On the improvement of creep strength and ductility of Ni-20 pct Cr by small zirconium additions

The creep and fracture properties of high-purity Ni-20 pct Cr and Ni-20 pct Cr-0.11 pct Zr alloys are compared at 1073 K in vacuum. The Ni-20 pct Cr alloy cavitates at the grain boundaries and fractures intergranularly after strains of typically 20 pct. The observed cavity growth rates are in keeping with those predicted. Alloying with zirconium substantially increases the creep strength and ductility. Creep rupture associated with dynamic recrystallization occurs, and voids are observed only in heavily necked parts of the samples. In addition to Ni₅Zr and ZrO₂ inclusions, a Zr₄C₂S₂ carbo-sulfide was identified. Thus, the sulfur-gettering effect of zirconium even at very low residual sulfur levels (20 wt ppm) was confirmed. The zirconium-induced increase in the creep strength is discussed, and the inhibition of creep cavitation by zirconium is examined within the framework of thermal cavity nucleation. Lowering of the grain boundary diffusivity and the grain boundary free energy as well as dynamic recrystallization are likely to reduce cavity nucleation and growth rates in Ni-Cr-Zr and will thus increase its ductility. Finally, the results are used to illustrate the critical importance of minor alloying additions in constructing and using fracture mechanism maps.     

Segregation of molybdenum atoms to the liquid-solid interfaces in liquid phase sintering of W-8 pct Mo-7 pct Ni-3 pct Fe

Partitioning of elements during sintering of W-8 pct Mo-7 pct Ni-3 pct Fe alloy was investigated with respect to various isothermal holding times, ranging from 5 to 240 minutes, at a sintering temperature of 1500 °C. It was found that the precipitation of W and Mo atoms from the liquid phase onto the W-Mo grains was competitive in nature, with W atoms showing a greater tendency to precipitate. Due to this fact, Mo atoms gradually segregated to the interface between W-Mo grains and the liquid phase. The accumulation of Mo atoms near the interfaces thus changed the interfacial properties and, consequently, reduced the rate of interfacial reaction (solution and precipitation), which was responsible for the transition of the controlling mechanism of grain growth from diffusion of W atoms in the liquid phase to the interfacial reaction.     

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.     

Formability of low-interstitial 18 pct Cr-2 pct Mo ferritic stainless steel

Because of its excellent corrosion resistance, low-interstitial 18 pct Cr-2 pct Mo ferritic stainless steel is being considered for a wide range of applications, many of which involve the forming of sheet. The present investigation was undertaken to examine the effects of rolling schedule on the formability of titanium-stabilized 18 pct Cr-2 pct Mo ferritic stainless steel sheet. Formability and texture development were evaluated by utilizing 1) plastic strain ratios and work-hardening exponents derived from tensile tests; 2) Swift and Olsen cup tests; and 3) X-ray pole figure analysis. Increasing the degree of cold reduction from 70 pct to 92 pct prior to the final recrystallization anneal led to substantial increases in deep drawability through changes in the recrystallization texture. Schedules of two-step cold rolling with an intervening recrystallization anneal, leading to increased total cold reduction, produced significantly higher plastic strain ratios than those produced by the one-step schedules. The crystallographic textures of the sheets were determined and correlated with the observedr values. This paper is based on a presentation made at a symposium on “New Developments in Ferritic and Duplex Stainless Steels,” held at the Fall Meeting in Cleveland, Ohio, on October 19, 1972, under the sponsorship of the Corrosion Resistant Metals Committee on TMS-IMD and the Corrosion and Oxidation Activity of the ASM.     

The effects of stress level and grain size on the ambient temperature creep deformation behavior of an alpha Ti-1.6 wt pct V alloy

Ambient (room) temperature studies have been carried out on an α-Ti-1.6 wt pct V alloy to determine the effects of stress level and grain size on ambient temperature creep behavior. Creep tests were performed at five different stress levels ranging from 75 to 95 pct of the yield stress value on specimens with an average grain size of 226 μm. It has been found that the alloy exhibits appreciable creep at stress levels far below the yield stress, with creep occurring at values as low as 75 pct of the yield stress. The extent of creep strain was found to decrease with a decrease in stress level. Creep tests were also performed on this alloy with different grain sizes ranging from 38 to 226 μm at a stress level of 90 pct of the yield stress. It was seen that the extent of creep strain decreased with a decrease in grain size. Fine slip and time-dependent twinning were found to be the creep deformation mechanisms. Based on the results of this investigation and earlier studies, it is suggested that time-dependent twinning is a major creep deformation mechanism in α-titanium alloys that contain small amounts of alloying elements. The time-dependent twinning phenomenon has been attributed to the diffusion of oxygen away from the twin-matrix interface, permitting the growth of twins.     

Origin of Significant Grain Refinement in Co-Cr-Mo Alloys Without Severe Plastic Deformation

We have previously reported that ultrafine-grained (UFG) microstructures can be obtained in a Co-29Cr-6Mo (wt pct) alloy by utilizing dynamic recrystallization (DRX) that occurs during conventional hot deformation (Yamanaka et al.: Metall. Mater. Trans. A, 2009, vol. 40A, pp. 1980?94). The present study investigates the novel DRX mechanism of this alloy in detail. The microstructure evolution during hot deformation under relatively high Zener?CHollomon (Z) parameter conditions for which ultrafine grains can develop was systematically investigated by electron backscatter diffraction (EBSD) and transmission electron microscopy. This alloy exhibited a different flow stress behavior and microstructural development from conventional DRX mechanisms. The deformation microstructure contained a large number of stacking faults, which implies that planar dislocation slip is the primary deformation mechanism in the hot deformation of the Co-29Cr-6Mo alloy due to its abnormally low stacking fault energy (SFE) at elevated temperatures. Inhomogeneities in local strain distributions induced by planar slip will enhance grain subdivision by geometrically necessary (GN) dislocation boundaries. Deformation twinning may also contribute to grain refinement. The DRX mechanism operating in the Co-29Cr-6Mo alloy is discussed by considering the relationships between anomalous dislocation structures, flow stress behavior, texture development, and nucleation behavior.     

The thermal activation energy for fatigue of Fe- 1 pct Cr- 0.5 pct Mo

The temperature dependence of fatigue crack propagation is considered in an Fe-1 pct Cr-0.5 pct Mo alloy steel. This material was tested at temperatures between 425 and 550 °C, a frequency of 1 Hz, and anR-ratio of 0.1. It is shown that the effect of temperature can be explained in terms of a thermal activation energy for fatigue. The magnitude of this activation energy is a function of ΔK and varies from more than 150 kJ/mole at 15 MPa√m to 30 kJ/mole above 30 MPa√m. The magnitude of these activation energies supports the idea that oxidation, and not creep, is the rate-controlling time-dependent process for the test conditions studied.     

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 creep behavior of W-5 re

Polycrystalline W-5 wt pct Re was creep-tested in tension from 1500° to 1900°C at stresses from 2500 to 10,000 psi in a vacuum of 10^?8 torr. The steady-state strain rate was directly proportional to stress to the 5.5 power, and the apparent activation energy for creep was 104 kcal per mole. Dislocation substructure that developed during high-temperature deformation was studied by transmission electron microscopy. The total dislocation density was dependent on stress to the 2.1 power and was insensitive to temperature and strain. No subgrains were found in creep tested specimens. The rate-controlling deformation mechanism was ascribed to dislocation climb where the governing diffusion process was dislocation core diffusion. Comparison of creep data for tungsten, W-5 wt pct Re, and W-25 wt pct Re showed that W-5 wt pct Re alloy has significantly better creep properties than the other two materials.     

The microstructural development of Mg-9 pct Al-1 pct Zn alloy during injection molding

Ex-situ microstructural analysis was used in order to assess the high-temperature transformations of the Mg-9 pct Al-1 pct Zn alloy within the injection-molding system. In addition to as-cast ingot, chipped feedstock, and final products, the alloy samples at different stages of the process were investigated. It was revealed that the cold deformation during ingot chipping and recrystallization during initial stages of residency inside the barrel led to nucleation and growth of the equiaxed grain structure. Subsequent melting of the Al-rich phase followed by liquid-alloy wetting of α-Mg grain boundaries initiated the formation of the slurry with globular solid particles. The structural evolution of the semisolid alloy under the simultaneous influence of temperature gradient and injection-screw shear is considered, and the mechanisms involved are discussed. It is concluded that during processing of partially remelted alloy the temperature profile along the injection-molding barrel in combination with the feedstock structure are key factors that control both the transformation of the thixotropic slurry and the final morphology of the primary solid phase.     

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.     

Microstructure-property relationships of two AI-3Li-2Cu-0.2Zr-XCd alloys

The microstructure and tensile properties of two A1-3 wt pct Li-2 wt pct Cu-0.2 wt pct Zr alloys, one Cd-free and one containing 0.2 wt pct Cd, have been investigated. The Cd-free alloy remained unrecrystallized for all solutionizing treatments studied, whereas a special treatment had to be developed to prevent recrystallization during solutionizing of the 0.2 wt pct Cd alloy. In combination with cadmium, zirconium either enters into, or nucleates on, the course Al₇Cu₂Fe and T₂ phases during high temperature annealing. This reduces the volume fraction of small coherent Al₃Zr particles in the matrix which normally inhibits recrystallization. Consequently, a low temperature anneal to precipitate Al₃Zr is necessary prior to high temperature solutionizing in order to prevent recrystallization in the Cd-containing alloy. Unlike its effect in lower lithium, higher copper content aluminum alloys, cadmium does not significantly affect the nucleation of the strengthening precipitates. If anything, cadmium has a detrimental effect on the age hardening response of this alloy, since it increases the formation of coarse Al-Cu-Li equilibrium phases at grain and subgrain boundaries and thus removes some of the copper and lithium from participating in the formation of the strengthening precipitates T₁ and δ′. Subgrain boundary fracture occurred during tensile tests of both alloys in the unrecrystallized condition; however, transgranular fracture occurred in tests of the partially recrystallized 0.2 wt pct Cd alloy. Both types of fractures are believed due to a form of strain localization associated with precipitate free zones and shearable precipitates. Formerly with the Fracture and Fatigue Research Laboratory, Georgia Institute of Technology, Atlanta, GA     

A castability model based on elemental solid-liquid partitioning in advanced nickel-base single-crystal superalloys

A castability model that accounts for the characteristic segregation behavior of constituent elements in Ni-base superalloys has been developed and experimentally verified in production scale casting trials. The model ranks alloy compositions with respect to their susceptibility to freckle formation during directional solidification. Thirty-nine distinct Ni-base single-crystal superalloys encompassing a broad range of compositions were investigated to assess the influence of the constituent elements on their solidification characteristics. Linear regression was applied to the fitted solid-liquid partition coefficients of the major constituent elements to develop formulas capable of describing elemental interactions. The high-density refractory elements Ta, W, and Re were found to segregate most severely during solidification. Increasing the amount of Cr and Mo in high-refractory single-crystal alloys reduced the extent of W and Re microsegregation during solidification. This effect was found to minimize the occurrence of freckle defects due to the corresponding decrease in the density inversion term, which is effectively the driving force for thermosolutal convective instabilities known to cause macroscopic grain defects during single-crystal solidification. Model predictions were validated using production scale casting trials where additions of 1.5 wt pct (1.9 at. pct) Cr and 3.0 wt pct (2.0 at. pct) Mo to a high-refractory superalloy more than halved the number of solidification-related grain defects formed. These findings suggest that elemental interactions between Cr, Mo, W, and Re need to be considered when optimizing alloys for high-temperature creep properties.     

Influence of molybdenum on the creep properties of nickel-base superalloy single crystals

The influence of Mo on the creep properties of single crystals of a model nickel-base superalloy has been investigated. The Mo content was systematically varied from 9.8 to 14.6 wt pet in an alloy series based on Ni-6 wt pet Al-6 wt pet Ta. The optimum initial γ-γ′ microstructure for raft development and creep strength was produced in each alloy prior to testing. The creep lives at 982 °C and 234 MPa exhibited a steep peak as a function of Mo content, with the maximum in life occurring at about 14.0 wt pet Mo. Deviations of less than 1 wt pet Mo from the optimum composition resulted in an order of magnitude drop in properties. As the Mo content was increased from 9.8 to 14.0 wt pct, the magnitude of lattice mismatch significantly increased, which was believed to be beneficial because of stronger γ-γ′ interfaces. As the Mo content was increased further from 14.0 to 14.6 w/o, the mechanical properties degraded because of the precipitation of a deleterious third phase. The results suggest that small variations in refractory metal content and initial gg′ size can have profound effects on mechanical properties. Hence, composition ranges and microstructures for the attainment of optimum mechanical properties may be somewhat limited and require close process control.     

Evolution of microstructure and tensile strength of rapidly solidified Al-4.7 pct Zn-2.5 pct Mg-0.25 pct Zr-X wt pct Mn alloys

Analytical transmission electron microscopy and thermal analysis of as-extruded Al-4.7 pct Zn-2.5 pct Mg-0.2 pct Zr-X wt pct Mn alloys, with Mn contents ranging from 0.5 to 2.5 wt pct, were carried out to elucidate the microstructural change and accompanying mechanical properties during subsequent heat treatments. The as-extruded alloy was fabricated from rapidly solidified powder and consisted of a fine, metastable manganese dispersoid and the ternary eutectic T phase (Al₂Mg₃Zn₃). Solution heat treatment resulted in the formation of the stable Al₆Mn phase and complete dissolution of the T phase. Formation of stable Al₆Mn was made by two routes: by phase transition from metastable Mn dispersoids which already existed, and from the supersaturated solid solution by homogeneous nucleation. The density of the Al₆Mn phase increased with the addition of manganese, while the shape and average size remained unchanged. A significant increase in the hardness was observed to coincide with the formation of the Al₆Mn phase. Similarly, the tensile strength increased further after the aging treatment, and the increment was constant over the content of Mn in the alloy, which was explained by the contribution from the same amount of precipitates, MgZn₂. Results of thermal analysis indicated that the dissolution of the T phase started near 180 °C and that formation of Al₆Mn occurred at about 400 °C, suggesting that further enhancement of strength is possible with the modification of the heat-treatment schedule.     

On the microstructure and mechanical behavior of melt-spun Fe-24 pct Ni-0.5 pct C Ribbons: Effect of austenite grain size

The role of carbon on the retention and decomposition of austenite in a melt-quenched Fe-24 wt pct Ni-0.5 wt pct C alloy made by the melt-spinning method has been investigated, using a combination of X-ray diffractometry, optical and TEM metallography, microhardness measurements, and tensile tests. It is found that the addition of 0.5 wt pct C to Fe-24 wt pct Ni alloy leads to retention of austenite to a temperature close to -196 °C, when the alloy is quenched from the melt. The austenite grain size varies from ∼0.2 μm to ∼2 μm on going from the wheel to the gas side. The cooling rate, accordingly, changes from 5 × 10⁷ to 4 × 10⁴ Ks^-1. The changes in the mechanical properties have been correlated with the accompanying changes in the ribbon microstructure. The Central Metallurgical Research and Development Institute, National Research Centre, Dokki, Cairo, Egypt     

Displacive transformations in Au-18 wt pct Cu-6 wt pct Al

A gold alloy with 18 wt pct Cu and 6 wt pct Al undergoes a reversible displacive phase transformation between an incompletely ordered L2₁ parent phase and a tetragonal product. The characteristics of these transformations were studied using acoustic emission, dilatometry, X-ray diffraction, and metallography. The morphology of the transformation products, the structure of the parent phase, and the generation of significant acoustic emission during the transformations indicate that they are at least quasi-martensitic, if not martensitic, and that this system is an example of a β-phase shape-memory alloy (SMA). The onset temperatures of the transformations depend on the prior thermal history of the sample. The martensite start (M _s ) temperature is between 30 °C and 20 °C. The system exhibits hysteresis and will revert to the parent phase when reheated, with an austenite start (A _s ) temperature between 55 °C and 80 °C. However, freshly cast or solution-annealed and quenched samples of the alloy do not transform to the tetragonal phase. Aging of such material at temperatures between 30 °C and 200 °C is required before they will manifest the displacive transformation. The “martensite” phase is considerably more resistant to aging-induced stabilization than that of most other SMAs.     

The low strain tensile behavior of U-7.5 wt pct Nb-2.5 wt pct Zr

The stress-strain response of polycrystalline, γ-quenched U-7.5 wt pct Nb-2.5 wt pct Zr alloy was studied as a function of strain rate and compared to equilibrium stress-strain tests performed by allowing the strain to reach a maximum value at incrementally increasing stresses. Equilibrium stress-strain tests were also performed on prestressed samples. Sheet tensile specimens were held at various states of strain in an X-ray diffractometer to determine crystal structural changes during deformation. Prestressed tensile bars were sectioned and examined metallographically and with the X-ray diffractometer. Two linear regions were observed in the equilibrium stress-strain tests: a low stress region with a slope of 5.3 to 5.5 x 10⁶ psi, and a region above 40,000 psi with a slope of 3.3 x 10⁶ psi. Finite strain rates tended to increase both slopes. The diffractometer experiments yielded plots of lattice parameter vs strain which showed a shift from a bcc structure of the γ^s phase, to a bct structure of the γ₀ phase between 1 and 3 pct deformation. It is postulated that this is a thermoelastic martensite transformation. A semiempirical equation was developed which describes the equilibrium stress-strain behavior of this alloy in terms of a stress induced phase transformation.     

X-ray diffraction and resistivity studies of titanium-molybdenum alloys

The phase transformation behavior of the metastable beta phase in hydrogen charged Ti-Mo alloys was investigated using electrical resistivity and X-ray diffraction techniques. Hydrogen charging was found to have little effect on athermal omega phase formation in a highly susceptible alloy (16 wt pct Mo) but suppressed athermal omega in alloys with compositions near the critical composition for the transition to diffuse (incommensurate) type omega (∼20 wt pct Mo). No evidence was found for a hydrogen induced omega phase in a concentrated alloy (30 wt pct Mo). The incipient stages of the beta + beta’ phase separation in Ti-30 wt pct Mo were detected after aging slightly below the beta transus.     

X-ray diffraction and resistivity studies of titanium-molybdenum alloys

The phase transformation behavior of the metastable beta phase in hydrogen charged Ti-Mo alloys was investigated using electrical resistivity and X-ray diffraction techniques. Hydrogen charging was found to have little effect on athermal omega phase formation in a highly susceptible alloy (16 wt pct Mo) but suppressed athermal omega in alloys with compositions near the critical composition for the transition to diffuse (incommensurate) type omega (∼20 wt pct Mo). No evidence was found for a hydrogen induced omega phase in a concentrated alloy (30 wt pct Mo). The incipient stages of the beta + beta’ phase separation in Ti-30 wt pct Mo were detected after aging slightly below the beta transus.