Effects of thermal cycling on the kinetics of the γ → ε martensitic transformation in an Fe-17 wt pct Mn alloy

The thermal cycling of an Fe-17 wt pct Mn alloy between 303 and 573 K was performed to investigate the effects of thermal cycling on the kinetics of the γ → ε martensitic transformation in detail and to explain the previous, contrasting results of the change in the amount of ε martensite at room temperature with thermal cycling. It was observed that the shape of the γ → ε martensitic transformation curve (volume fraction vs temperature) changed gradually from a C to an S curve with an increasing number of thermal cycles. The amount of ε martensite of an Fe-17 wt pct Mn alloy at room temperature increased with thermal cycling, in spite of the decrease in the martensitic start (M _s) temperature. This is due to the increase in transformation kinetics of ε martensite at numerous nucleation sites introduced in the austenite during thermal cycling.     

Effects of thermal cycling on the martensitic transformation in two-phase α/β brasses

The effects of thermal cycling between the parent and martensite phases of two-phase α/β CuZn alloys have been studied by electrical resistance-temperature measurements, optical microscopy, and transmission electron microscopy (TEM). The martensite start (M_s) temperature is dominated primarily by the composition of the β phase but increases substantially between the first and second cycles because of deformation of the α particles and a resultant change in the internal strain fields of the system. With increasing thermal cycling, the M_s temperature increases slightly and eventually becomes constant. However, the transformation hysteresis becomes smaller, and more perfect thermoelastic behavior is found. The number of vestigial deformation markings in the β phase is increased by thermal cycling and becomes more distinct; the dislocation density in the β phase is also increased and features a more crystallographic arrangement. The vestigial deformation of the β phase is instrumental in subsequent martensite nucleation and in creating a martensite microstructural memory.     

Origin of Microstructural Irreversibility in Ni-Ti Based Shape Memory Alloys during Thermal Cycling

Different microstructures of Ni-Ti- and Ni-Ti-Fe-based shape memory alloys were subjected to thermal cycling: dipping in liquid nitrogen, for approximately 5 minutes, and then bringing it back to room temperature or austenite (cubic: B2) ↔ martensite (monoclinic: B19′) reversible solid-state phase transformation. Direct electron backscattered diffraction (EBSD) observations could bring out aspects of microstructural irreversibilities: namely, changes in grain size, misorientation buildup, and presence of retained martensite. The average changes in grain size (Δd) differed by almost 2 to 4 times between different microstructures. The highest Δd was typically observed in structures having maximum clustering of fine (d < 5 μm) grains. The sample with highest Δd was also subjected to multiple thermal cycling. Although Δd scaled linearly with d after the first thermal cycle, the scatter increased during subsequent thermal cycles. Grain or orientations deviating from the linear behavior were clearly anisotropic crystallographically. With repeated thermal cycling, the patterns of changes in Δd, austenite misorientation, and retained martensite content were similar. A phenomenological model or hypothesis, based on 40 deg á 001 ñ \left\langle {001} \right\rangle orientation relationship between austenite and martensite phases, was proposed to address the observed patterns of microstructural irreversibility.     

The martensite transformation in FeNiC alloys

The effect of austenite defect structure upon the sub-zero martensite burst transformation temperature in FeNiC has been investigated using a combination of optical and electron microscopy, differential scanning calorimetry and microhardness testing. In the absence of a change in composition or dislocation density, the martensite start transformation temperature (M_s) was found to be determined by the grain size of the austenite. Above a grain size of 150 μm, M_s was found to be independent of grain size, but below 150 μm, the transformation temperature was strongly depressed by up to approximately 50 K at a grain size of 10 μm. For any given grain size, an increase in the dislocation density from that typical of a fully recrystallised specimen, i.e. approximately 10¹⁰ lines m⁻², to that of approximately 10¹⁵ lines m⁻² raised M_s by approximately 15 K. The depression of M_s and reduction in the initial burst size of the transformation with decreasing grain size was found to be related to the observation that a fine grain size results in a heterogeneous transformation restricted to a few small pockets of grains. The depression of M_s in the fine grained alloy is consistent with a segregation of active martensite nuclei into a few small grains, a suppression of the autocatalytic stimulation of martensite plates between adjacent grains, and a possible reduction in the number of martensite nuclei.     

An investigation of the effects of austenite strength and austenite stacking fault energy on the morphology of martensite in Fe-Ni-Cr-0.3C alloys

The relative effects of austenite stacking fault energy and austenite yield strength on martensite morphology have been investigated in a series of three Fe-Ni-Cr-C alloys. Carbon content (0.3 wt pct) andM ₆ temperature (− 15°) were held constant within the series. Austenite yield strength atM _s was measured by extrapolating elevated temperature tensile data. Austenite stacking fault energy was measured by the dislocation node technique. Martensite morphologies were characterized by transmission electron microscopy and electron diffraction techniques. A transition from plate to lath martensite occurred with decreasing austenite stacking fault energy. The austenite yield strength atM _s for the low SFE, lath-forming alloy was found to be higher than previously reported for lath-forming alloys. The relative effects of these variables on martensite morphologies in these alloys is discussed.     

Stabilization mechanisms of retained austenite in transformation-induced plasticity steel

Three stabilization mechanisms—the shortage of nuclei, the partitioning of alloying elements, and the fine grain size—of the remaining metastable austenite in transformation-induced plasticity (TRIP) steels have been studied by choosing a model alloy Fe-0.2C-1.5Mn-1.5Si. An examination of the nucleus density required for an athermal nucleation mechanism indicates that such a mechanism needs a nucleus density as large as 2.5 · 10¹⁷ m⁻³ when the dispersed austenite grain size is down to 1 μm. Whether the random nucleation on various heterogeneities is likely to dominate the reaction kinetics depends on the heterogeneous embryo density. Chemical stabilization due to the enrichment of carbon in the retained austenite is the most important operational mechanism for the austenite retention. Based on the analysis of 57 engineering steels and some systematic experimental results, an exponential equation describing the influence of carbon concentration on the martensite start (M _s) temperature has been determined to be M _s (K)=273+545.8 · e ^−1.362w _c(mass pct). A function describing the M _s temperature and the energy change of the system has been found, which has been used to study the influence of the grain size on the M _s temperature. The decrease in the grain size of the dispersed residual austenite gives rise to a significant decrease in the M _s temperature when the grain size is as small as 0.1 μm. It is concluded that the influence of the grain size of the retained austenite can become an important factor in decreasing the M _s temperature with respect to the TRIP steels.     

The reversible martensite transformation in iron-platinum alloys near Fe3Pt

A series of iron-platinum alloys containing 25 or 27 at. pct platinum and with ordering of the γ-phase varying from substantial disorder to nearly complete order have been thermally cycled between 25°C and - 196°C. The kinetics of the γ⇌α transformations, the hysteresis revealed by electrical resistanceJtemperature plots, the thermoelastic growth and the reappearance of an identical microstructure after thermal cycling (the microstructural memory effect) were studied as a function of the ordering of the γ-phase. Thermoelastic growth does not appear to be affected by changes in the degree of order of partially ordered specimens but the microstructural memory was imperfect in the most highly ordered specimen examined. In agreement with earlier observations by Dunne and Wayman,³ the difference between the A_s and M_s temperatures and the hysteresis decrease markedly as the order is increased. It is shown by transmission electron microscopy that in all but the most highly-ordered specimens the α- γ transformation produces plates of austenite with a high density of dislocations. These plates are separated from the surrounding untransformed parent austenite by arrays of dislocation loops lying in the interfaces between untransformed parent austenite and the original martensite plates. All the dislocations have a Burgers vector direction which is the same as that of the usual slip dislocation in austenite. Such dislocations lying in a habit plane must be sessile. In the well-ordered specimen dislocation pairs, typical of glide dislocations in a crystal with long-range order, were formed in the austenite formed by the reverse transformation. These dislocations were segregated into roughly plate-like clusters, but the number of clusters in unit volume was appreciably less than the number of original plates of martensite. In this case, no arrays of sessile loops of dislocations mark the locations of the original martensite-austenite interface. It is deduced from the microscopic and kinetic results that the inherited nuclei responsible for the microstructural memory effect are located in localized volumes of highly dislocated austenite formed by the α- γ transformation. No unique dislocation configurations which could be associated with specific nuclei were found. The effects of ordering on the various kinetic effects and the microstructural memory are discussed in terms of the concept of inherited nuclei, the change of the flow stress of the γ-phase with ordering and temperature and the variation of T_o and the transformation driving-force with ordering. Formerly at Northwestern University     

Substructure of ausformed martensite in Fe-Ni and Fe-Ni-C alloys

The martensite substructure after ausforming has been studied for two different martensite morphologies: partially twinned, lenticular martensite (Fe-33 pct Ni, M_s =-105‡C) and completely twinned “thin plate” martensite (Fe-31 pct Ni-0.23 pct C, M_s = -170‡C), and in both cases ausforming produces a dislocation cell structure in the austenite which is inherited, without modification, by the martensite. In the Fe-Ni alloy, the dislocation cell structure is found in both the twinned (near the midrib) and untwinned (near the interface) regions, the latter also containing a regular dislocation network generated by the transformation itself and which is unaltered by the austenite dislocation cell structure. Similarly, in the Fe-Ni-C alloy, the transformation twins are unimpeded by the prior cell structure. These observations show that carbide precipitation during ausforming is not necessarily required to pin the austenite cell structure and that the martensite-austenite interface, backed by either twins or dislocations, does not exhibit a ”sweeping” effect. Although the martensite transformation twins are not inhibited by the ausforming cell structure, they do undergo a refinement with increased ausforming, and it is indicated that the transformation twin width in martensite depends on the austenite hardness. However, the relative twin widths remain unchanged, as expected from the crystallographic theory. T. MAKI, Formerly with the University of Illinois     

The Effect of an Inert Oxide Particle Dispersion on the Morphology of Martensite in Fe-27Ni-0.025C Alloys

A series of dispersion strengthened Fe-Ni alloys has been prepared by powder metallurgical techniques. This series was designed to permit evaluation of the relative effects of M_s temperature, chemical driving force, and austenite yield strength on resultant martensite morphology without altering matrix chemistry. Using a carefully selected lath-forming Fe-27Ni-.025C base alloy, incremental additions of an inert oxide dispersion resulted in a decrease in M_s temperature, an increase in the thermodynamic driving force at M_s, and an increase in the austenite yield strength at M_s to values beyond those previously associated with the lath-to-plate morphology transition. As the M_s temperature dropped below about 0 °C, martensite morphology shifted from lath to an intermediate “twinned lath” to plate, while holding constant both matrix chemistry and thermal history. Previous correlations of thermodynamic driving force and austenite yield strength with martensite morphology have been shown to break down. It is concluded that the observed transition from lath to plate martensite in the present alloy series was induced primarily by the depression of M_s temperature into the plate-forming temperature regime of the Fe-Ni system.     

Influence of strain rate and temperature on the deformation behavior of a metastable high carbon iron-nickel austenite

Austenitic specimens of Fe-15 wt pct Ni-0.8 wt pct C were tested in tension at strain rates of 10⁻⁴ s⁻¹ and 10⁻¹ s⁻¹ over the temperature range −20°C to 60 °C. The influence of strain rate and temperature on the deformation behavior depended on whether stress-assisted or strain-induced martensitic trans-formation occurred during testing. Under conditions of stress-assisted transformation, the ductility was low and independent of strain rate. However, when strain-induced transformation occurred, the duc-tility increased significantly and the higher strain rate resulted in greater ductility and more transfor-mation. Although the ductility increased continuously with temperature, the amount of strain-induced transformation decreased and no martensite was observed above 40 °C. Microstructural examination showed that the martensite was replaced by intense bands and that these bands contained very fine (111) fcc twins. The twinning resulted in enhanced plasticity by providing an additional mode of deformation as slip became more difficult due to dynamic strain aging at the higher temperature. This study confirms that the substructure following deformation will depend on the proximity of the deformation temperature to theM _s ^σ temperature. At temperatures much greater thanM _s ^σ , austenite twinning will occur, while at temperatures close toM _s ^σ , bcc martensite will form.     

Magnetic investigation of martensite ⇌ austenite transformations in Fe-Ni-Co alloys

The martensite ⇌ austenite transformations were investigated in Fe-Ni-Co alloys containing about 65 wt pct Fe and up to 15 wt pct Co. A change in morphology of martensite from plate-like to lath-type occurred with increasing cobalt content; this change in morphology correlates with the disappearance of the Invar anomaly in the austenite. The martensite-to-austenite reverse transformation differed depending on martensite morphology. Reversion of plate-like martensite was found to occur by simple disintegration of the martensite platelets. Reverse austenite formed from lath-type martensite was not retained when quenched from much aboveA _s, with microcracks forming during theM→γ→M transformation.     

The relationship between austenite strength and the transformation to martensite in Fe-10 pct Ni-0.6 pct C alloys

The effect of austenite yield strength on the transformation to martensite was investigated in Fe-10 pct Ni-0.6 pct C alloys. The strength of the austenite was varied by 1) additions of yttrium oxide particles to the base alloy and 2) changing the austenitizing temperature. The austenite strength was measured at three temperatures above theM _s temperature and the data extrapolated to the experimentally determinedM _s temperature. It is shown that the austenite yield strength is determined primarily by the austenite grain size and that the yttrium oxide additions influence the effect of austenitizing temperature on grain size. As the austenite yield strength increases, both theM _s temperature and the amount of transformation product at room temperature decrease. The effect of austenitizing temperature on the transformation is to determine the austenite grain size. The results are consistent with the proposal¹ that the energy required to overcome the resistance of the austenite to plastic deformation is a substantial portion of the non-chemical free energy or restraining force opposing the transformation to martensite.     

The enhancement of strengthening dislocated martensite

The basis of this work was the investigation of improving the tensile properties of dislocated martensites by dispersion of precipitates in the austeniteprior to the martensite transformation. Two types of precipitation-hardenable austenitic alloys were used. One is based on Fe-22 Ni-4 Mo-0.28 C where the precipitates are Mo₂C and are obtained by ausforming and aging, and the other is Fe-28 Ni-2 Ti where the precipitates are the coherent fccγ’ (Ni₃Ti) ordered phase obtained by ausaging. After the austenitic dispersion treatment both alloys were transformed to martensite by quenching to liquid nitrogen and the properties measured and compared to martensites obtained by conventional heat treatment (i.e. no precipitates in austenite). The results show that prior dispersions increase the strength of martensite and this is interpreted as being due to an increase in dislocation density resulting from dislocation multiplication at the particles during the γ →M _s transformation. In addition, the stabilities of the austenitic alloys are such that upon certain aging treatments, the alloys transform partially to martensite (due to precipitation) and “composite” materials are obtained whose strength depends on the volume fraction and yield strengths of the phases present. Formerly Graduate Student, Department of Materials Science and Engineering, University of California, Berkeley, Calif.     

The development of martensitic microstructure and microcracking in an Fe-1.86C alloy

The development of the martensitic microstructure in a 1.86 wt pct C steel has been followed by quantitative metallographic measurements over the transformation range of 0.12 to 0.50 fraction transformed (f). The transformation kinetics are described by the equationf = 1 − exp [−0.008 (M _s − T_q)] where M_s and T_q are the martensite start and the quenching temperatures respectively. Fullman’s analysis shows that the average volume per martensite plate decreases by almost an order of magnitude over the transformation range studied, but this decrease is less than that predicted by the Fisher analysis for partitioning of austenite by successive generations of martensite. Microcracking increases with increasingf up to 0.3, but does not increase forf above 0.3 where transformation proceeds by the nucleation of large numbers of small martensite plates. These observations indicate that a critical size of martensite plate is necessary to cause microcracking. Formerly Postdoctoral Fellow at Lehigh University     

Shock-induced martensitic transformations in near-equiatomic NiTi alloys

Shock-impact generated tensile-stress pulses were used to induce B2-to-monoclinic martensitic transformations in two near-equiatomic NiTi alloys having different martensite transformation start (M _s ) temperatures. The NiTi-I alloy (M _s ≈+27 °C) impacted at room temperature at 2.0 and 2.7 GPa tensile stress-pulse magnitude, showed acicular martensite morphology. These martensite needles had a substructure containing microtwins, typical of “stress-assisted” martensite. The NiTi-II alloy (M _s ≈−45 °C) showed no martensite formation when shocked with tensile-stress pulses of 2 GPa. For tensile stresses of 4.1 GPa, the alloy showed spall initiation near the region of maximum tensile-stress duration. In addition, monoclinic martensite needles, with a well-defined dislocation substructure, typical of “strain-induced” martensite, were seen clustering around the spall region. No stress-assisted martensite was formed in this alloy due to its very low M _s temperature. The present article documents results of the use of a metallurgical technique for generating large-amplitude tensile stress pulses of finite duration for studies of phase transformations involving changes from a high density to a low density state.     

Substructure of ausformed martensite in Fe-Ni and Fe-Ni-C alloys

The martensite substructure after ausforming has been studied for two different martensite morphologies: partially twinned, lenticular martensite (Fe-33 pct Ni, M_s =-105?C) and completely twinned “thin plate” martensite (Fe-31 pct Ni-0.23 pct C, M_s = -170?C), and in both cases ausforming produces a dislocation cell structure in the austenite which is inherited, without modification, by the martensite. In the Fe-Ni alloy, the dislocation cell structure is found in both the twinned (near the midrib) and untwinned (near the interface) regions, the latter also containing a regular dislocation network generated by the transformation itself and which is unaltered by the austenite dislocation cell structure. Similarly, in the Fe-Ni-C alloy, the transformation twins are unimpeded by the prior cell structure. These observations show that carbide precipitation during ausforming is not necessarily required to pin the austenite cell structure and that the martensite-austenite interface, backed by either twins or dislocations, does not exhibit a ”sweeping” effect. Although the martensite transformation twins are not inhibited by the ausforming cell structure, they do undergo a refinement with increased ausforming, and it is indicated that the transformation twin width in martensite depends on the austenite hardness. However, the relative twin widths remain unchanged, as expected from the crystallographic theory.     

Stress-Assisted and strain-induced martensites in FE-NI-C alloys

A metallographic study was made of the martensite formed during plastic straining of metastable, austenitic Fe-Ni-C alloys withM _s temperatures below 0°C. A comparison was made between this martensite and that formed during the deformation of two TRIP steels. In the Fe-Ni-C alloys two distinctly different types of martensite formed concurrently with plastic deformation. The large differences in morphology, distribution, temperature dependence, and other characteristics indicate that the two martensites form by different transformation mechanisms. The first type, stress-assisted martensite, is simply the same plate martensite that forms spontaneously belowM _s except that it is somewhat finer and less regularly shaped than that formed by a temperature drop alone. This difference is due to the stress-assisted martensite forming from cold-worked austenite. The second type, strain-induced martensite, formed along the slip bands of the austenite as sheaves of fine parallel laths less than 0.5μm wide strung out on the {111}_γ planes of the austenite. Electron diffraction indicated a Kurdjumov-Sachs orientation for the strain-induced martensite relative to the parent austenite. No stress-assisted, plate martensite formed in the TRIP steels; all of the martensite caused by deformation of the TRIP steels appeared identical to the strain-induced martensite of the Fe-Ni-C alloys. It is concluded that the transformation-induced ductility of the TRIP steels is a consequence of the formation of strain-induced martensite. Formerly a graduate student at Stanford University     

Influence of austenite strength on martensite start temperature Ms

It is known that austenite strength determines the morphology of the new phase during martensitic transformation. As the strength of austenite influences the growth of a martensite crystal, i.e. the movement of the austenite/martensite interface, a correlation between strength of the parent phase and M_s has to exist. M_s depends on thermodynamical and mechanical properties of the alloys. To distinguish the individual variables, austenite strength was changed by different hardening mechanisms: solid solution hardening, plastic deformation or both.     

The effect of quench rate on the properties and morphology of ferrous martensite

The effect of high quench rate on theM _s temperature, percent transformed, martensite morphology and austenite hardness has been studied for several Fe-Ni-C steels. For these steels the quench rate was varied only in the austenite region. TheM _s temperature was found to increase with increased quench rate for both high- and low carbon steels while the percent transformation increased or decreased depending upon the morphology of the steel. No variations in martensite hardness were found in the as-quenched condition, but a difference in tempering rate was found between fast and slow quenched specimens. Austenite hardness decreased slightly with increasing quench rate while the martensite morphology changed from lath to plate. Parallel aligned plate structures were observed which resemble a twinned lath morphology. It was demonstrated that the actual difference between this morphology and a true lath morphology is the self-accommodating nature of the lath structure. The morphology changes were compared to the measured changes in martensite properties in order to identify the mechanism of the morphology shift. It was concluded that for these alloys the morphology was controlled by the austenite shear mode. S. J. Donachie was formerly a Graduate Assistant.     

Effect of heat and thermomechanical treatments on the linear thermal expansion coefficient of an N30K10T3 invar

The N30K10T3 invar that has a temperature of the onset of martensite transformation of austenite M _s ≈ −80°C and a Curie point θ_C ≈ 200°C after water-quenching from 1150°C is studied. The decomposition of a supersaturated solid solution is shown to substantially influence the linear thermal expansion coefficient. The alloy is studied in the following three initial states: after quenching, after phase transformation-induced hardening (γ → α_m → γ_p.h), and after cold (20°C) plastic deformation by 30%.