Simultaneous creep and oxidation of an Fe-1 wt pct Ai alloy at 973 to 1073 K

Studies of the simultaneous creep and oxidation of an Fe-lwt pct Al alloy at constant stresses of 16 to 26 MN/m² in the temperature range 973 to 1073 K have shown that the steady state creep obeys a power law. The stress exponentn was found to be 6.9 for creep in an argon atmosphere (Po₂ = 10^?3 mbar). Values of the apparent activation energy for creep were in the range 225 to 351 kJ/mol and appeared to be dependent on the P_{0 2} of the test environment. Oxidationstrengthening (?e decreasing) occurred at 998 K but only at P_{0 2} = 10^?3 mbar and was primarily due to intergranular oxidation and the mechanical constraint of a strongly adherent scale. Oxidationweakening (?e increasing), however, occurred at 973 to 1073 K in environments of the lowest P_{0 2} (10^?9 and 10^?5 mbar) and in the highest P_{0 2} (162 to 1013 mbar). The factors contributing to weakening are believed to be oxidation-induced vacancies, weakly adherent scales and the loss of solute strengthening aluminum through selective oxidation.     

Microstructural investigation of the oxidation of an Fe-3 pct Cr alloy

The microstructure and microchemistry of the oxide scale on an Fe-3 wt pct Cr alloy have been investigated after oxidation in the temperature range 700 to 800 °C. Transmission and scanning electron microscopy along with energy dispersive X-ray analysis and Auger electron spectroscopy techniques were used for the investigation. Multilayered scales are observed which vary in composition and structure; the innermost oxide is an Fe-Cr spinel of the type Fe(Fe_2•xCr_x)O₄. The intermediate layer and the outer oxide layer are both α-Fe₂O₃ hematite. The outer hematite layer is nonadherent and wrinkling is observed. Spallation occurs readily at the inner hematiteJspinel interface and at the spinel oxideJalloy interface. The poor oxidation resistance of the alloy is discussed in terms of these observations.     

The kinetics of the internal nitriding of Fe-2 at. pct Al alloy

The kinetics of the precipitation of aluminum nitride on internal nitriding the Fe-2 at. pct Al alloy was investigated for cold-rolled and recrystallized specimens exhibiting “ideally weak” interaction behavior of the solutes Al and N. The kinetic analysis was performed using mass-increase data obtained for thin foils (thickness ⪯0.1 mm) upon nitriding in a NH₃/H₂ gas mixture at temperatures in the range 803 to 853 K. Activation-energy analysis revealed that precipitation of AlN in the recrystallized specimens is associated with a Gibbs free energy barrier for the formation of a precipitate of critical size; the precipitation rate is controlled by both nucleation and growth. On the other hand, precipitation of AlN in the cold-rolled specimens occurs without a Gibbs free energy barrier for formation of a precipitate of critical size; the precipitation rate is controlled by growth with kinetics governed by volume diffusion of alu-minum. Analysis of the total Gibbs free energy of formation of AlN in the α-Fe matrix showed that in the case of the recrystallized specimens, the formation of incoherent AlN precipitates with a hexagonal crystal structure is favored. In the case of the cold-rolled specimens, containing a high dislocation density, the formation of coherent AlN precipitates with cubic crystal structure is favored, at least in the beginning of precipitation.     

Influence of the precipitate-free zone width on the tensile properties of an Al-6 Wt pct Zn-1.2 Wt pct Mg alloy

The mechanical properties of an Al-6 wt pct Zn-1.2 wt pct Mg alloy with various width of precipitate-free zones have been investigated. The width of the precipitate-free zone (PFZ) has been changed by the quench interruption technique without any appreciable change in the size and distribution of precipitates. An important relationship has been observed between the width of the PFZ and the quench-interruption period;i.e., the width of the PFZ increases in proportion to the square root of the holding time at 200°C. From the analysis of stress-strain curves as well as the observation of dislocation arrangements in slightly deformed specimens, the plastic deformation has been found to occur preferentially in the PFZ. The initial stage of deformation is much affected by the change in the width of the PFZ, but in the later stage, the work-hardening rate seems to be almost independent of the PFZ width. Tensile tests show that the ultimate tensile strength and the 0.2 pct proof stress decrease very little with increasing width of the PFZ, while the uniform elongation is practically constant regardless of the reduction in the nonuniform elongation. The work-hardening rate at the initial stage of deformation is found to decrease in proportion to the reciprocal of the PFZ width. This relationship can be explained from the dislocation model for work hardening.     

The stress-dependence of high temperature creep of tungsten and a tungsten-2 Wt pct ThO2alloy

Constant-load creep tests were conducted with pure tungsten and a W-2 wt pct ThO₂ alloy at temperatures between 1600° and 2200°C and at strain rates of about 1 × 10^-8 to 4 × 10^-5 sec^-1. The results were evaluated by the empirical correlations of Robinson and Sherby and also Mukherjeeet al. which describe the stress dependence of the creep of metals and alloys. The agreement of the present experimental data with these correlations was found to be poor. However, when the following empirical relationship was used: •ε _c =A’(σ _c /σ _f ) ⁿ the present creep data for tungsten and the tungsten alloy at various temperatures were much better correlated. Here, •ε _c is the experimental creep rate, σ_c is the applied stress for creep, σf is the flow stress of the material at the same temperature in a constant strain rate tensile test, andA’ is function of temperature, structure, and strain rate.     

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     

The tempering of martensite in an Fe-1.5 pct N alloy

The tempering of Fe 1.5 pct N martensite has been studied at temperatures up to 300°C using X-ray and electron microscope techniques. Stage 1 decomposition occurs below 270°C by the general precipitation, resembling spinodal morphology, of fine τa^" (Fe₁₆ N₂) lamellae on 001 habit planes in both matrix and twin crystals of the partially 112 twinned martensite plates. Yet, gaged by changes in the X-ray spectrum, the reaction is discontinuous, the tetragonal martensite doublets decaying in intensity without change in their Bragg positions. The anomaly and the failure to detect by electron microscopy regions exhibiting fractional stages of the fine scale α^’ → α + α^" reaction is attributed to its occurrence at different times in different martensite (or parts of martensite) plates. It is believed that transformation occurs in this manner because the nucleation of coherent α^" plates is controlled by the prevailing internal stress field. Thus the time exponent “n” for the reaction decays from a normal value between 1 and 0.67 to less than 0.3 as stress relief by recovery dominates the more protracted stages of the reaction. Above 200°C the more stable nitride γ^’ (Fe₄N) forms at an increasing rate as plates on 012 habit planes, accompanied by marked softening.     

Molybdenum accumulation at ferrite: Austenite interfaces during isothermal transformation of an Fe-0.24 pct C-0.93 pct Mo alloy

A scanning transmission electron microscope (STEM) technique was used to measure Mo concentrations at ferrite:austenite (α:γ) interfaces in an Fe-0.24 pct C-0.93 pct Mo alloy partially transformed at 650°C, 630°C, and 610°C. These concentrations were quite small at 650°C, which is just below the bay temperature of the time-temperature-transformation (TTT) curve for the initiation of ferrite formation. There were larger concentrations at 630°C, a temperature at which transformation stasis (incomplete transformation) occurred. Concentrations at 610°C were intermediate between the values observed at 650°C and 630°C. The average accumulation at the latter temperatures increased appreciably as a function of transformation time. After each heat treatment, there was considerable variation in Mo accumulation from one α:γ interface to another and, to a lesser extent, from one region to another along the same interface. These higher Mo concentrations were deduced to have developed largely through volume diffusion of Mo, mainly through ferrite, to interfaces whose ledgewise growth had been interrupted by growth stasis. (Mo₂C precipitation at α:γ boundaries occurred only at the end of growth stasis.) It appears that only a very small amount of Mo segregation is needed, probably at specific interfacial sites, in order to produce growth cessation. Growth kinetics anomalies of this kind continue to provide the best evidence available for the operation of a coupled-solute drag effect. This article is based on a presentation given in the symposium “The Effect of Alloying Elements on the Gamma to Alpha Transformation in Steels,” October 6, 2002, at the TMS Fall Meeting in Columbus, Ohio, under the auspices of the McMaster Centre for Steel Research and the ASM-TMS Phase Transformations Committee.     

Elevated temperature deformation behavior of an Al-8.4 wt pct Fe-3.6 wt pct Ce alloy

The elevated temperature deformation characteristics of a rapidly solidified Al-8.4 wt pct Fe-3.6 wt pct Ce alloy have been investigated. Constant true strain rate compression tests were performed between 523 and 823 K at strain rates ranging from 10⁻⁶ to 10⁻³ s⁻¹. At temperatures below approximately 723 K, the alloy is significantly stronger than oxide dispersion strengthened (ODS) aluminum. However, at higher temperatures, the strength of the Al-Fe-Ce alloy falls rapidly with increasing temperature while ODS aluminum exhibits an apparent threshold stress. It is shown that particle coarsening cannot fully account for the reduction in strength of the Al-Fe-Ce alloy at elevated temperatures. The true activation energy for deformation of the Al-Fe-Ce alloy at temperatures between 723 and 773 K is significantly greater than that for self-diffusion in the matrix. This is unlike the behavior of ODS alloys, which contain nondeformable particles and exhibit true activation energies close to that for self-diffusion in the matrix. Since abnormally high true activation energies for deformation are also exhibited by materials containing deformable particles, such as γ^′ strengthened superalloys, it is concluded that elevated temperature deformation in ythe Al-Fe-Ce alloy involves deformation of both the matrix and the precipitates. The loss of strength of the Al-Fe-Ce alloy appears to be related to a reduction in strength of at least some of the second phase particles at temperatures above 723 K. Formerly Research Assistant, Department of Materials Science and Engineering, Stanford University.     

Partition of Mn during the growth of proeutectoid ferrite allotriomorphs in an Fe-1.6 at. pct C-2.8 at. pct Mn alloy

A STEM analysis is made of the Mn distribution around grain boundary allotriomorphs of proeutectoid ferrite in an Fe-1.6 at. Pct C-2.8 at. Pct Mn alloy. Whereas the Mn enriched region is readily observed to extend along the austenite grain boundary, no substantial build-up or depletion of Mn near the ferrite : austenite interface is detected, consistent with the electron probe microanalysis previously reported. In the temperature range where the partition-local equilibrium (P-LE) mode has been proposed to prevail, measured parabolic growth rate constantsfall 1 to 2 orders of magnitude above that predicted from this model, but also below that calculated from the paraequilibrium (PE) model by roughly the same amount. A modification of the theory of grain boundary diffusion-aided growth of precipitates,i.e., the collector/rejector plate mechanism, on the other hand, accounts fairly well for the observed growth kinetics of ferrite allotriomorphs. However, only a slightly better accounting than the P-LE model is provided by this mechanism for the temperature dependence of Mn partition. Data on Ni partition, obtained in an Fe-0.5 at. Pct C-3.1 at. Pct Ni alloy, are also analyzed with the rejector plate model.     

Effect of carbon content and helium gas environment on creep crack growth properties of Ni-26 pct Cr-17 pct W-0.5 pct Mo alloy at 1273 K

Creep crack growth tests were conducted on Ni-26 pct Cr-17 pct W-0.5 pct Mo alloys with different carbon contents in air and in helium gas environment at 1273 K using the compact-type (CT) specimen, and the effects of carbon content and environment on creep crack growth rate are discussed. Creep crack growth rateda/dt is evaluated by theC* parameter. Theda/dt is faster in higher-carbon alloys than in lower-carbon alloys in each environment. This effect of carbon content is attributed to the lower creep ductility due to the increase of fine trans-granular carbides in higher-carbon alloys. The environmental effect on theda/dt vs C* relations is scarcely observed in higher-carbon alloys. In the 0.003 pct C alloy, however,da/dt is much lower in the He gas environment than in air. Carburization is observed ahead of the crack tip in the He gas environment at 1273 K. The intergranular carbides precipitated due to carburi-zation have a granular configuration and are considered to prevent the grain boundary sliding in lower-carbon alloys.     

The microstructure of discontinuously precipitated lamellae in an austenitic Fe-42.4 Wt Pct Ni- 4.15 Wt Pct AI-0.45 Wt Pct C alloy

Phase decomposition of austenitic Fe-42.4 wt pct Ni-4.15 wt pct Al-0.45 wt pct C on aging at 823 K was investigated by means of electron microscopy, selected area diffraction and microdiffraction, and microprobe chemical analysis. During annealing, κ phase of L′l₂ structure fully coherent with the matrix formedvia the nucleation and growth mechanism. The matrix phase and cubic κ carbide were later gradually encroached upon by discontinuously precipitated lamellar phases. The duplex fine lamellae are composed of alternately arranged carbon-depleted Ll₂ phase and cementite. Between the two constituents in the lamellae, the Pitsch orientation relationship is fulfilled, and at the same time, the matrix phase of the grain which the discontinuously precipitated lamellar colony has left behind maintains the crystallographic cube-to-cube correspondence with the product Ll₂ phase.     

Reaction sintering of an Fe-6 Wt Pct B-48 Wt Pct Mo alloy in the presence of liquid phases

The mechanism of liquid phase sintering of an Fe-6 wt pct B-48 wt pct Mo alloy was investigated by means of thermal dilatometry, differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). A fine composite microstructure of Mo₂FeB₂ and ferrite was produced from powders of Fe, Mo, and FeB by a reaction sintering process involving two liquid phases. The hard phase Mo₂FeB₂ is produced in the compact prior to liquid formation initially by the reaction 2Mo+2FeB=Mo₂FeB₂+Fe and later by the reaction 2Mo+2Fe₂B=Mo₂FeB₂+ 3Fe. Above 1365K, considerable densification results from the initial stage rearrangement of the solid phases (austenite and Mo₂FeB₂) coexisting with the first formed liquid phase (L₁). Another liquid (L₂) which forms above 1415K, where Mo₂FeB₂ is the only coexisting solid phase, is required for complete densification. L₂, having a high solubility for Mo₂FeB₂, provides for solution/reprecipitation processes which characterize the intermediate stage of liquid phase sintering. The effective separation of the initial and intermediate stages by L₁ and L₂ is considered essential for the control of the sintered microstructure of the ternary alloy. Teiichi Ando, formerly with the Technical Research Laboratory, Toyo Kohan Co., Ltd., is with the Department of Materials Science and Engineering, Massachusetts Institute of Technology, Cambridge, MA 02139.     

The compressive creep behavior of a Pu-1 wt pct Ga δ-stabilized alloy at elevated temperatures

Constant stress compression creep tests were performed in vacuum on a high-purity Pu-1 wt pct Ga ö-stabilized alloy over the temperature range from 252° to 382°C for stresses from 700 to 2500 psi. Although the primary creep behavior could not be correlated by established techniques, the creep rates developed after true creep strains of about 0.15 provided good agreement with the temperature and stress dependence of creep for pure metals and dilute alloys. A power stress law for steady-state creep of the alloy was found forδ/E values less than 5 x 10′4, with the stress exponent being 4.0, and it was concluded that the alloy exhibits Class I solid solution behavior. For higher stress, exponential stress dependence was observed. The true activation energy for creep was found to be 38,900 cal per mole which is in good agreement with the value for self-diffus ion of plutonium in the ô-stabilized alloy. The primary creep behavior could be divided into three types: 1) at low strain rates, the creep rate gradually increases to a nearly steady-state; 2) at intermediate strain rates, the creep rate first decreases and then increases to steady-state; and 3) at high strain rates, the creep rate decreases gradually to steady-state. It was concluded that the failure of established creep correlations for primary creep of Pu-1 wt pct Ga was the result of some temperature-dependent component of creep structure, possibly resulting from radiation damage byα particles.     

Effect of Mg and Sr additions on the formation of intermetallics in Al-6 Wt pct Si-3.5 Wt pct Cu-(0.45) to (0.8) Wt pct Fe 319-type alloys

Al-Si alloys are materials that have been developed over the years to meet the increasing demands of the automotive industry for smaller, lighter-weight, high-performance components. An important alloy in this respect is the 319 alloy, wherein silicon and copper are the main alloying elements, and magnesium is often added in automotive versions of the alloy for strengthening purposes. The mechanical properties are also ameliorated by modifying the eutectic silicon structure (strontium being commonly employed) and by reducing the harmful effect of the β-Al₅FeSi iron intermetallic present in the cast structure. Magnesium is also found to refine the silicon structure. The present study was undertaken to investigate the individual and combined roles of Mg and Sr on the morphologies of Si, Mg₂Si, and the iron and copper intermetallics likely to form during the solidification of 319-type alloys at very slow (close to equilibrium) cooling rates. The results show that magnesium leads to the precipitation of Al₈Mg₃FeSi₆, Mg₂Si, and Al₅Mg₈Cu₂Si₆ intermetallics. With a strontium addition, dissolution of a large proportion of the needle-like β-Al₅FeSi intermetallic in the aluminum matrix takes place; no transformation of this phase into any other intermetallics (including the Al₁₅(Fe,Mn)₃Si₂ phase) is observed. When both Mg and Sr are added, the diminution of the β-Al₅FeSi phase is enhanced, through both its dissolution in the aluminum matrix as well as its transformation into Al₈Mg₃FeSi₆. The reactions and phases obtained have been analyzed using thermal analysis, optical microscopy, image analysis, and electron microprobe analysis (EMPA) coupled with energydispersive X-ray (EDX) analysis.     

Molybdenum-Nitride Precipitation in Recrystallized and Cold-Rolled Fe-1 at. pct Mo Alloy

Nitriding of recrystallized and cold-rolled Fe-1 at. pct Mo alloy at 853 K (580 °C) in a NH₃/H₂ gas mixture leads to the formation of cubic nanometer-sized Mo₂N-type precipitate platelets. These platelets obey a Baker–Nutting orientation relationship with the ferrite matrix. After prolonged nitriding, micrometer-sized colonies of lamellae consisting of a hexagonal MoN-type nitride and ferrite develop in a discontinuous precipitation reaction. These nitride lamellae have a Burgers-type orientation relationship with the ferrite lamellae. As compared to the recrystallized specimens, in the cold-rolled specimens, the precipitation of the initial Mo₂N-type platelets occurs much faster and moreover leads to incoherently diffracting precipitates; upon continued nitriding, a much earlier but only partially occurring transition of Mo₂N-type to MoN-type precipitates is observed. The results indicate that incorporation of iron in the nitrides can occur, if at all, only up till a negligible level, thereby invalidating earlier data.