Microstructural dependence of Fe-high Mn tensile behavior

The tensile properties of Fe-high Mn (16 to 36 wt pct Mn) binary alloys were examined in detail at temperatures from 77 to 553 K. The Mn content dependence of the deformation and fracture behavior in this alloy system has been clarified by placing special emphasis on the starting microstructure and its change during deformation. In general, the intrusion of hcp epsilon martensite (ε) into austenite (γ) significantly increases the work hardening rate in these alloys by creating strong barriers to further plastic flow. Due to the resulting high work hardening rates, large amounts of e lead to high flow stresses and low ductility. Alloys of 16 to 20 wt pct Mn are of particular interest. While these alloys are thermally stable with respect to bcc α’ martensite formation, 16 to 20 wt pct Mn alloys undergo a deformation induced ε →α’ transformation. The martensitic transformation plays two contrasting roles. The stress-induced ε→ α’ transformation decreases the initial work hardening rate by reducing locally high internal stress. However, the work hardening rate increases as the accumulated α’ laths become obstacles against succeeding plastic flow. These rather complicated microstructural effects result in a stress-strain curve of anomolous shape. Since both the M_s and M_d temperatures for both the ε and α’-martensite transformations are strongly dependent on the Mn content, characteristic relationships between the tensile behavior and the Mn content of each alloy are observed.     

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.     

Tensile deformation behavior of mechanically stabilized Fe-Mn austenite

The tensile deformation behavior of mechanically-stabilized austenite is investigated in Fe-Mn binary alloys. A 30 pct thickness reduction by rolling at 673 K (above the A_f temperature) largely suppresses the austenite (γ) to hcp epsilon martensite (ε) transformation in 17Mn and 25Mn steels. However, the deformation behavior of the mechanically stabilized austenite in the two alloys differs significantly. In 25Mn steel, the onset of plastic deformation is due to the stress-induced γ→ ε transformation and results in a positive temperature dependence of the yield strength. The uniform elongation is enhanced by the γ → ε transformation during deformation. In 17Mn steel, bccα′ martensite is deformation-induced along with e and a plateau region similar to Lüders band deformation appears at the beginning of the stress-strain curve. The mechanical stabilization of austenite also suppresses the intergranular fracture of 17Mn steel at low temperatures. M. STRUM, formerly Candidate for Ph.D. at the University of California at Berkeley     

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.     

A new equation for the Cr equivalent in 9 to 12 pct Cr steels

In advanced 9 to 12 pct Cr steels, the Cr equivalent is used as a measure to check the formation of δ-ferrite. In the present analysis, 29 alloys of varying composition were vacuum induction melted, and the amounts of δ-ferrite were measured in as-tempered conditions. Based on this and previous results on 9 to 12 pct Cr steels, a new equation for the Cr equivalent is proposed and correlated with the amount of δ-ferrite formation. Results indicate that the new Cr equivalent equation shows better correlation than previous equations and predicts the amount of δ-ferrite formed reasonably well.     

The microstructure of an Fe-Mn-Si-Cr-Ni stainless steel shape memory alloy

The microstructure and phase stability of the Fe-15Mn-7Si-9Cr-5Ni stainless steel shape memory alloy in the temperature range of 600 °C to 1200 °C was investigated using optical and transmission electron microscopy, X-ray diffractometry (XRD), differential scanning calorimetry (DSC), and chemical analysis techniques. The microstructural studies show that an austenite single-phase field exists in the temperature range of 1000 °C to 1100 °C, above 1100 °C, there exists a three-phase field consisting of austenite, δ-ferrite, and the (Fe,Mn)₃Si intermetallic phase; within the temperature range of 700 °C to 1000 °C, a two-phase field consisting of austenite and the Fe₅Ni₃Si₂ type intermetallic phase exists; and below 700 °C, there exists a single austenite phase field. Apart from these equilibrium phases, the austenite grains show the presence of athermal ɛ martensite. The athermal α′ martensite has also been observed for the first time in these stainless steel shape memory alloys and is produced through the γ-ɛ-α′ transformation sequence.     

Microstructure and high-temperature tensile deformation of tiai(si) alloys made from elemental powders

Two ternary TiAl-based alloys with chemical compositions of Ti-46.4 at. pct Al-1.4 at. pct Si (Si poor) and Ti-45 at. pct Al-2.7 at. pct Si (Si rich), which were prepared by reaction powder processing, have been investigated. Both alloys consist of the intermetallic compounds y-TiAl, α₂-Ti₃Al, and ξ-Ti₅(Si, Al)₃. The microstructure can be described as a duplex structure(i.e., lamellar γ/α₂ regions distributed in γ matrix) containing ξ precipitates. The higher Si content leads to a larger amount of ξ precipitates and a finer y grain size in the Si-rich alloy. The tensile properties of both alloys depend on test temperature. At room temperature and 700 °C, the tensile properties of the Si-poor alloy are better than those of the Si-rich alloy. At 900 °C, the opposite is true. Examinations of tensile deformed specimens reveal ξ-Ti₅(Si, Al)₃ particle debonding and particle cracking at lower test temperatures. At 900 °C, nucleation of voids and microcracks along lamellar grain boundaries and evidence for recovery and dynamic recrystallization were observed. Due to these processes, the alloys can tolerate ξ-Ti₅(Si, Al)₃ particles at high temperature, where the positive effect of grain refinement on both strength and ductility can be utilized.     

Effect of Co Addition on the Microstructure, Martensitic Transformation and Shape Memory Behavior of Fe-Mn-Si Alloys

The effect of Co addition has been studied in Fe-30Mn-6Si-xCo (x = 0 to 9 wt pct) shape memory alloys in terms of their microstructure, martensitic transformation and shape recovery. Microstructural investigations reveal that in Fe-Mn-Si-Co alloys, the microstructure remains single-phase austenite (??) up to 5 pct Co and beyond that becomes two-phase comprising ?? and off-stoichiometric (Fe,Co)₅Mn₃Si₂ intermetallic ??-phases. The forward ??-?? martensite transformation start temperature (M _S) decreases with the addition of Co up to 5 pct, and alloys containing more than 5 pct Co, show slightly higher M _S possibly on account of two-phase microstructure. Unlike M _S, the ??-?? reverse transformation start temperature (A _S) has been found to remain almost unaltered by Co addition. In general, addition of Co to Fe-Mn-Si alloys deteriorates shape recovery due to decreasing resistance to plastic yielding concomitant with the formation of stress induced ?? martensite. However, there is an improvement in shape recovery beyond 5 pct Co addition, possibly due to the strengthening effect arising from the presence of (Fe,Co)₅Mn₃Si₂ precipitates within the two-phase microstructure and due to higher amount of stress induced ?? martensite.     

A melting and solidification study of alloy 625

The melting and solidification behavior of Alloy 625 has been investigated with differential thermal analysis (DTA) and electron microscopy. A two-level full-factorial set of chemistries involving the elements Nb, C, and Si was studied. DTA results revealed that all alloying additions decreased the liquidus and solidus temperatures and also increased the melting temperature range. Terminal solidification reactions were observed in the Nb-bearing alloys. Solidification microstructures in gastungsten-arc welds were characterized with transmission electron microscopy (TEM) techniques. All alloys solidified to an austenitic (γ) matrix. The Nb-bearing alloys terminated solidification by forming various combinations of γ/MC(NbC), γ/Laves, and γ/M₆C eutectic-like constituents. Carbon additions (0.035 wt pct) promoted the formation of the γ/MC(NbC) constituent at the expense of the γ/Laves constituent. Silicon (0.4 wt pct) increased the formation of the yJLaves constituent and promoted formation of the γ/M₆C carbide constituent at low levels (<0.01 wt pct) of carbon. When both Si (0.4 wt pct) and C (0.035 wt pct) were present, the γ/MC(NbC) and γ/Laves constituents were observed. Regression analysis was used to develop equations for the liquidus and solidus temperatures as functions of alloy composition. Partial derivatives of these equations taken with respect to the alloying variables (Nb, C, Si) yielded the liquidus and solidus slopes t(m _L , m _S ) for these elements in the multicomponent system. Ratios of these liquidus to solidus slopes gave estimates of the distribution coefficients (k) for these same elements in Alloy 625.     

The relationship between toughness and microstructure in Fe-high Mn binary alloys

The influence of Mn content on the ductile-brittle transition in 16 to 36 wt pct Mn steels was investigated and interpreted in light of the evolving microstructure. It was found that when hcp ε martensite is present in the as-quenched condition or forms during deformation, it lowers the toughness. In 25Mn steel, the stress concentrations at e plate intersections result in the formation of planar void sheets along the {111}_γ planes. The deformation-induced α’ martensite in 16 to 20 pct Mn alloys enhances the toughness, but leads to a ductile-to-brittle transition at low temperatures that is due to the intrusion of an intergranular fracture mode. Binary alloys with greater than 31 pct Mn also fracture in an intergranular mode at 77 K although the impact energy remains quite high. Auger spectroscopy of the fracture surfaces shows no evidence of significant impurity segregation, which suggests the importance of slip heterogeneity in controlling intergranular fracture in these alloys.     

The Influence of Cr on the Solidification Behavior of Polycrystalline γ(Ni)/γ′(Ni3Al)-δ(Ni3Nb) Eutectic Ni-Base Superalloys

In the current investigation, the effect of Cr on the solidification characteristics and as-cast microstructure of pseudobinary γ-δ eutectic alloys based on a near-eutectic composition (Ni-5.5Al-13.5Nb at. pct) was investigated. It was found that Cr additions promote the formation of a higher volume fraction of γ-δ eutectic microstructure in the interdendritic region. Increasing levels of Cr also triggered morphological changes in the γ-δ eutectic and the formation of γ-γ′-δ ternary eutectic during the last stage of solidification. A detailed characterization of the as-cast alloys also revealed that Cr additions suppressed the liquidus, solidus, and γ′ precipitation temperature of these γ/γ′-δ eutectic alloys. A comparison of the experimental results with thermodynamic calculations using the CompuTherm Pandat database (CompuTherm LLC, Madison, WI) showed qualitative agreement.     

Effects of carbon content and ausaging on γ ↔ α′ transformation behavior and reverse-transformed structure in Fe-Ni-Co-Al-C alloys

The effects of carbon content and ausaging on austenite γ ↔ martensite (α′) transformation behavior and reverse-transformed structure were investigated in Fe-32Ni-12Co-4Al and Fe-(26,28)Ni-12Co-4Al-0.4C (wt pct) alloys. TheM _s temperature, the hardness of γ phase, and the tetragonality of α′ increase with increasing ausaging time, and these values are higher in the carbon-bearing alloys in most cases. The γ → α′ transformation behavior is similar to that of thermoelastic martensite; that is, the width of α′ plate increases with decreasing temperature in all alloys. The αt’ → γ reverse transformation temperature is lower in the carbon-bearing alloys, which means that the shape memory effect is improved by the addition of carbon. The maximum shape recovery of 84 pct is obtained in Fe-28Ni-12Co-4Al-0.4C alloy when the ausaged specimen is deformed at theM _s temperature and heated to 1120 K. There are two types of reverse-transformed austenites in the carbon-bearing alloy. One type is the reversed y containing many dislocations which were formed when the γ/α′ interface moved reversibly. The plane on which dislocations lie is (01 l)_γ if the twin plane is (112)_α′. The other type of reverse-transformed austenite exhibits γ islands nucleated within the α′ plates.     

Martensitic transformations induced by plastic deformation in the Fe-Ni-Cr-C system

Martensitic transformations induced by plastic deformation are studied comparatively in various alloys of three types: Fe-30 pct Ni, Fe-20 pct Ni-7 pct Cr, and Fe-16 pet Cr-13 pct Ni, with carbon content up to 0.3 pct. For all these alloys the tensile properties vary rapidly with temperature, but there are large differences in the value of the temperature rangeM _s toM _d, which strongly increases with substitution of chromium for nickel or with carbon addition. Using the node method, it is found that the intrinsic stacking fault energy in the austenite drastically increases with temperature in all the chromium-bearing alloys investigated. This variation is consistent with the observed influence of temperature on the appearance of twinning or ε martensite during plastic deformation. Very different α’ martensite morphologies can result from spontaneous and plastic deformation induced transformations, especially in Fe-20 pct Ni-7 pct Cr-type alloys where platelike and lath martensites are respectively observed. As in the case of ε martensite, the nucleation process is analyzed as a deformation mode of the material, using a dislocation model. It is then possible to account for the morphology of plastic deformation induced α’ martensite in both Fe-20 pct Ni-7 pct Cr and Fe-16 pct Cr-13 pct Ni types alloys and for the largeM _s toM _d range in these alloys. This paper is based upon a thesis submitted by F. LECROISEY in partial fulfillment of the degree of Doctor of Philosophy at the University of Nancy.     

Observations of aging effects in a Cu-Sn shape memory alloy

A Cu-15.0 at. pct Sn alloy has been chosen as a model alloy for the study of aging effects in copper-based shape memory alloys. Different thermal aging treatments were carried out to determine the effects of both parent phase and martensite aging on the amount of shape recovery and the characteristic transformation temperaturesM _s ,A _s , andA _f . Aging of the martensite reduces both the amount of shape recovery and the extent of the reverse martensite → parent transformation. High martensite heating rates promote complete shape recovery and reverse transformation while the aging occurring during slow heating can inhibit or prohibit both. But irrespective of the martensite heating rate the transformation temperature hysteresis as given by (M _s -A _s ) is large for the Cu-15 pct Sn alloy compared to other shape memory alloys exhibiting thermoelastic behavior. On the other hand, some beneficial effects were noted when the Cu-15 pct Sn alloy was aged in the parent phase condition prior to subsequent transformation to martensite. TheM _s ,A _s , andA _f were lowered following prior parent phase aging, possibly because of a change in long range order, but prior parent phase aging was found to diminish the deleterious effect of martensite aging. Both shape recovery and the extent of the reverse martensite → parent transformation are enhanced by prior parent phase aging. The enhancement is greater the higher the aging temperature or the longer the aging time at a given temperature. J. D. STICE, formerly Research Assistant at the University of Illinois     

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.     

Alloy design of FeMnSiCrNi shape-memory alloys related to stacking-fault energy

The stacking-fault energy (γ _sf ) of iron-based shape-memory alloys was calculated by the extended dislocation-node method. The results show that Ni and Mn increase the γ _sf of the alloys with an austenite structure, while Cr and Si decrease it. An expression relating the alloying elements of Ni, Cr, Mn, and Si to the γ _sf of the alloys is established. Moreover, in terms of the γ _sf values of the alloys and the Schaeffler diagram, the alloy design of iron-based shape-memory alloys is carried out. It is found that the alloy having the lowest γ _sf has the best shape-memory effect (SME), with a martensite transition temperature (M _s ) being a little lower than ambient temperature. The corresponding composition of the alloy is located in the γ-phase zone near the phase line between the γ and γ+ε phase zone and the triple point of α+γ+ε in the Schaeffler diagram.     

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.     

Effect of cooling after welding on microstructure and mechanical properties of 12 Pct Cr steel weld metals

The microstructure of three 12 pct cr steel weld metals with different nickel and nitrogen contents was studied in as-welded condition and after postweld heat treatment with and without intercooling. Tensile strength and impact toughness of the weld metals were investigated in different postweld heat treatment conditions. In weld metals heat treated without intercooling, austenite decomposed by a eutectoid reaction that resulted in M₂₃C₆ aggregates around retained δ-ferrite. Two morphologies of M₂N and MN precipitates were found in a low-dislocation α-ferrite. It was concluded that these phases were also transformed from austenite. In weld metals heat treated with intercooling, M₂₃C₆ precipitates were smaller and more homogeneously distributed. Different MN precipitates were found in the tempered martensite. The fracture mode of the weld metals at room temperature was mainly transgranular cleavage with some fibrous fracture. Intercooling treatment improved Charpy impact toughness of the 12 pct Cr steel weld metals substantially. It was found that the important microstructural factors affecting the impact toughness of the weld metals which were heat treated without intercooling were the sizes of the α-ferrite grains, nonmetallic inclusions, and M₂₃C₆ aggregates. For the weld metals heat treated with intercooling, the factors which affect the toughness of the weld metals were the sizes of martensite packets and nonmetallic inclusions.     

Thermal transformations in mechanically alloyed Fe-Zn-Si materials

The ball milling of elemental powders corresponding to Γ (Fe₃Zn₁₀)+0.12 wt pct Si; Γ₁ (Fe₅Zn₂₁) + 0.12 wt pct Si; δ (FeZn₇)+0.12 wt pct Si; and ζ (FeZn₁₃)+0.12 wt pct Si composition ratios yields crystalline, mechanically alloyed phases. Differential scanning calorimetry (DSC) measurements of these materials show that they evolve differently, with well-defined characteristic stages. The activation energies for processes corresponding to these stages, based on kinetic analyses, are determined and correlated to microstructural evolvements. The processes occurring during the first stage below 250 °C, for all of the materials studied using X-ray diffraction (XRD) analysis, are associated with release of strain, recovery, and limited atomic diffusion. The activation energies for recovery processes are 120 kJ/mole for the Γ+0.12 wt pct Si, 131 kJ/mole for δ+0.12 wt pct Si, and 96 kJ/mole for ζ+0.12 wt pct Si alloys. At higher temperatures, recrystallization and other structural transformations occur with activation energies of 130 and 278 kJ/mole for Γ+0.12 wt % Si; of 161 kJ/mole for Γ₁+0.12 wt pct Si; of 167 and 244 kJ/mole for δ+0.12 wt pct Si; and of 641 kJ/mole for the ζ+0.12 wt pct Si. In addition, a eutectic reaction at 420 °C±3 °C, corresponding to the Zn-Si system, and a melting of Zn in Fe-Zn systems are observed for the ζ+0.12 wt pct Si material. The relation of FeSi formation in the Sandelin process is discussed.