An Investigation of the Massive Transformation from Ferrite to Austenite in Laser-Welded Mo-Bearing Stainless Steels

A series of 31 Mo-bearing stainless steel compositions with Mo contents ranging from 0 to 10 wt pct and exhibiting primary δ-ferrite solidification were analyzed over a range of laser welding conditions to evaluate the effect of composition and cooling rate on the solid-state transformation to γ-austenite. Alloys exhibiting this microstructural development sequence are of particular interest to the welding community because of their reduced susceptibility to solidification cracking and the potential reduction of microsegregation (which can affect corrosion resistance), all while harnessing the high toughness of γ-austenite. Alloys were created using the arc button melting process, and laser welds were prepared on each alloy at constant power and travel speeds ranging from 4.2 to 42 mm/s. The cooling rates of these processes were estimated to range from 10 K (°C)/s for arc buttons to 10⁵ K (°C)/s for the fastest laser welds. No shift in solidification mode from primary δ-ferrite to primary γ-austenite was observed in the range of compositions or welding conditions studied. Metastable microstructural features were observed in many laser weld fusion zones, as well as a massive transformation from δ-ferrite to γ-austenite. Evidence of epitaxial massive growth without nucleation was also found when intercellular γ-austenite was already present from a solidification reaction. The resulting single-phase γ-austenite in both cases exhibited a homogenous distribution of Mo, Cr, Ni, and Fe at nominal levels.     

Kinetics of peritectic reaction and transformation in Fe-C alloys

In situ dynamic observation of the progress of a peritectic reaction and transformation of Fe-(0.14 pct C)- and Fe-(0.42 pct C)-peritectic Fe-C alloys has been successfully made with a combination of a confocal scanning laser microscope and an infrared image furnace. The peritectic reaction is characterized by the formation of the γ-austenite phase at the junction of the liquid and the grain boundary of δ-ferrite crystals and subsequent propagation of the three-phase point, liquid/γ/δ, along the liquid/δ boundary, whereas the peritectic transformation occurs by the thickening of the intervening γ toward both the liquid side and the δ side. The rates of the peritectic reaction for the two peritectic alloys are found to be much faster than the rate that would be controlled by carbon diffusion, suggesting that either massive transformation to γ or solidification as γ controls the rate. This is also the case for the Fe-0.14%C transformation in the hypoperitectic alloy. However, the rate of the peritectic transformation in the Fe-0.42%C alloy is determined by carbon diffusion. This article is based on a presentation made in the “Geoffrey Belton Memorial Symposium,” held in January 2000, in Sydney, Australia, under the joint sponsorship of ISS and TMS.     

Modeling of the peritectic reaction and macro-segregation in casting of low carbon steel

Macro-microscopic models have been developed to describe the macrosegregation behavior associated with the peritectic reaction of low carbon steel. The macrosegregation model has been established on the basis of previously published work and experimental data. A microscopic model of a three-phase reaction L+δ→γ has been modeled by using Fredriksson’s approach. Four horizontal and unidirectional solidified experimental groups simulating continuous casting have been performed with a low carbon steel containing 0.13 wt pct carbon. The extent of macrosegregation of carbon was determined by wet chemical analysis of millings. It is confirmed, by comparing calculated results with experimental results, that this model successfully predicts the occurrence of macrosegregation. The results indicate that a peritectic reaction which is associated with a high cooling rate generates high thermal contraction and a high tensile strain rate at the peritectic temperature. Therefore, the macrosegregation, particularly at the ingot surface, is very sensitive to the cooling rate, where extremely high positive segregation was observed in the case of a high cooling rate. However, in the case of slow cooling rate, negative segregation was noted. The mechanism of macrosegregation with peritectic reaction is discussed in detail.     

Phase Transformations and Microstructural Evolution of Mo-Bearing Stainless Steels

The good corrosion resistance of superaustenitic stainless steel (SASS) alloys has been shown to be a direct consequence of high concentrations of Mo, which can have a significant effect on the microstructural development of welds in these alloys. In this research, the microstructural development of welds in the Fe-Ni-Cr-Mo system was analyzed over a wide variety of Cr/Ni ratios and Mo contents. The system was first simulated by construction of multicomponent phase diagrams using the CALPHAD technique. Data from vertical sections of these diagrams are presented over a wide compositional range to produce diagrams that can be used as a guide to understand the influence of composition on microstructural development. A large number of experimental alloys were then prepared via arc-button melting for comparison with the diagrams. Each alloy was characterized using various microscopy techniques. The expected δ-ferrite and γ-austenite phases were accompanied by martensite at low Cr/Ni ratios and by σ phase at high Mo contents. A total of 20 possible phase transformation sequences are proposed, resulting in various amounts and morphologies of the γ, δ, σ, and martensite phases. The results were used to construct a map of expected phase transformation sequence and resultant microstructure as a function of composition. The results of this work provide a working guideline for future base metal and filler metal development of this class of materials. An erratum to this article can be found at     

The influence of the ferrite to austenite transformation on the formation of sulfidesx

Steel solidifies either by a primary precipitation of δ-Fe or by a primary precipitation of γ-Fe. In the former case the steel can either go through a peritectic reaction or a solid state transformation to form y-Fe during cooling. The influence of the rate of solidification and/or the transformation sequence on the sulfide precipitation in steels was studied in unidirectionally solidified Fe-Ni-S and Fe-Ni-Mn-S alloys. Nickel was used to govern the solidification sequence. It was shown that the solid state transformation could give rise to iron sulfide films according to a metatectic reaction. It was also shown that the peritectic reaction favored the formation of iron sulfide films. These films solidified at a very low temperature. During cooling the films contracted and small sulfide particles were formed. If the alloy contained manganese the composition of the films was changed during cooling from nearly pure iron sulfide to nearly pure manganese sulfide due to diffusion of manganese from the matrix.     

Spatially resolved X-ray diffraction mapping of phase transformations in the heat-affected zone of carbon-manganese steel arc welds

Phase transformations that occur in the heat-affected zone (HAZ) of gas tungsten arc welds in AISI 1005 carbon-manganese steel were investigated using spatially resolved X-ray diffraction (SRXRD) at the Stanford Synchrotron Radiation Laboratory. In situ SRXRD experiments were performed to probe the phases present in the HAZ during welding of cylindrical steel bars. These real-time observations of the phases present in the HAZ were used to construct a phase transformation map that identifies five principal phase regions between the liquid weld pool and the unaffected base metal: (1) α-ferrite that is undergoing annealing, recrystallization, and/or grain growth at subcritical temperatures, (2) partially transformed α-ferrite co-existing with γ-austenite at intercritical temperatures, (3) single-phase γ-austenite at austenitizing temperatures, (4) δ-ferrite at temperatures near the liquidus temperature, and (5) back transformed α-ferrite co-existing with residual austenite at subcritical temperatures behind the weld. The SRXRD experimental results were combined with a heat flow model of the weld to investigate transformation kinetics under both positive and negative temperature gradients in the HAZ. Results show that the transformation from ferrite to austenite on heating requires 3 seconds and 158°C of superheat to attain completion under a heating rate of 102°C/s. The reverse transformation from austenite to ferrite on cooling was shown to require 3.3 seconds at a cooling rate of 45 °C/s to transform the majority of the austenite back to ferrite; however, some residual austenite was observed in the microstructure as far as 17 mm behind the weld.     

Optimization of the johnson-mehl-avarami equation parameters for <Emphasis Type="Italic">α</Emphasis>-ferrite to <Emphasis Type="Italic">γ</Emphasis>-austenite transformation in steel welds using a genetic algorithm

A nonisothermal Johnson-Mehl-Avarami (JMA) equation with optimized JMA parameters is proposed to represent the kinetics of transformation of α-ferrite to γ-austenite during heating of 1005 steel. The procedure used to estimate the JMA parameters involved a combination of numerical heat-transfer and fluid-flow calculations, the JMA equation for nucleation and growth for nonisothermal systems, and a genetic algorithm (GA) based optimization tool that used a limited volume of experimental kinetic data. The experimental data used in the calculations consisted of phase fraction of γ-austenite measured at several different monitoring locations in the heat-affected zone (HAZ) of a gas tungsten arc (GTA) weld in 1005 steel. These data were obtained by an in-situ spatially resolved X-ray diffraction (SRXRD) technique using synchrotron radiation during welding. The thermal cycles necessary for the calculations were determined for each monitoring location from a well-tested three-dimensional heat-transfer and fluid-flow model. A parent centric recombination (PCX) based generalized generation gap (G3) GA was used to obtain the optimized values of the JMA parameters, i.e., the activation energy, pre-exponential factor, and exponent in the nonisothermal JMA equation. The GA based determination of all three JMA equation parameters resulted in better agreement between the calculated and the experimentally determined austenite phase fractions than was previously achieved.     

Study of microstructure of low-temperature plasma-nitrided AISI 304 stainless steel

The microstructure of the low-temperature plasma-nitrided layer on AISI 304 austenitic stainless steel was studied by transmission electron microscopy (TEM). The results show that the surface of the layer consists of a supersaturated solid solution (γ′_N) based on the γ′-Fe₄N phase whose electron diffraction pattern (EDP) has a strong diffuse scattering effect resulting from supersaturating nitrogen (above 20 at. pct) and 〈110〉 streaks arising from matrix elastic strain due to the formation of paired or clustered Cr-N. The latter is due to the N above the 20 at. pct γ′-Fe₄N-phase value and leads to a lattice parameter that is greater than that of the γ′-Fe₄N phase. The subsurface of the layer is composed of a supersaturated solid solution based on γ-austenite, which is an expanded austenite, γ _N. Its morphology shows the basketweave or “tweedlike” contrast consisting of so-called stacking fault precipitates having twin relationships with the matrix whose EDP shows diffuse scattering streaks with certain directions. The ε martensite transformation was observed in the subsurface of the layer. The increase in stacking faults compared with the original stainless steel and formation of ε martensite in the subsurface of the layer indicate that nitrogen lowers the stacking fault energy of austenite.     

Kinetics of the peritectic phase transformation: In-situ measurements and phase field modeling

An experimental study has been conducted into the role of cooling rate on the kinetics of the peritectic phase transformation in a Fe−C alloy. The interfacial growth velocities of the peritectic phase transformation were measured in situ for cooling rates of 100, 50, and 10 K/min. In-situ observations were obtained using high-temperature laser scanning confocal microscopy (HTLSCM) in a concentric solidification configuration. The experimentally measured interface velocities of the liquid/austenite (L/γ) and austenite/delta-ferrite (γ/δ) interphase boundaries were observed to increase with higher cooling rates. A unique finding of this study was that as the cooling rate increased there was a transition point where the L/γ interface propagated at a higher velocity than the γ/δ interface, contrary to the findings of previous researchers. Phase field modeling was conducted using a commercial multicomponent, multiphase package. Good correlation was obtained between model predictions and experimental observations in absolute values of interface velocities and the effect of cooling rate. Analysis of the simulated microsegregation in front of the L/γ and γ/δ interfaces as a function of cooling rate revealed the importance of solute pileup. This microsegregation plays a pivotal role in the propagation of interfaces; thus, earlier modeling work in which complete diffusion in the liquid phase was assumed cannot fully describe the rate of propagation of the L/γ and δ/γ interfaces during the course of the peritectic transformation.     

Kinetics of the peritectic phase transformation: In-situ measurements and phase field modeling

An experimental study has been conducted into the role of cooling rate on the kinetics of the peritectic phase transformation in a Fe-C alloy. The interfacial growth velocities of the peritectic phase transformation were measured in situ for cooling rates of 100, 50, and 10 K/min. In-situ observations were obtained using high-temperature laser scanning confocal microscopy (HTLSCM) in a concentric solidification configuration. The experimentally measured interface velocities of the liquid/austenite (L/γ) and austenite/delta-ferrite (γ/δ) interphase boundaries were observed to increase with higher cooling rates. A unique finding of this study was that as the cooling rate increased, there was a transition point where the L/γ interface propagated at a higher velocity than the γ/δ interface, contrary to the findings of previous researchers. Phase field modeling was conducted using a commercial multicomponent, multiphase package. Good correlation was obtained between model predictions and experimental observations in absolute values of interface velocities and the effect of cooling rate. Analysis of the simulated microsegregation in front of the L/γ and γ/δ interfaces as a function of cooling rate revealed the importance of solute pileup. This microsegregation plays a pivotal role in the propagation of interfaces; thus, earlier modeling work in which complete diffusion in the liquid phase was assumed cannot fully describe the rate of propagation of the L/γ and δ/γ interfaces during the course of the peritectic transformation.     

Kinetics of the peritectic phase transformation: In-situ measurements and phase field modeling

An experimental study has been conducted into the role of cooling rate on the kinetics of the peritectic phase transformation in a Fe−C alloy. The interfacial growth velocities of the peritectic phase transformation were measuredin situ for cooling rates of 100, 50, and 10 K/min.In-situ observations were obtained using high-temperature laser scanning confocal microscopy (HTLSCM) in a concentric solidification configuration. The experimentally measured interface velocities of the liquid/austenite (L/γ) and austenite/delta-ferrite (γ/δ) interphase boundaries were observed to increase with higher cooling rates. A unique finding of this study was that as the cooling rate increased there was a transition point where the L/γ interface propagated at a higher velocity than the γ/δ interface, contrary to the findings of previous researchers. Phase field modeling was conducted using a commercial multicomponent, multiphase package. Good correlation was obtained between model predictions and experimental observations in absolute values of interface velocities and the effect of cooling rate. Analysis of the simulated microsegregation in front of the L/γ and γ/δ interfaces as a function of cooling rate revealed the importance of solute pileup. This microsegregation plays a pivotal role in the propagation of interfaces; thus, earlier modeling work in which complete diffusion in the liquid phase was assumed cannot fully describe the rate of propagation of the L/γ and δ/γ interfaces during the course of the peritectic transformation.     

Effects of composition and microstructure on fatigue of γ/γ′-δ type eutectic alloys

Room temperature tension-tension fatigue tests were performed on two lamellar γ/γ′-δ alloys, one with 0 pct Cr and one with 6 pct Cr. The 6 pct Cr alloy was solidified at 3 cmJh while the 0 pct Cr alloy was solidified at 3 cm/h and 5.7 cm/h. Fatigue testing was done on both alloys in the as-directionally solidified condition and on the 0 pct Cr alloy after heat treatment. Increasing the growth speed of the 0 pct Cr alloy increased the fatigue life of the material at stresses above the 10⁷ cycle fatigue limit. Partial solution treating and aging of the 0 pct Cr alloy,R = 3 cm/h, increased the fatigue life relative to the as-directionally solidified material at high stresses, to the same extent as increasing the growth speed. Full solution treatment and aging of the 0 pct Cr alloy,R = 5.7 cm/ h, caused a reduction in the fatigue life relative to the as-directionally solidified material. Fatigue cracking tended to be faceted in the 6 pct Cr alloy as opposed to the more ductile failure of the 0 pct Cr alloy. Microstructural perfection, grain size and shape, interlamellar spacing, longitudinal cracking, and longitudinal and transverse ductility all are believed to have influenced the fatigue resistance of the alloys.     

Solidification of an alloy 625 weld overlay

The solidification behavior (microsegregation, secondary phase formation, and solidification temperature range) of an Alloy 625 weld overlay deposited on 2.25Cr - 1Mo steel by gas metal arc welding was investigated by light and electron optical microscopy, electron microprobe, and differential thermal analysis techniques. The overlay deposit was found to terminate solidification at ≈ 1216 °C by aγ/Laves eutectic-type reaction. The Laves phase was highly enriched in Nb, Mo, and Si. The solidification reaction and microsegregation potential of major alloying elements in the overlay deposit are compared to other Nb-bearing Ni base alloys and found to be very similar to those for Alloy 718. Solidification cracks observed in the overlay were attributed to the wide solidification temperature range (≈170 °C) and formation of interdendritic (γ+Laves) constituent. Reasonable agreement is obtained between the calculated and measured volume percent (γ+Laves) constituent with the Scheil equation by treating the overlay system as a simpleγ-Nb “binary” and using an experimentally determinedk ^Nb value from electron microprobe data.     

Kinetics of austenite-ferrite and austenite-pearlite transformations in a 1025 carbon steel

Isothermal and continuous-cooling transformation kinetics have been measured dilatometrically for the γ → α+ γ′ and γ′→ P reactions in a 1025 steel. The isothermal transformation of austenite for each reaction was found to fit the Avrami equation after the fraction transformed was normalized to unity at the completion of the reaction and a transformation-start time was determined. The transformation kinetics under isothermal conditions therefore were characterized in terms of then andb parameters from the Avrami equation together with the transformation-start times. The parametern was found to be independent of temperature over the range studied (645 to 760 ‡C) and to have values of 0.99 and 1.33 for the ferrite and pearlite reactions, respectively. This indicates that the nucleation condition is essentially constant and site saturation occurs early in the transformation process. The continuous-cooling experiments were conducted at cooling rates of 2 to 150 ‡C per second to determine the transformation-start times for the ferrite and pearlite reactions and the completion time for transformation to pearlite under CCT conditions. Both reactions were found to obey the Additivity Principle for continuous cooling provided that the incubation (pre-transformation) period was not included in the transformation time. The isothermal transformation data and CCT transformation-start times have been incorporated in a mathematical model to predict continuous-cooling transformation kinetics that agree closely with measurements made at three cooling rates.     

Auger electron spectroscopy study of grain boundary segregation in alloy K-500: Part I. Behavior in as-processed state

Increased interest has been paid to grain boundary segregation in alloy K-500 due to severe intergranular cracking recently observed in forged bars. However, little systematic study of this segregation has been performed so far. A detailed auger electron spectroscopy (AES) study of grain boundary segregation in alloy K-500 has been carried out as a function of alloy chemistry. To determine C segregation, the C and O contamination rates in a vacuum chamber were measured and the necessary condition for C grain boundary segregation determination was established. It has been found that severe C, Al, and Cu segregation to grain boundaries occurred and depended on alloy chemistry. High bulk Ni and low bulk Al promoted C and Al grain boundary segregation, and low bulk Ni and high bulk Al significantly enhanced Cu segregation to grain boundaries. The depth profiles of intergranularly segregated elements also showed different features for high and low Ni content alloys. In high Ni alloys, C and Al levels dropped continuously as a function of distance from the grain boundaries but the Cu level dropped only slightly. In low Ni alloys, the Al and C levels rose from relatively low grain boundary levels to a peak at a certain distance from the grain boundary where the high grain boundary Cu level dramatically dropped. Transmission electron microscope (TEM) observation revealed a grain boundaryγ′-depleted zone followed by a region with coarser and denserγ′ particles in low Ni and high Al alloys but quite uniformly distributedγ′ particles with no depleted zone in high Ni and low Al alloys. These can be explained by the observed segregation behavior. The occurrence of Cu segregation is explained according to available theories about surface segregation in binary Ni-Cu alloys, and the segregation of C and Al to grain boundaries is suggested to be probably due to their interaction with Ni and Cu.     

Phase relationships in the Fe-Cr-Ni system at solidification temperatures

The phase relationships between the liquid phase and the primary solid phases were investigated in the iron-rich corner of the Fe-Cr-Ni system as part of a larger study of the Fe-Cr-Ni-C system. The investigation consisted of measurements and modeling of tie-lines and the liquidus surfaces of the liquid-delta (bcc) and liquid-gamma (fcc) equilibria and the peritectic surface involving all three phases in the iron-rich corner of the Gibbs triangle bounded by 0 to 25 wt pct Cr and 0 to 25 wt pct Ni (bal Fe). The temperature ranged from the melting point of iron (1811 K) to about 1750 K. Compositions for tie-lines were obtained from liquid-solid equilibrium couples and temperatures for the surfaces were obtained by differential thermal analysis. Parameters for modeling the system were then selected in the subregular solution model to minimize the square of the difference between experimental and calculated tie-lines. With one ternary parameter employed for each phase, calculations by the model are in excellent agreement with the tie-line and liquidus measurements and in fair agreement with the temperatures for the peritectic surfaceL + δ/L + δ + γ. The usefulness of the model is demonstrated by calculation of the solidification paths of selected alloys in the composition field investigated for the limiting cases of (a) complete equilibrium followed by the alloy system, and (b) no solid diffusion (i.e., segregation) with equilibrium maintained at the solidifying front and complete mixing in the liquid phase.     

Microscopic modeling of fundamental phase transformations in continuous castings of steel

A model has been developed to describe the microscopic behavior of phase transformation of carbon steels in the range of cooling rate occurring in continuous casting. In the liquid-to solidphase transformation, this model simulates the phenomena of dendrite nucleation and growth during solidification. Both δ- and γ-dendrites are involved. The nucleation and growth model has been established on the basis of published experimental data and previous work. Also, a model of the peritectic transformation of carbon steels has been included. In the solid-to solidphase transformation, the model considers the δ→ γ, γ→ α, and γ→ α + Fe₃C phase transformations. The δ→ γ and γ→ α phase transformations have been modeled by using the Johnson-Mehl equation, also known as the Avrami equation. For the pearlite transformation, a nucleation law, as well as the growth kinetics, has been established. Good agreement has been found between the prediction of the model and the experimental data.     

Solidification of M2 high speed steel

The freezing process in AISI type M2 high speed tool steel (6 pct W, 5 pct Mo, 4 pct Cr, 2 pct V, 0.8 pct C) was studied by metallographic and thermal analysis techniques. Unidirectional solidification of small laboratory melts in a modified crystal growing apparatus was employed to provide metallographic sections of known macroscopic growth direction. Also cooling curves were obtained on 40 g specimens solidified in thimble crucibles. X-ray microradiography, electron probe scanning techniques, and quantitative microanalysis of dendrites and interdendritic carbides were extensively used to supplement conventional metallography. Carbon and vanadium contents of M2 were varied in order to observe the effect of an austenite and ferrite stabilizer on the thermal analysis curves and microstructure. The nonequilibrium freezing process in M2 includes three major liquid-solid reactions: 1) Liquid → Ferrite, 1435°C; 2) Liquid + Ferrite → Austenite, 1330°C; 3) Liquid → Austenite + M₆C + MC, 1240°C. These reactions account for the as-cast structure of the commercial alloy. The addition of carbon depresses the liquidus (1) and solidus temperatures (3) and narrows the gap between the liquidus (1) and peritectic transformation (2). This gap is eliminated at > 1.39 wt pct C, where the initial freezing reaction is the crystallization of austenite. The accompanying microstructural change is the elimination of σ eutectoid dendrite cores. The addition of vanadium promotes ferrite formation by strongly depressing the peritectic reaction and thus widening the gap between the liquidus and the peritectic.