate in the single tempered microstructures. The principal strengthening is produced by the presence of martensite in the microstructure. Additional strengthening is provided by a second tempering treatment at 400 °C due to the precipitation of ultrafine (Cr, Mo) (C,N) particles in the ferrite.     

Temperature Dependent Deformation Mechanisms of a High Nitrogen‐Manganese Austenitic Stainless Steel

The influence of temperature on the deformation behaviour of a Fe‐16.5Cr‐8Mn‐3Ni‐2Si‐1Cu‐0.25N (wt%) austenitic stainless steel alloy was investigated using transmission electron microscopy and X‐ray diffraction measurements. Recrystallized samples were deformed under tension at ?75°C, 20°C, and 200°C and the microstructures were characterized after 5% strain and after testing to failure. Deformation to failure at ?75°C resulted in extensive transformation induced plasticity (TRIP) with over 90% α′‐martensite. The sample deformed to 5% strain at ?75°C shows that the austenite transformed first to ?‐martensite which served to nucleate the α′‐martensite. Transformation induced martensite prohibits localized necking providing total elongation to failure of over 70%. At room temperature, in addition to some TRIP behaviour, the majority of the deformation is accommodated by dislocation slip in the austenite. Some deformation induced twinning (TWIP) was also observed, although mechanical twinning provides only a small contribution to the total deformation at room temperature. Finally, dislocation slip is the dominant deformation mechanism at 200°C with a corresponding decrease in total elongation to failure. These changes in deformation behaviour are related to the temperature dependence on the relative stability of austenite and martensite as well as the changes in stacking fault energy (SFE) as a function of temperature.     

Effect of Annealing Temperature on Microstructure and Mechanical Properties of Bulk 316L Stainless Steel with Nano- and Micro-crystalline Dual Phases

Microstructures and mechanical properties of 316L stainless steels with dual phases austenite prepared by an aluminothermic reaction casting were explored. It is found that the steels consist of nano- and micro-crystalline austenite phases, a little δ ferrite and contaminations. Before and after annealing at 1073 K and 1273 K (800 °C and 1000 °C), average grain sizes of the nanocrystalline austenite phase are about 32, 31, 38 nm, respectively. Tensile strength increases first from 371 to 640 MPa and then decreases to 454 MPa. However, elongation ratio increases gradually from 16 to 23 and then 31 pct after annealing. The results illustrate that the steel after annealing at 1073 K (800 °C) has better properties, also indicating that combination of dual nano- and micro-crystalline austenite phase is conductive to improving tensile properties of materials.