Strength of Initially Virgin Martensites at — 196 °C after Aging and Tempering

The compressive strength at —196°C of martensites in Fe-0.26 pct C-24 pct Ni, Fe-0.4 pct C-21 pct Ni, and Fe-0.4 pct C-18 pct Ni-3 pct Mo alloys, all with subzero M_s temperatures, has been determined in the virgin condition and after one hour at temperatures from —80 to +400 °C. The effects of ausforming (20 pct reduction in area of the austenite by swaging at room temperature prior to the martensitic transformation) were also investigated. For the unausformed martensites, aging at temperatures up to 0 °C results in relatively small increases in strength. Above 0 °C, the age hardening increment increases rapidly, reaching a maximum at 100 °C. Above 100 °C, the strength decreases continuously with increasing tempering temperature except for the molybdenum-containing alloy, which exhibits secondary hardening on tempering at 400 °C. For the ausformed martensites, the response to aging at subzero temperatures is greater than for unausformed material. Strength again passes through a maximum on aging at 100 °C. However, on tempering just above 100 °C, the ausformed materials show a slower rate of softening than the unausformed martensites. The strengthening produced by the ausforming treatment is largest for the Fe-0.4 pct C-18 pct Ni-3 pct Mo alloy, but there is no evidence of carbide precipitation in the deformed austenite to account for this effect of molybdenum. This paper is based on a presentation made at the “Peter G. Winchell Symposium on Tempering of Steel” held at the Louisville Meeting of The Metallurgical Society of AIME, October 12-13, 1981, under the sponsorship of the TMS-AIME Ferrous Metallurgy and Heat Treatment Committees.     

Strength of initially virgin martensites at - 196 °C after aging and tempering

The compressive strength at -196°C of martensites in Fe-0.26 pct C-24 pct Ni, Fe-0.4 pct C-21 pct Ni, and Fe-0.4 pct C-18 pct Ni-3 pct Mo alloys, all with subzero M temperatures, has been determined in the virgin condition and after one hour at temperatures from -80 to +400 °C. The effects of ausforming (20 pct reduction in area of the austenite by swaging at room temperature prior to the martensitic transformation) were also investigated. For the unausformed martensites, aging at temperatures up to 0 °C results in relatively small increases in strength. Above 0 °C, the age hardening increment increases rapidly, reaching a maximum at 100 °C. Above 100 °C, the strength decreases continuously with increasing tempering temperature except for the molybdenum-containing alloy, which exhibits secondary hardening on tempering at 400 °C. For the ausformed martensites, the response to aging at subzero temperatures is greater than for unausformed material. Strength again passes through a maximum on aging at 100 °C. However, on tempering just above 100 °C, the ausformed materials show a slower rate of softening than the unausformed martensites. The strengthening produced by the ausforming treatment is largest for the Fe-0.4 pct C-18 pct Ni-3 pct Mo alloy, but there is no evidence of carbide precipitation in the deformed austenite to a°Count for this effect of molybdenum.     

Investigation into the effect of substituting Mo by W on the behavior,during aging,of the maraging type ternary alloys

The substitution of W for Mo in the Fe-16.4 Ni-8.2 Mo alloys produces a dual component alloy: i) lath martensite containing 5 wt pet W and ii) 2 pct intermetallic phase, the composition of which is 33.3 Fe-4.4 Ni-62.3 W. The behavior of the two alloys Fe-16.4 Ni-8.2X (X)=Mo or W) is compared during heating (between 20 and 950°C) at a rate of 300°C/h. For both alloys, the martensite transforms into austenite in three successive steps by a predominantly diffusional mechanism. The behavior of the two alloys in similar during isothermal aging at temperatures less than or equal to 550°C. In fact, the aging process takes place in three successive stages which are studied using the small-angle X-ray scattering technique and electron microscopy.     

High Cycle Fatigue of (Fe,Ni, Co)3V type alloys

High cycle fatigue tests in vacuum have been performed on ordered (Fe, Co, Ni)₃V alloys between 25 °C and 850 °C. Heat-to-heat variations in fatigue properties of a Co-16.5 wtpct Fe-25 pct alloy, LRO-1, appeared to be due to differing quantities of grain boundary precipitates. Modification of this alloy with 0.4 pct Ti, to produce an alloy designated LRO-23, reduced the density of grain boundary precipitates and increased ductility, resulting in superior fatigue strength at high temperatures. The fatigue lives of LRO-1 and LRO-23 decreased rapidly above 650 °C, and increased intergranular failure was noted. The fatigue resistance of a cobalt-free alloy, Fe-29 pct Ni-22 pct V-0.4 pct Ti (LRO-37), was examined at 25 °C, 400 °C, and 600 °C; there was little evidence for intergranular fracture at any of these temperatures. Fatigue behavior of the LRO alloys is compared to that of conventional high temperature alloys.     

Investigation of the Effects of Ni, Fe, and Mn on the Formation of Complex Intermetallic Compounds in Al-Si-Cu-Mg-Ni Alloys

The aim of this work is to partially substitute Fe and Mn for Ni in the 3HA piston alloy and to study the consequences through microstructural evaluation and the thermal analysis technique. Three types of near-eutectic alloys containing (2.6 wt pct Ni-0.2 wt pct Fe-0.1 wt pct Mn), (1.8 wt pct Ni-0.75 wt pct Fe-0.3 wt pct Mn), and (1 wt pct Ni-1.15 wt pct Fe-0.6 wt pct Mn) were produced, and their solidification was studied at the cooling rate of 0.9 K/s (°C/s) using the computer-aided thermal analysis technique. Optical microscopy and scanning electron microscopy were used to study the microstructure of the samples, and energy dispersive X-ray (EDX) analysis was used to identify the composition of the phases. Also, the quantity of the phases was measured using the image analysis technique. The results show that Ni mainly participates as Al₃Ni, Al₉FeNi, and Al₃CuNi phases in the high Ni-containing alloy (2.6 wt pct Ni). In addition, substitution of Ni by Fe and Mn makes Al₉FeNi the only Ni-rich phase, and Al₁₂(Fe,Mn)₃Si₂ appears as an important Fe-rich intermetallic compound in the alloys with the higher Fe and Mn contents.     

The role of thermal stabilization in martensite transformations

The variation of the kinetics of the martensite transformation with carbon content and martensite habit plane has been investigated in several Fe−Ni based alloys. Transformation in an Fe-25 wt pct Ni-0.02 wt pct C alloy exhibits predominantly athermal features, but some apparently isothermal transformation also occurs. In a decarburized alloy, on the other hand, the observed kinetic features, such as the dependence ofM _s on cooling rate, were characteristic of an isothermal transformation. In contrast, Fe-29.6 wt pct Ni-10.7 wt pct Co alloys with carbon contents of 0.009 wt pct C and 0.003 wt pct C transform by burst kinetics to {259}_γ plate. At both these carbon levels, theM _b temperatures of the Fe−Ni−Co alloys are independent of cooling rate. It is proposed that the change in kinetic behavior of the Fe-25 pct Ni alloy with the different carbon contents is due to the occurrence of dynamic thermal stabilization in the higher carbon alloy. Dynamic thermal stabilization is relatively unimportant in the Fe−Ni−Co alloys which transform by burst kinetics to {259}_γ plate martensite. P. J. FISHER, formerly with the University of New South Wales D. J. H. CORDEROY, formerly with the University of New South Wales     

Structure-property relations in a metastable β Ti alloy containing Si

The hardness response, tensile behavior, and phase transformations occurring in a quenched and aged metastable β phase Ti-30 at. pct V-l at. pct Si alloy have been inves-tigated. Upon aging at 570°C, as-quenched samples show a broad hardness peak which is associated with the formation of rod-like, hexagonal (Ti,V)_xSi_y transition phase precipi-tates. The equilibrium silicide is observed upon aging at 570°C in the form of faceted, tetragonal particles. A loss of tensile ductility and a transition to intergranular fracture occurs after extended aging at 570°C and is related to Si segregation to the grain bound-aries. Comparing the behavior of Ti-30V to that of Ti-30V-lSi shows that the presence of Si strongly retards α-phase formation. However, a substantial age hardening re-sponse still occurs upon aging at 450°C, especially after prior cold work (the yield strength increases from 635 to 982 MPa). This hardening response is combined with a retention of a ductile, transgranular fracture even after extended aging at 450°C. Aging first at 570°C followed by aging at 450°C results in an increase in the volume fraction of α-phase formed but a subsequent decrease in ductility and hardness response upon aging at 450°C. These results are discussed in terms of the structure/property relationships which result from the influence of Si on the formation of, a) (Ti.V)_xSi_y precipitates, b) the equilibrium silicide, and c) the α-phase.     

Effect of carbon addition on the strength and creep resistance of FeAl alloys

We investigated the effect of carbon content (0.05, 0.12, and 0.2 wt pct C) and heat-treatment temperature (1100°C and 1300°C for 2 hours and air cooled) on the tensile and the creep properties of Fe-24 wt pct Al alloy. The increase of carbon content increased the yield strength without affecting the tensile ductility of the alloys. Carbon content appears to be beneficial in suppressing the hydrogen embrittlement at the grain boundary, because the fracture mode changes from predominantly intergranular failure in a low carbon (0.05 wt pct C) alloy to a predominantly transgranular cleavage failure in a high carbon (0.2 wt pct C) alloy. With the increase of carbon content, the anomalous yield strength peak shifted to a higher temperature possibly due to the interaction between carbon and vacanies. Significant improvements were noted in the tensile and the creep properties of medium (0.12 wt pct C) and high carbon (0.2 wt pct C) alloys after heat treating at 1300°C. The improvements in the tensile and the creep properties were attributed to the synergetic effect of retained vacancies and fine carbide precipitates present in the alloys after 1300°C heat treatment. However, the improved strength and creep properties associated with 1300 °C heat treatment were lost when the heat-treated alloys were further subjected to a vacancy removal annealing. Our results suggest that the retained vacancies present in the FeAl alloys after high-temperature heat treatment and air cooling are effective in improving the creep resistance at 700°C, and yield strength up to 800°C. The creep resistance of the present high carbon FeAl alloy is comparable to or better than several grades commercial heat-resistant Fe-based and Ni-based alloys. The work was carried out when the authors were with Chrysalis Technologies Inc., Richmond, VA. This article is based on a presentation made in the symposium entitled “Fundamentals of Structural Intermetallics,” presented at the 2002 TMS Annual Meeting, February 21–27, 2002, in Seattle, Washington, under the auspices of the ASM and TMS Joint Committee on Mechanical Behavior of Materials.     

Experiments on directional martensitic transformation in steel

This paper describes some preliminary experiments on the feasibility of producing steels with an aligned martensitic microstructure. The parent austenite is initially textured, following which the martensite habit plane “activity” is regulated by transforming under strain. An Fe-20 pct Ni-5 pct Mn alloy exhibiting a lowM _s temperature and a lath mar-tensite morphology was found suitable for producing aligned martensite. On heavy defor-mation this alloy developed a typical (123) [412] fcc texture. Subsequent annealing then produced a strong (001) [100] cube texture. Nearly 80 pct of the martensite formed was aligned when such a cube-textured specimen was strained 2.5 pet at 45 deg to the rolling direction followed by cooling under strain in liquid nitrogen to produce martensite. M. Khobaib and R. Quattrone, Formerly with the Construc-tion Engineering Research Laboratory, U.S. Army Corps of Engineers, Champaign, Illinois     

Aging and brittleness in an Fe-Ni-Mn alloy

A study of the aging behavior of an Fe-12 Ni-6 Mn alloy has been made. Rapid hardening was found to occur over a wide temperature range. Extraction of the overaged precipitate has been carried out and the precipitate identified as fct θ NiMn by electron diffraction. Studies of the effect of aging on the toughness and tensile ductility have shown that severe embrittlement occurs over a wide temperature range. The relationship between the hardening and the embrittlement was studied by comparison of “activation energies” determined from Arrhenius plots. It is suggested that embrittlement in this alloy is the result of segregation of manganese to prior austenite grain boundaries resulting in intergranular failure. To avoid embrittlement, aging was performed at temperatures above the embrittlement range which resulted in good toughness with moderate hardness. This paper is based upon a thesis submitted by D. R. SQUIRES in partial fulfillment for a higher degree of CNAA at Sheffield Polytechnic.     

Dynamic recrystallization during creep in a 45 Pct Ni-35 pct Fe-20 pct Cr alloy system

A combined 3.5 wt pct Mo + 1.2 wt pct Ti imparted dynamic recrystallization in a 35 wt pct Fe-45 wt pct Ni-20 wt pct Cr alloy system during creep at 700 °C, whereas 3.5 wt pct Mo addition alone did not initiate recrystallization. Dynamic recrystallization substantially increased the creep elongation and produced a high ductile fracture topography in the present alloy system. A subgrain coalescence nucleation mechanism for dynamic recrystallization mechanism was operative during creep. The critical initiation strain requirements are also discussed.     

Aging embrittlement and grain boundary

“Clean” 3.5NiCrMoV steels with limited contents in trace elements (P, Sn, As, Sb) are commonly provided for manufacturing big rotor shafts. The possible increase in temperature in future steam turbines has promoted the development of “superclean” steels characterized by an extra drastic decrease of manganese and silicon contents. Their higher cost in comparison to “clean” steels leads to concern above which temperature they must be considered as mandatory for resisting aging embrittlement in operation. 3.5NiCrMoV “clean” steel samples (Mn = 0.30 pct; Si = 0.10 pct) were aged at 300 °C, 350 °C, and 400 °C for 10,000 hours up to 30,000 hours. No embrittlement results from aging at 300 °C and 350 °C, but holding at 400 °C is highly detrimental. Auger spectroscopy confirms that, when aging at 400 °C, phosphorus is the main embrittling trace element. It is suggested that grain boundary embrittlement is associated with the building of a layer that contains, on the one hand, Ni and P and, on the other hand, Mo and Cr. Head of the Testing and Head of the Testing and Head of the Testing and     

A small-angle x-ray scattering investigation of the zone formation of “maraging” type alloys

The small angle X-ray scattering from “Maraging” type alloys previously aged at temperatures below 450°C has been studied at room temperature. The behavior, during aging, of two high purity alloys containing Fe Ni Co and Fe Ni Co Mo is compared with an industrial Vascomax 300 type steel. The existence of G.P. zones is pointed out for the two Mo containing alloys. In the case of the quaternary alloy, the evolution of these zones during the aging is clearly defined. For the industrial steel, the interpretation of the observed phenomena is more complex due to the additional small amounts of Ti, Cu, Al and is discussed.     

Effect of molybdenum on the fracture characteristic of high-speed steel quenched matrix

The fractures of three model alloys, imitating by their chemical composition the matrixes of the quenched high-speed steels of various Mo: W relations were analyzed. According to the measurements of the stress intensity factor K_Ic and the differences in the precipitation processes of carbides it was found out that the higher fracture toughness of the matrix of the molybdenum high-speed steels than on the tungsten ones is the results of the differences in the kinetics of precipitation from the martensite matrix of these steels during tempering. After tempering at 250 and 650°C the percentage of the intergranular fracture increases with the increase of the relation of Mo to W in the model alloys of the high-speed steel matrix. This is probably the result of higher precipitation rate of the M₃C carbide (at 250°C) and the MC and M₆C carbides (at 650°C) in the privileged regions along the grain boundaries. The change of the character of the model alloy fractures after tempering at 450°C from the completely transgranular one in the tungsten alloy to the nearly completely intergranular one in the molybdenum alloy indicates that the coherent precipitation processes responsible for the secondary hardness effect in the tungsten matrix begin at a lower temperature than in the molybdenum matrix. After tempering for the maximum secondary hardness the matrix fractures of the high-speed steels reveal a transgranular character regardless the relation of Mo to W. The higher fracture toughness of the Mo matrix can be the result of the start of the coherent precipitation processes at a higher temperature and their intensity which can, respectively, influence the size of these precipitations, their shape and the degree of dispersion. The transgranular character of the fractures of the S 6-5-2 type high-speed steel in the whole range tempering temperatures results from the presence of the undissolved carbides which while cracking in the region of stress concentration can constitute flaws of critical size which form the path of easy cracking through the grains. The transgranular cracking of the matrix of the real high-speed steels does not change the adventageous influence of molybdenum upon their fracture toughness. On the other hand, the carbides, undissolved during austenitizing, whose size distribution in the molybdenum steels from the point of view of cracking mechanics seems to be unsatisfactory, influence significantly the fracture toughness of these steels.     

Phase Evolution and Mechanical Properties of Nano-TiO2 Dispersed Zr-Based Alloys by Mechanical Alloying and Conventional Sintering

The present study deals with the synthesis of 1.0 to 2.0 wt pct nano-TiO₂ dispersed Zr-based alloy with nominal compositions 45.0Zr-30.0Fe-20.0Ni-5.0Mo (alloy A), 44.0Zr-30.0 Fe-20.0Ni-5.0Mo-1.0TiO₂ (alloy B), 44.0Zr-30.0Fe-20.0Ni-4.5Mo-1.5TiO₂ (alloy C), and 44.0Zr-30.0Fe-20.0Ni-4.0Mo-2.0TiO₂ (alloy D) by mechanical alloying and consolidation of the milled powders using 1 GPa uniaxial pressure for 5 minutes and conventional sintering at 1673 K (1400 °C). The microstructural and phase evolution during each stage of milling and the consolidated products were studied by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM), and energy-dispersive spectroscopy. The particle size of the milled powder was also analyzed at systemic intervals during milling, and it showed a rapid decrease in particle size in the initial hours of milling. XRD analysis showed a fine crystallite size of 10 to 20 nm after 20 hours of milling and was confirmed by TEM. The recrystallization behavior of the milled powder was studied by differential scanning calorimetry. The hardness of the sintered Zr-based alloys was recorded in the range of 5.1 to 7.0 GPa, which is much higher than that of similar alloys, developed via the melting casting route.     

Tensile flow and fracture behavior of

The tensile properties, fracture modes, and deformation mechanisms of two DO₃ alloys, Fe-25 and Fe-31 at. pct Al, have been investigated as a function of temperature up to 600 °C. The first alloy was produced by powder metallurgy and hot-extrusion, the second by casting and hot-extrusion. At room temperature extensive plastic deformation occurs in these intermetallics, exhibiting an elongation to fracture of 8 pct and 5.6 pct, respectively. In the Fe-25Al alloy the deformation process consisted of motion and extensive cross-slip of ordinary dislocations and associated formation of antiphase-boundary (APB) bands, while in the Fe-31Al alloy, plasticity occurred by the motion of superlattice dislocations which eventually dissociated to form APB bands. At room temperature both alloys exhibited transgranular cleavage fracture modes. The variation of tensile properties and fracture modes with temperature is presented. Formerly with the Materials Laboratory of the Air Force Wright Formerly with the Materials Laboratory of the Air Force Wright Formerly with the Materials Laboratory of the Air Force Wright     

Tensile flow and fracture behavior of DO3 Fe-25 at. pct Al and Fe-31 at. pct al alloys

The tensile properties, fracture modes, and deformation mechanisms of two DO₃ alloys, Fe-25 and Fe-31 at. pct Al, have been investigated as a function of temperature up to 600°C. The first alloy was produced by powder metallurgy and hot-extrusion, the second by casting and hot-extrusion. At room temperature extensive plastic deformation occurs in these intermetallics, exhibiting an elongation to fracture of 8 pct and 5.6 pct, respectively. In the Fe-25Al alloy the deformation process consisted of motion and extensive cross-slip of ordinary dislocations and associated formation of antiphase-boundary (APB) bands, while in the Fe-31 Al alloy, plasticity occurred by the motion of superlattice dislocations which eventually dissociated to form APB bands. At room temperature both alloys exhibited transgranular cleavage fracture modes. The variation of tensile properties and fracture modes with temperature is presented. H. A. LIPSITT, formerly with the Materials Laboratory of the Air Force Wright Aeronautical Laboratories, Wright-Patterson Air Force Base, OH 45433-6533     

On the stress exponent and the rate-controlling mechanism of high-temperature creep in some solid solutions

The internal stress, σ_i, and the effective-stress exponent of the dislocation velocity,m*, have been determined during creep of Fe-3.5 at. pct Mo alloy at 1123 K under 10.8 to 39.2 MN/m² and of Ni-10.3 at. pct W alloy at 1173 K under 19.6 to 88.2 MN/m². Both alloys have been classified among class I alloys under a certain condition including the present one, because the applied-stress exponent of the steady-state creep rates,n, is almost 3. Values of σ_i obtained by stress-transient dip test were small and almost independent of the applied stress, σ_c, in Fe-3.5 Mo alloy. On the other hand, in Ni-10.3 W alloy σ_i increased with increasing σ_c as in the case of many pure metals. The value ofm* obtained by analyzing stress-relaxation curves immediately after creep deformation was unity in Fe-3.5 Mo alloy, whereas in Ni-10.3 W alloy it was about 2.5. These results indicate that the rate-controlling mechanisms in creep are different from each other in these two alloys and that the classification according ton-value does not always coincide with the classification according to the rate-controlling mechanisms. It is concluded that the fact thatn ≃ 3 is not a sufficient evidence supporting that creep is controlled by one of microcreep mechanisms.     

The fracture toughness of a ferrous maraging alloy containing manganese

A Fe-20 pct Co-15 pct Mn-5 pct Mo maraging alloy has been found to exhibit low toughness and brittle fracture throughout its response to age-hardening. Intergranular embrittlement associated with segregation of manganese and with residual oxygen (15 to 300 ppm) in the early stages of aging was replaced by brittle inter-lath separation as aging progressed, the latter mode being associated with intermetallic precipitation and, possibly, the presence of finely-dispersed austenite. Formerly a Research Student in the Department of Metallurgy, University of Sheffield