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.     

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.     

Effect of Destabilizing Heat Treatment on Solid-State Phase Transformation in High-Chromium Cast Irons

This work describes the influence of secondary carbide precipitation at destabilizing heat treatment on kinetics of austenite phase transformation at a subcritical range of temperatures in high-Cr cast irons, alloyed with 4 to 6 wt pct of Mn or by complex Mn-Ni-Mo (Mn-Cu-Mo). The samples were soaked at 1073 K to 1373 K (800  °C to 1100  °C) (destabilization) or at 573 K to 973 K (300  °C to 700  °C) (subcritical treatment); the combination of destabilization and subcritical treatment was also used. The investigation was carried out with application of optical and electron microscopy and bulk hardness measurement. Time-temperature-transformation (TTT) curves of secondary carbide precipitation and pearlite transformation for as-cast austenite and destabilized austenite were built in this work. It was determined that the secondary carbide precipitation significantly inhibited the pearlite transformation rate at 823 K to 973 K (550  °C to 700  °C). The inhibition effect is more evident in cast irons alloyed with complex Mn-Ni-Mo or Mn-Cu-Mo. The possible reasons for transformation decelerating could be austenite chemical composition change (enriching by Ni, Si, and Cu, and depleting by Cr) and stresses induced by secondary carbide precipitation.     

Replacement of Ni by Mn in High-Ni-Containing Austenitic Cast Steels used for Turbo-Charger Application

High-temperature tensile properties of austenitic cast steels fabricated by replacing Ni by Mn in a 20 wt pct Ni-containing steel were investigated. In a steel where 8 wt pct Ni was replaced by 9.2 wt pct of Mn, 17.4 and 9.8 pct of ferrite existed in equilibrium phase diagrams and actual microstructures, respectively, because a role of Mn as an austenite stabilizer decreased, and led to deterioration of high-temperature properties. When 2 to 6 wt pct Ni was replaced by 2.3 to 6.9 wt pct Mn, high-temperature properties were comparable to those of the 20 wt pct Ni-containing steel because ferrites were absent, which indicated the successful replacement of 6 wt pct Ni by Mn, with cost reduction of 27 pct.     

Phase relationships in the fe-cr-mn-ni-c 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 quinary system Fe-Cr-Mn-Ni-C. Of the five quaternary systems that comprise the quinary system, this study was limited to the three quaternary systems which contain both carbon and iron as two of the components;viz.: Fe-Cr-Mn-C, Fe-Cr-Ni-C, and Fe-Mn-Ni-C, as well as all of the binary and ternary subsystems that have iron as a component. This paper discusses the modeling efforts for these systems, with particular emphasis on the ternary systems Fe-Cr-Mn and Fe-Mn-Ni and the quaternary systems Fe-Cr-Mn-C and Fe-Mn-Ni-C. The experimental investigation consisted of measurements of tie-lines for the liquid-delta (bcc) and the liquid-gamma (fcc) equilibria in the iron-rich corner of the Gibbs simplex bounded by 0 to 25 wt pct Cr, 0 to 12 wt pct Mn, 0 to 25 wt pct Ni, and 0 to 1.2 wt pct C (bal. Fe). The temperature ranged from 1811 to about 1750 K. Compositions for the tie-lines were obtained from liquid-solid equilibrium couples, and the temperatures for the equilibrium by differential thermal analysis (DTA). Parameters were selected in a thermodynamic model of the alloy system to minimize the square of the difference between experimentally and calculated tie-lines, the latter being implicitly a function of the derived parameters in the model. Binary and higher-order parameters were generally required. Ternary parameters were obtained on ironcarbon base alloys Fe-Cr-C, Fe-Mn-C, and Fe-Ni-C, and for the Fe-Cr-Ni system, but not for the Fe-Cr-Mn and Fe-Mn-Ni systems. Of the quaternary systems investigated, quaternary parameters were required only for theL/δ equilibrium in the Fe-Cr-Ni-C system; the Fe-Cr-Mn-C and Fe-Mn-Ni-C systems were found to be represented adequately by employing only binary and ternary parameters.     

Carbon paraequilibrium in austenitic stainless steel

Carburization of austenitic stainless steels under paraequilibrium conditions—i.e., at (low) temperatures where there is essentially no substitutional diffusion—leads to a family of steels with remarkable properties: enhanced hardness, resulting in improved wear behavior, enhanced fatigue, and corrosion resistance, and with essentially no loss in ductility. These enhanced properties arise from an enormous carbon solubility, which, absent carbide formation, is orders of magnitude greater than the equilibrium solubility. Using interaction parameters from the latest CALPHAD assessment of the Fe-Cr-Ni-carbon system, the authors have calculated the equilibrium and paraequilibrium carbon solubility in a model Fe-18Cr-12 Ni (wt pct) austenitic steel (essentially a model 316L composition), as well as the carbon solubility in this austenite when paraequilibrium carbide formation occurs (i.e., when carbides form in a partitionless manner). For temperatures in the range 725 to 750 K, the calculations predict a paraequilibrium carbon solubility of ～5.5 at. pct. Carburization of 316L stainless steel at these temperatures, however, results in significantly higher concentrations of carbon in solid solution—up to 12 at. pct. Much better agreement with experimental data is obtained by calculating the paraequilibrium carbon solubility using Wagner interaction parameters, taken from the most comprehensive experimental study of this system. The discrepancy between the two predicted solubilities arises because the CALPHAD Cr-carbon interaction parameters are not sufficiently exothermic at the low temperatures used for paraequilibrium carburization. After multiple paraequilibrium carburization cycles, carbide formation can occur. The carbides that form under these conditions do so in a near-partitionless manner (there is modest Ni rejection to the austenite/carbide interface) and have an unusual stoichiometry: M₅C₂ (the Hägg or η carbide).     

Phase relationships in the Fe-Cr-C 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-C system. The investigation consisted of measurements of tie-lines and the liquidus surface of the liquid-delta (bcc) and liquid-gamma (fcc) equilibria in the Gibbs triangle, bounded by 0 to 1.4 wt pct C and 0 to 25 wt pct Cr (bal. Fe). The peritectic surface of the three-phase equilibrium was also measured. The temperature ranged from 1811 to about 1750 K. The tie-lines were obtained from liquid-solid equilibrium couples, and the liquidus and peritectic surfaces, by differential thermal analysis (DTA). A statistical procedure was applied to determine from the experimental results the parameters required for a thermodynamic model of the system. Calculations by the model are in good agreement with the experimental results. As a consequence the model can be used to interpolate and extrapolate properties and compositions of phases in equilibrium in the system within the composition and temperature field investigated. D.M. KUNDRAT, formerly Research Fellow at Massachusetts Institute of Technology M. CHOCHOL, formerly Research Assistant, Massachusetts Institute of Technology     

Evaluation of Carbon Partitioning in New Generation of Quench and Partitioning (Q&P) Steels

Quenching and partitioning (Q&P) and a novel combined process of hot straining (HS) and Q&P (HSQ&P) treatments have been applied to a TRIP-assisted steel in a Gleeble®3S50 thermomechanical simulator. The heat treatments involved intercritical annealing at 800 °C and a two-step Q&P heat treatment with a partitioning time of 100 seconds at 400 °C. The “optimum” quench temperature of 318 °C was selected according to the constrained carbon equilibrium (CCE) criterion. The effects of high-temperature deformation (isothermal and non-isothermal) on the carbon enrichment of austenite, carbide formation, and the strain-induced transformation to ferrite (SIT) mechanism were investigated. Carbon partitioning from supersaturated martensite into austenite and carbide precipitation were confirmed by means of atom probe tomography (APT) and scanning transmission electron microscopy (STEM). Austenite carbon enrichment was clearly observed in all specimens, and in the HSQ&P samples, it was significantly greater than in Q&P, suggesting an additional carbon partitioning to austenite from ferrite formed by the deformation-induced austenite-to-ferrite transformation (DIFT) phenomenon. By APT, the carbon accumulation at austenite/martensite interfaces was observed, with higher values for HSQ&P deformed isothermally (≈ 11 at. pct), when compared with non-isothermal HSQ&P (≈ 9.45 at. pct) and Q&P (≈ 7.6 at. pct). Moreover, a local Mn enrichment was observed in a ferrite/austenite interface, indicating ferrite growth under local equilibrium with negligible partitioning (LENP).

     

Solidification of undercooled Fe-Cr-Ni alloys: Part I. Thermal behavior

Solidification of undercooled Fe-Cr-Ni alloys was studied by high-speed pyrometry during and after recalescence of levitated, gas-cooled droplets. Alloys were of 70 wt pct Fe, with Cr varying from 15 to 19.7 wt pct, balance was Ni. Undercoolings were up to about 300 K. Alloys of Cr content less than that of the eutectic (18.1 wt pct) have face-centered cubic (fee) (austenite) as their equilibrium primary phase, and alloys of higher Cr content have body-centered cubic (bcc) (ferrite) as their equilibrium primary phase. However, except at low undercoolings in the hypoeutectic alloys, all samples solidified with bcc as the primary phase; the bcc then transformed to fcc during initial recalescence for the lower Cr contents or during subsequent cooling for the higher Cr contents. The bcc-to-fcc transformation, whether in the semisolid or solid state, was detected by a second recalescence. In the hypoeutectic alloys, the growth of primary metastable bcc apparently results from preferred nucleation of bcc. The subsequent nucleation of fcc may occur at bcc/bcc grain boundaries. Formerly Graduate Student, Department of Materials Science and Engineering, Massachusetts Institute of Technology     

Optimization of Fe/Cr/C base structural Steels for improved strength and toughness

Optimization of the composition and the heat treatments to provide a microduplex structure of dislocated-autotempered lath martensite and thin film retained austenite for good combinations of mechanical properties has been attained for Fe/Cr/C base steels. Substituting 0.5 wt pct Mo to reduce Cr from 4 pct to 3 pct did not affect the microstructures nor the properties. It was found that air melting as compared to vacuum melting does not cause deterioration of toughness in Mn containing alloys but does so in Ni containing alloys. Tempered martensite embrittlement was confirmed as being due to the decomposition of retained austenite. Further improvements in the fracture toughness are achieved by double heat treatments which provide grain refinement. These alloys are considered to be very promising for structural applications.     

Effects of Heating and Cooling Rates on Phase Transformations in 10 Wt Pct Ni Steel and Their Application to Gas Tungsten Arc Welding

10 wt pct Ni steel is a high-strength steel that possesses good ballistic resistance from the deformation induced transformation of austenite to martensite, known as the transformation-induced-plasticity effect. The effects of rapid heating and cooling rates associated with welding thermal cycles on the phase transformations and microstructures, specifically in the heat-affected zone, were determined using dilatometry, microhardness, and microstructural characterization. Heating rate experiments demonstrate that the Ac₃ temperature is dependent on heating rate, varying from 1094 K (821 °C) at a heating rate of 1 °C/s to 1324 K (1051 °C) at a heating rate of 1830 °C/s. A continuous cooling transformation diagram produced for 10 wt pct Ni steel reveals that martensite will form over a wide range of cooling rates, which reflects a very high hardenability of this alloy. These results were applied to a single pass, autogenous, gas tungsten arc weld. The diffusion of nickel from regions of austenite to martensite during the welding thermal cycle manifests itself in a muddled, rod-like lath martensitic microstructure. The results of these studies show that the nickel enrichment of the austenite in 10 wt pct Ni steel plays a critical role in phase transformations during welding.     

Elevated temperature elastic constants of Fe-30 wt pct Ni in austenitic and martensitic conditions

A pulsed laser technique was used to measure the polycrystalline elastic moduli of the martensite and austenite phases of an Fe-30.1 wt pct Ni alloy between 298 and 900 K. The moduli of an Fe-29.5 wt pct Ni-0.1 wt pct C alloy were similarly determined at 298 K. These data showed that the shear modulus and Young’s modulus of martensite were slightly decreased by carbon. The moduli of austenite behaved in the expected manner, changing monotonically with temperature above the Curie temperature. The moduli of the martensite changed monotonically with temperature from 298 K until the martensite-to-austenite transformation temperature was reached at 650 K. At this temperature abrupt changes in moduli were observed. The same austenite start temperatures were determined both from moduli measurements and from dilatometric measurements. No unusual decrease of the martensite elastic constants was observed as a precursor to the reverse martensite-to-austenite transformation. Formerly with Sandia Laboratories, Albuquerque, New Mexico     

Atom-Probe Tomographic Investigation of Austenite Stability and Carbide Precipitation in a TRIP-Assisted 10 Wt Pct Ni Steel and Its Weld Heat-Affected Zones

Newly developed low-carbon 10 wt pct Ni-Mo-Cr-V martensitic steels rely on the Ni-enriched, thermally stable austenite [formed via multistep intercritical Quench-Lamellarization-Tempering (QLT)-treatment] for their superior mechanical properties, specifically ballistic resistance. Critical to the thermal stability of austenite is its composition, which can be severely affected in the weld heat-affected zones (HAZs) and thus needs investigations. This article represents the first study of the nanoscale redistributions of C, Ni, and Mn in single-pass HAZ microstructures of QLT-treated 10 wt pct Ni steels. Local compositions of Ni-rich regions (representative of austenite compositions) in the HAZs are determined using site-specific 3-D atom-probe tomography (APT). Martensite-start temperatures are then calculated for these compositions, employing the Ghosh-Olson thermodynamic and kinetics approach. These calculations predict that austenite (present at high temperatures) in the HAZs is susceptible to a martensitic transformation upon cooling to room temperature, unlike the austenite in the QLT-treated base-metal. While C in the QLT-treated base-metal is consumed primarily in MC and M₂C-type carbide precipitates (M is Mo, Cr, V), its higher concentration in the Ni-rich regions in the HAZs indicates the dissolution of carbide precipitates, particularly M₂C carbide precipitates. The role of M₂C carbide precipitates and austenite stability is discussed in relation to the increase in microhardness values observed in the HAZs, relative to the QLT-treated base-metal. Insights gained from this research on austenite stability and carbide precipitation in the single-pass HAZ microstructures will assist in designing multiple weld cycles for these novel 10 wt pct Ni steels.     

Effects of Residual Elements Arsenic,Antimony, and Tin on Surface Hot Shortness

Scrap-based electric arc furnace (EAF) steelmaking is limited by a surface cracking problem in the recycled steel products, which is known as surface hot shortness. This problem originates from the excessive amount of copper (Cu) in the steel scrap, which enriches during the oxidation of iron (Fe) and consequently melts and penetrates into the austenite grain boundaries. In this article, the effects of arsenic (As), antimony (Sb), and tin (Sn) on surface hot shortness were investigated. A series of Fe-0.3 wt pct Cu-x wt pct (As, Sb, or Sn) alloys with x content ranging from 0.06 to 0.10 wt pct was oxidized in air at 1423 K (1150 °C) for 60, 300, and 600 seconds inside the chamber of a thermogravimety analyzer (TGA) where heat is supplied through infrared radiation. Scanning electron microscopy (SEM) investigations show that (1) the presence of Sb and Sn results in severe grain boundary cracking, whereas the presence of As does not, (2) open cracks with Fe oxides were found beneath the oxide/metal interface in the Sb and Sn alloys, and (3) the oxide/metal interfaces for all As, Sb, and Sn alloys are planar. Penetration experiments of pure Cu and Cu-30 wt pct Sn liquid were also conducted in the chamber of a hot-stage confocal laser scanning microscopy (CLSM) in nonoxidizing atmosphere: (1) on the Fe-35 wt pct manganese (Mn) alloys to study the correlation between cracking and grain boundary characters, and (2) on the pure Fe substrates to exclude the bulk segregation effects of Sn on grain boundary cracking. It was found that grain boundary cracking rarely took place on low-energy grain boundaries. The results also suggest that the bulk segregation of Sn in the substrate is not necessary to promote significant grain boundary cracking, and as long as the liquid phase contains Sn, it will be highly embrittling.     

The distribution of chromium between ferrite and austenite and the thermodynamics of the α/γ equilibrium in the Fe-Cr and Fe-Mn Systems

New measurements of the α/γ equilibrium in the Fe-Cr system are presented and all the relevant experimental information now available, including thermodynamic data, is evaluated using a regular solution model. The two-phase field is calculated in good agreement with most of the experimental measurements. The point of minimum is obtained at 1119 K and 7.0 at. pct Cr (6.6 wt pct Cr) and the maximum solubility in austenite is 11.9 at. pct Cr (11.2 wt pct Cr). The thermodynamic quantities describing the effect of chromium on the relative stability of ferrite and austenite are similar to those for manganese. The comparison is based upon a new evaluation of the Fe-Mn system. In particular, low chromium contents are found to have a stabilizing effect on austenite up to a temperature of 1675 K.     

Determination of the Fe-Ni and Fe-Ni-P phase diagrams at low temperatures (700 to 300 °C)

The α + γ two-phase fields of the Fe-Ni and Fe-Ni (P saturated) phase diagrams have been determined in the composition range 0 to 60 wt pet Ni and in the temperature range 700 to 300 °C. The solubility of Ni in (FeNi)₃P was measured in the same temperature range. Homogeneous alloys were austenitized and quenched to form α₂, martensite, then heat treated to formα (ferrite) + γ (austenite). The compositions of the α and γ phases were determined with electron microprobe and scanning transmission electron microscope techniques. Retrograde solubility for the α/(α + γ) solvus line was demonstrated exper-imentally. P was shown to significantly decrease the size of the α + γ two-phase field. The maximum solubility of Ni in α is 6.1 ± 0.5 wt pct at 475 °C and 7.8± 0.5 wt pct at 450 °C in the Fe-Ni and Fe-Ni (P saturated) phase diagrams, respectively. The solubility of Ni in α is 4.2 ± 0.5 wt pct Ni and 4.9 ± 0.5 wt pct Ni at 300 °C in the Fe-Ni and Fe-Ni (P saturated) phase diagrams. Ternary Fe-Ni-P isothermal sections were constructed between 700 and 300 °C. Formerly Research Assistant in Department of Metallurgy & Materials Engineering, Lehigh University, Bethlehem, PA.     

Evolution of secondary phases in Cr-V low-alloy steels during aging

The influence of both bulk vanadium content and aging conditions on the evolution of secondary phases in Cr-V low-alloy steels was studied. Three 0.1C-0.9Cr-V steels with different vanadium contents (0, 0.258, and 0.512 wt pct) were aged for 100 to 5,000 hours at 773, 853, 953, and 993 K. In the investigation, a limited experimental program (transmission electron microscopy (TEM)) was combined with credible thermodynamic predictions (ThermoCalc). Going out from the good agreement between the predicted and experimental results, behavior of the iron-rich M₇C₃ carbide in time-temperature scale was characterized. The influence of bulk vanadium content was determined on appearance of the M₃C carbide in equilibrium, temperature of the M₇C₃ carbide precipitation, metal compositions of M₃C or M₇C₃ carbides, and vanadium portion in the metallic part of the MX phase.     

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

The phase relationships between the liquid phase and the primary solid phases were investigated in the iron-rich comer of the Fe-Cr-Ni-C system as part of a larger study of the Fe-Cr-Mn-Ni-C system. The investigation consisted of measurements of tie-lines for the liquid-delta (bcc) and the liquid-gamma (fcc) equilibria in the iron-rich corner of the Gibbs tetrahedron bounded by 0 to 25 wt Pct Cr, 0 to 25 wt Pct Ni, and 1.2 wt Pct C (bal. Fe). The temperature ranged from 1811 to 1750 K. Compositions for the tie-lines were obtained from liquid-solid equilibrium couples and the temperatures of the equilibrium, by differential thermal analysis (DTA). A mathematical procedure was employed on the experimental data to obtain parameters for a thermodynamic model of the alloy system. This involved minimization of an error function. The details of this analysis are discussed fully in this paper. Calculations by the model employing the “best-set” parameters are in good agreement with the experimental results. The usefulness of the model is demonstrated by calculation of the three-phase equilibrium in the quaternary system as a function of temperature. Formerly Research Fellow, Massachusetts Institute of Technology, is Senior Research Engineer, Armco Inc., Middletown, OH 45043     

Effects of Ni on austenite stability and fracture toughness in high Co-Ni secondary hardening steel

Three kinds of high Co-Ni secondary hardening steels with different Ni contents were studied.The nanoscale austenite layers formed at the interface of matensite laths were observed.Both observation and diffusion kinetic simulation results showed that both Ni and Co did not obtain enough time to get the equilibrium content in this system.The Ni content in austenite layers decreased significantly,and Co content increased slightly with the decrease of Ni content in overall composition.The austenite stability was estimated by Olson-Cohen model,in which both chemical and mechanical driving force could be calculated by equilibrium thermodynamic and Mohr′s circle methods,respectively.Simulation and mechanical test results showed that the decrease of Ni content in austenite layers would cause the change of austenite stability and decrease the fracture toughness of the steels.When the Ni content in the overall composition was lower than 7wt.%,the Ni content inγphase would be lower than 20 wt.%.And the simulation value of Mσs(stress-induced critical martensite transformation temperature)would be up to 80°C,which was about 60°C higher than room temperature.Based on the analysis,the Ni content in the overall composition of high Co-Ni secondary hardening steels should be higher than 8wt.% in order to obtain a good fracture toughness.     

Decomposition of Fe-Ni martensite: Implications for the low-temperature (≤500 °C) Fe-Ni phase diagram

The low-temperature (<500 °C) decomposition of Fe-Ni martensite was studied by aging martensitic Fe-Ni alloys at temperatures between 300 °C and 450 °C and by measuring the composition of the matrix and precipitate phases using the analytical electron microscope (AEM). For aging treatments between 300 °C and 450 °C, lath martensite in 15 and 25 wt pct Ni alloys decomposed with γ [face-centered cubic (fcc)] precipitates forming intergranularly, and plate martensite in 30 wt pct Ni alloys decomposed with γ (fcc) precipitates forming intragranularly. The habit plane for the intragranular precipitates is {111}_fcc parallel to one of the {110}_bcc planes in the martensite. The compositions of the γ intergranular and intragranular precipitates lie between 48 and 58 wt pct Ni and generally increase in Ni content with decreasing aging temperature. Diffusion gradients are observed in the matrix α [body-centered cubic (bcc)] with decreasing Ni contents close to the martensite grain boundaries and matrix/precipitate boundaries. The Ni composition of the matrix α phase in decomposed martensite is significantly higher than the equilibrium value of 4 to 5 wt pct Ni, suggesting that precipitate growth in Fe-Ni martensite is partially interface reaction controlled at low temperatures (<500 °C). The results of the experimental studies modify the γ/α + γ phase boundary in the present low-temperature Fe-Ni phase diagram and establish the eutectoid reaction in the temperature range between 400 °C and 450 °C. Formerly Research Assistant, Department of Materials Science and Engineering, Lehigh University