The effect of high temperature plastic flow on the superconducting transition in A15 compounds

Low temperature heat capacity measurements have been made on hot isostatically pressed Nb₃Sn and arc cast, homogenized, and A15 transformation annealed V-23.3 at. pct Ga and V-18.1 at. pct Ga. The heat capacity measurements display the superconducting transition temperature (T _c), and have been used to evaluate the effects of plastic deformation on theT _c range. Plastic deformation to the extent of 15 pct compression at 1525 and 1650 °C does not alter the superconducting transition in polycrystalline Nb₃Sn. Plastic deformation to the extent of 15 pct compression at 1050 and 1200 °C does not alter the superconducting transition in polycrystalline V-23.3Ga, transformed to A15 structure with a fifty-hour 1150 °C anneal. The same statement can be made for A15 V-18.1Ga, deformed at 1050 °C after a fifty-hour, 1150 °C anneal. With onlyfive hours annealing at 1150 °C, A15 V-23.2Ga displays a lowering and broadening of theT _c range upon 1050 and 1200 °C plastic deformation. With onlyfive hours annealing at 1150 °C, A15 V-18.1Ga displays a broad, but increasedT _c range after plastic deformation at 1050 °C.     

The effect of grain size on the high temperature plastic deformation of nb3sn

A study of high temperature plastic deformation has been undertaken on 10, 20, and 60 μm grain size Nb₃Sn. The materials were produced by the hot isostatic pressing of powder blends. The 20 and 60 μm grain size material involved a stoichiometric blend of Nb and Sn powder, whereas the 10 μm grain size material involved a blend of 30.2 wt pct Sn powder and 69.8 wt pct Nb-1 Zr powder. The ZrO₂ formed during processing limits grain size and NbO formation. Through compression testing and load relaxation testing, deformation has been studied over a strain rate range from 10^-6 to 10^-2 per second and a temperature range from 1150 to 1650 °C. “Power law creep” was generally observed, although stress exponent reduction at the higher temperatures and lower strain rates suggests substructural coarsening. Analysis of stress-strain rate-temperature data projected an activation energy for creep of 400 to 500 kJ/mol. Grain size refinement clearly strengthened the polycrystals. Assuming a Hall-Petch relationship, “lattice friction stresses” and “unpinning constants” were calculated, both increasing with decreased temperature and increased strain rate. Grain size refinement from 60 to 10 μm lowered the ductile-to-brittle transition temperature for simple compression by the order of 125 °C.     

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.     

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

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

Constitutive properties of hard-alpha titanium

The flow and fracture behavior of hard-alpha Ti was studied as a function of nitrogen content, stress state, strain rate, and temperature. Hard-alpha Ti specimens with nitrogen contents ranging from 2 to 11.6 wt pct were fabricated by powder-metallurgy techniques. Stress-strain curves were obtained under various states of stress by performing uniaxial compression, indirection tension, indentation, and plane-strain compression tests at two strain rates. By varying the test technique and the specimen geometry, deformation and fracture in hard-alpha Ti was characterized for mean pressures as high as 6 times the flow stress. Most of these tests were conducted at 954 °C, but some were performed at 25 °C, 927 °C, and 982 °C. The experimental results indicated that, during compression testing at 927 °C to 982 °C, hard-alpha Ti exhibited substantial plastic deformation for nitrogen contents less than 4 wt pct, but showed brittle fracture with little plastic flow for nitrogen contents of 5.5 to 11.6 wt pct. Both the yield and fracture strengths increase with increasing nitrogen content and pressure, but decrease with increasing temperature. The yield strength increases with strain rate, while the fracture strength shows little or no rate sensitivity. The fracture strength in tension is substantially lower than that in compression. These observed deformation and fracture characteristics are explained on the basis of microcrack formation during inelastic deformation.     

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.     

Localized vs homogeneous deformation in Fe82B15Si3 amorphous alloy

Amorphous alloys are known to deform plastically either by a localized shear mode or in a homogeneous manner. Conditions that favor homogeneous deformation in an amorphous alloy consisting of 82Fe, 15B and 3Si in at. pct have been established by a free-bend test over a range of temperatures. These results are in turn related to the stress-strain rate-temperature relationship obtained by a load relaxation testing method. The intense, localized shear deformation is shown to occur at relatively high strain rate and low temperature regions where the rate sensitivity of flow stress,m, is small. With increasingm, plastic flow tends to take place homogeneously provided that the mode of deformation remains stable. The strain rate sensitivity of flow stress increases with decreasing strain rate and increasing temperature; the computed diffuse shear transformation zone also changes in the same manner. However, the general trend changes above the glass transition temperature, i.e., the diffuse shear transformation zone decreases and the flow strength increases with increasing temperature.     

Plastic deformation in polycrystalline Nb3Sn

A study of the high temperature plastic deformation of polycrystalline Nb₃Sn has been undertaken on hot isostatically pressed material having grain sizes in the 12 to 60 (μm range. Through compression testing and load-relaxation testing deformation has been studied over a strain rate range from 10⁻⁶to 10⁻²s and a temperature range from 1150 to 1650 °C. Plastic deformation can be observed in compression at 1400 °C and above and extensive deformation is possible at 1650°C. Except for the lowest strain rates at 1650 °C, load-relaxation stress-strain rate relationships are consistent with “power law creep”. Analysis of stress-strain rate-temperature relationships projects an activation energy for creep of very roughly 500 kJ/mol. Observations on yield point behavior and fracture mode transition are presented. A comparison to monocrystalline V₃Si behavior is made, and the role of the sub-structure during testing is considered.     

Ductility and strain-induced transformation in a high-strength transformation-induced plasticity-aided dual-phase steel

The influence of forming temperature and strain rate on the ductility and strain-induced transformation behavior of retained austenite in a ferritic 0.4C-1.5Si-1.5Mn (wt pct) dual-phase steel containing fine retained austenite islands of about 15 vol pct has been investigated. Ex- cellent combinations of total elongations (TELs), about 48 pct, and tensile strength (TS), about 1000 MPa, were obtained at temperatures between 100 °C and 200 °C and at a strain rate of 2.8 X 10_-4/s. Under these optimum forming conditions, the flow curves were characterized by intensive serrations and increased strain-hardening rate over a large strain range. The retained austenite islands were mechanically the most stable at temperatures between 100 °C and 200 °C, and the retained austenite stability appeared to be mainly controlled by strain-induced martensite and bainite transformations (SIMT and SIBT, respectively), with deformation twinning occur- ring in the retained austenite. The enhanced TEL and forming temperature dependence of TEL were primarily connected with both the strain-induced transformation behavior and retained aus- tenite stability.     

Effect of nitrogen content on the environmentally-assisted cracking susceptibility of duplex stainless steels

The effect of nitrogen content on the stress corrosion cracking (SCC) behavior of 22 pct Cr duplex stainless steel (DSS) in chloride solutions was investigated in this study. Slow strain rate testing (SSRT) was employed to evaluate the SCC susceptibility. The experimental results showed that the tensile strength and ductility of 22 pct Cr DSS increased with increasing amount of nitrogen (in the range of 0.103 to 0.195 wt pct). Slow strain rate testing results indicated that 22 pct Cr DSSs were resistant to SCC in 3.5 wt pct NaCl solution at 80 °C. However, environmentally assisted cracking occurred in 40 wt pct CaCl₂ solution at 100 °C and in boiling 45 wt pct MgCl₂ solution at 155 °C, respectively. The effects of environment and nitrogen content in DSS on the cracking susceptibility are discussed in this article. Selective dissolution of ferrite phase was found to participate in the SCC process for tests in CaCl₂ solution. At temperatures above 80 °C, dynamic strain aging was found to occur in various environments at a strain beyond plastic deformation.     

Creep behavior of an Al-2. 0 wt pct Li alloy in the temperature range 300 °C to 500 °C

The elevated temperature deformation behavior of an Al-2. 0 wt pct Li alloy in the temperature range 300 °C to 500 °C was studied using constant extension-rate tension testing and constant true-stress creep testing under both isothermal and temperature cycling conditions. Optical microscopy and transmission electron microscopy (TEM) were employed to assess the effect of deformation on microstructure. The data showed that the stress exponent,n, has a value of about 5. 0 at temperatures above theα +δAlLi solvus (approximately 380 °C) and that subgrains form during plastic deformation. Models for dislocation-climb and dislocation-glide control of creep were analyzed for alloys deformed in the temperature range of stability of the terminal AlLi solid solution. A climb model was shown to describe closely the behavior of this material. Anomalous temperature dependence of the activation energy was observed in this same temperature range. This anomalous behavior was ascribed to unusual temperature dependence of either the Young’s modulus or the stacking fault energy, which may be associated, in turn, with a disorder-order transformation on cooling of the alloy. Formerly with the Materials Engineering Section. Department of Mechanical Engineering, Naval Postgraduate School.     

Hot deformation characteristics of INCONEL alloy MA 754 and development of a processing map

The characteristics of hot deformation of INCONEL alloy MA 754 have been studied using processing maps obtained on the basis of flow stress data generated in compression in the temperature range 700 °C to 1150 °C and strain rate range 0.001 to 100 s^-1. The map exhibited three domains. (1) A domain of dynamic recovery occurs in the temperature range 800 °C to 1075 °C and strain rate range 0.02 to 2 s^-1, with a peak efficiency of 18 pct occurring at 950 °C and 0.1 s^-1. Transmission electron microscope (TEM) micrographs revealed stable subgrain structure in this domain with the subgrain size increasing exponentially with an increase in temperature. (2) A domain exhibiting grain boundary cracking occurs at temperatures lower than 800 °C and strain rates lower than 0.01 s^-1. (3) A domain exhibiting intense grain boundary cavitation occurs at temperatures higher than 1075 °C. The material did not exhibit a dynamic recrystallization (DRX) domain, unlike other superalloys. At strain rates higher than about 1 s^-1 the material exhibits flow instabilities manifesting as kinking of the elongated grains and adiabatic shear bands. The material may be safely worked in the domain of dynamic recovery but can only be statically recrystallized.     

Dislocation energetics in alpha titanium

Stress relaxation measurements in commercially pure α-Ti (A-55) were performed at a plastic strain of 2×10^?3 in the temperature range 300° to 500°K. The long range component of the flow stress (τ_internal) was measured as a function of temperature over the entire range studied. Contrary to the normal assumption of its temperature independence, this parameter was observed to increase approximately 80 pct as the temperature declined from 500° to 300°K. Measurements of the temperature and strain rate dependence of the effective stress (τ^*) indicated that two distinct thermally activated dislocation motion processes control this mode of deformation in the temperature range studied. A low temperature process governs dislocation motion below 380°K and is characterized byH(τ^*→0)=0.3 ev. The high temperature process controls plastic flow above 400°K and is characterized byH(τ^*→0)?1.1 ev. The preexponential factor appearing in the Arrhenius equation \((\dot \gamma _0 )\) was also determined for both processes and found to be a sensitive function of the effective stress. Activation volume (ν^*): effective stress relationships for both processes were also obtained. The experimental findings quoted above will be discussed in terms of our current understanding of thermodynamics of plastic deformation and hypotheses will be introduced to account for the observed large variations of τ_internal with temperature and \(\dot \gamma _0 \) with τ^*. Mechanistic suggestions for both high and low temperature processes will also be offered.     

Superplasticity in Rapidly Solidified White Cast Irons

Superplastic properties of three different composition white cast irons were investigated in the temperature range of 630 to 725 °C. Fine structures consisting of 1 to 2 μm ferrite grains were developed in these materials by consolidation of rapidly solidified powders at intermediate temperatures below the A₁ critical temperature. Tensile elongations of 1410 pct were found for a 3.0 pct C + 1.5 pct Cr white cast iron, 940 pct for a 3.0 pct C white cast iron, and 480 pct for a 2.4 pct C white cast iron when tested at 700 °C and at a strain rate of 1 pct per minute. The superplastic white cast irons exhibited a high strain rate sensitivity exponent,m, of 0.5 and activation energies for plastic flow were found to be nearly equal to the activation energy for grain boundary self-diffusion in iron. These observations are in agreement with the creep behavior of superplastic materials controlled by grain boundary diffusion. OSCAR A. RUANO, formerly with the Department of Materials Science and Engineering, Stanford University. LAWRENCE E. EISELSTEIN, formerly with the Department of Materials Science and Engineering, Stanford University.     

Creep of fine wires of W-ThO2 alloys

The increasing interest in the application of fine wires as high strength structural components,e.g., in high temperature composite materials, makes an understanding of the differences between the creep behavior of large specimens and that of fine wires desirable. In this investigation, the creep properties of fine wires of recrystallized W-1 wt pct ThO₂ were studied over the temperature range between 1800° to 2750°C. In tungsten wires in which the dispersion of fine thoria particles stabilized a fine grained structure, the stress dependence of the creep rate varies with test temperature and stress. For test temperatures below 2500°C, a stress dependence ofn ~ 5 was found, indicative of creep deformation due to dislocation climb processes, while for temperatures above 2500°C and low stresses, values ofn < 2 were obtained, indicative of deformation by grain boundary sliding and diffusional creep processes. In wires which recrystallized to a large-grained structure, having a large aspect ratio, a high stress dependence of 15 was found when tested at 1800°C.     

Warm-temperature tensile ductility in Al-Mg alloys

Several binary and ternary Al alloys containing from 2.8 to 5.5 wt pct Mg were tested in tension at elevated temperatures (200 °C to 500 °C) over a range of strain rates (10⁻⁴ to 2.0 s⁻¹). Tensile ductilies of up to 325 pct were obtained in binary Al-Mg alloys with coarse grains deformed in the solute-drag creep regime. Under test conditions in which solute-drag creep controls deformation, Mg in concentrations from 2.8 to 5.5 wt pct neither affects tensile ductility nor influences strain-rate sensitivity or flow stress significantly. Strength is shown to increase with increasing Mg concentration, however, in the power-law-breakdown regime. The solute-drag creep process, which leads to superplastic-like elongations, is shown to have no observable grain-size dependence in a binary Al-Mg material. Ternary alloying additions of Mn and Zr are shown to decrease the strain-rate sensitivity during solute-drag creep, negatively influencing ductility. An important cause of reduced ductility in the ternary alloys during creep deformation is found to be a transition from necking-controlled failure in the binary alloys to cavitation-controlled failure in the ternary alloys investigated. An increase in ternary element concentration, which can increase the relative volume percentage of proeutectic products, increases cavitation.     

Characterization of superplastic deformation behavior of a fine grain 5083 Al alloy sheet

Superplastic deformation behavior of a fine grain 5083 Al sheet (Al-4.2 pct Mg-0.7 pct Mn, trade name FORMALL 545) has been investigated under uniaxial tension over the temperature range of 500 °C to 565 °C. Strain rate sensitivity values >0.3 were observed over a strain rate range of 3 × 10⁻⁵ s⁻¹ to 1 × 10⁻² s⁻¹, with a maximum value of 0.65 at 5 × 10⁻⁴ s⁻¹ and 565 °C. Tensile elongations at constant strain rate exceeded 400 pct; elongations in the range of 500 to 600 pct were obtained under constant crosshead speed and variable strain rates. A short but rapid prestraining step, prior to a slower superplastic strain rate, provided enhanced tensile elongation at all temperatures. Under the two-step schedule, a maximum tensile elongation of 600 pct was obtained at 550 °C, which was regarded as the optimum superplastic temperature under this condition. Dynamic and static grain growth were examined as functions of time and strain rate. It was observed that the dynamic grain growth rate was appreciably higher than the static growth rate and that the dynamic growth rate based on time was more rapid at the higher strain rate. Cavitation occurred during superplastic flow in this alloy and was a strong function of strain rate and temperature. The degree of cavitation was minimized by superimposition of a 5.5 MPa hydrostatic pressure during deformation, which produced a tensile elongation of 671 pct at 525 °C. R. VERMA, formerly Visiting Scientist, Department of Materials Science and Engineering, University of Michigan     

History Dependence of the Microstructure on Time-Dependent Deformation During <Emphasis Type="Italic">In-Situ</Emphasis> Cooling of a Nickel-Based Single-Crystal Superalloy

Time-dependent plastic deformation through stress relaxation and creep deformation during in-situ cooling of the as-cast single-crystal superalloy CMSX-4^® has been studied via neutron diffraction, transmission electron microscopy, electro-thermal miniature testing, and analytical modeling across two temperature regimes. Between 1000 °C and 900 °C, stress relaxation prevails and gives rise to softening as evidenced by a decreased dislocation density and the presence of long segment stacking faults in γ phase. Lattice strains decrease in both the γ matrix and γ′ precipitate phases. A constitutive viscoplastic law derived from in-situ isothermal relaxation test under-estimates the equivalent plastic strain in the prediction of the stress and strain evolution during cooling in this case. It is thereby shown that the history dependence of the microstructure needs to be taken into account while deriving a constitutive law and which becomes even more relevant at high temperatures approaching the solvus. Higher temperature cooling experiments have also been carried out between 1300 °C and 1150 °C to measure the evolution of stress and plastic strain close to the γ′ solvus temperature. In-situ cooling of samples using ETMT shows that creep dominates during high-temperature deformation between 1300 °C and 1220 °C, but below a threshold temperature, typically 1220 °C work hardening begins to prevail from increasing γ′ fraction and resulting in a rapid increase in stress. The history dependence of prior accumulated deformation is also confirmed in the flow stress measurements using a single sample while cooling. The saturation stresses in the flow stress experiments show very good agreement with the stresses measured in the cooling experiments when viscoplastic deformation is dominant. This study demonstrates that experimentation during high-temperature deformation as well as the history dependence of the microstructure during cooling plays a key role in deriving an accurate viscoplastic constitutive law for the thermo-mechanical process during cooling from solidification.     

Effect of friction stir processing on the kinetics of superplastic deformation in an Al-Mg-Zr alloy

The effect of friction stir processing on the superplastic behavior of extruded Al-4Mg-1Zr was examined at 350 °C to 600 °C and at initial strain rates of 1×10⁻³ to 1 s⁻¹. A combination of a fine grain size of 1.5 μm and high-angle grain boundaries in the friction stir-processed (FSP) alloy led to considerably enhanced superplastic ductility, much-reduced flow stress, and a shift to a higher optimum strain rate and lower optimum temperature. The as-extruded alloy exhibited the highest superplastic ductility of 1015 pct at 580 °C and an initial strain rate of 1×10⁻²s⁻¹, whereas a maximum elongation of 1280 pct was obtained at 525 °C and an initial strain rate of 1×10⁻¹s⁻¹ for the FSP alloy. The FSP alloy exhibited enhanced superplastic deformation kinetics compared to that predicted by the constitutive relationship for superplasticity in fine-grained aluminum alloys. A possible origin for enhanced superplastic deformation kinetics in the FSP condition is proposed.     

Dynamic phase transformation during superplastic deformation of Nb/Nb<Subscript>3</Subscript>Al <Emphasis Type="Italic">in-situ</Emphasis> composite

Nb_ss/Nb₃Al in-situ composite with the nominal composition of Nb-16 mol pct Al-1 mol pct B, consisting of bcc niobium solid solution (Nb_ss) and A15 ordered Nb₃Al, was synthesized by arc melting, homogenization annealing, and isothermal forging, and their superplastic deformation behavior was investigated by tensile tests and microstructure observations. Maximum superplastic elongation over 750 pct was obtained at 1573 K and at a strain rate of 1.6 × 10⁻⁴ s⁻¹ for as-forged specimens. Phase transformation from Nb_ss to Nb₃Al was observed to occur during superplastic deformation. Dynamic phase transformation during superplastic deformation progresses more quickly than static phase transformation during annealing without applied stress. Dynamic phase transformation is accompanied by phase-boundary migration, which operates as an accommodation process of grain-boundary sliding. Dislocation creep dominates deformation and grain-boundary sliding is inhibited at a high strain rate, while grain-boundary sliding and cavity formation are promoted at a low strain rate because of insufficient accommodation of grain-boundary sliding arising from sluggish dynamic phase transformation. It is concluded that there exists an optimum strain rate that guarantees the grain-boundary sliding and the rapid dynamic phase transformation to achieve maximum superplastic elongation.