Influence of test temperature and microstructure on the tensile properties of titanium alloys

Tensile tests were performed between room temperature and 500 °C on age-hardened Ti-Al and Ti-6A1-4V alloys to study the effect of various microstructural parameters on the temperature dependence of the yield stress. It was found that the concentration of interstitial solute atoms is responsible for the strong temperature dependence of the yield stress. Small interstitial concentrations increase the yield stress significantly at low test temperatures, while this hardening effect almost disappeared at temperatures above about 300 °C. Through variations of degree of age-hardening, grain size, texture, phase morphology, and phase dimensions of (α + β) microstructures, the absolute yield stress values were changed by constant amounts over the test temperature range without changing significantly the temperature dependence. The yield stress increased by increasing the degree of age-hardening, by decreasing the grain size or phase dimensions, by texture hardening, and by choosing equiaxed instead of lamellar phase morphologies.     

The effect of copper content and microstructure on the hydrogen embrittlement of AI-6Zn-2Mg alloys

Two commercially-processed Al-6Zn-2Mg alloys, 7050 and a “low copper” 7050, were tested for susceptibility to embrittlement by precharged hydrogen and by simultaneous cathodic charging and straining (SET procedure). Specimens were heat treated to underaged, peak-strength aged, and overaged conditions. In 7050, the peak strength and overaged conditions were not embrittled by hydrogen, though underaged material showed marked embrittlement. All microstructures tested for the low-copper alloy were embrittled. The results agree with the microstructural rationale established through earlier work on 7075 and 2124 aluminum alloys, particularly with respect to the susceptibility of underaged material to hydrogen. As in earlier work, the extent of dislocation transport of hydrogen, and local hydrogen accumulation at grain boundaries, evidently controlled the extent and degree of brittle fracture. These three important alloys can now be ranked in the order 7050, 2124, 7075 of increasing relative susceptibility to theonset of stress corrosion cracking.     

Grain boundary embrittlement of the iron-base superalloy IN903A

It is shown that a low coefficient of expansion, iron-base superalloy, IN903A, suffers severe tensile embrittlement following high temperature air exposure at 1000 °C. This embrittlement involves a transition to intergranular failure at low strains, with no reduction in yield strength, and is manifested in the room temperature to 800 °C range. In parallel with earlier observations on nickel-base superalloys, ductility is regained at 1000 °C. However, in contrast to these earlier results, air exposure enhances rather than hinders grain growth in the near surface regions, and, in addition, suppresses the occurrence of the jerky flow seen in vacuum-exposed material. Oxygen is demonstrated to be the damaging species, and it is show’n that boundaries are embrittled far ahead of any matrix internal oxidation. Small additions of boron are successful in eliminating the embrittlement, as they were in nickel-base alloys. The results of stress rupture tests are then reviewed, and it is concluded that the rapid failures which occur on air testing are a consequence of embrittled grain boundaries failing in tension, rather than the stress accelerated grain boundary oxidation mechanism previously proposed.     

Influence of microstructure on the mechanical

The significance of matrix and grain boundary microstructural characteristics on the mechanical properties and stress corrosion susceptibility of 7075 aluminum alloy has been evaluated. Maximum strength was found to be associated with a Guinier-Preston zone matrix. The precipitate-free-zone adjacent to high angle grain boundaries had only a slight effect on yield and tensile strength but a greater influence on hardness. Stress corrosion susceptibility was studied in an aqueous chloride environment over a 0.7–3.5 pH range. For material of highest strength, grain boundary precipitate spacing was found to be of primary importance to susceptibility. The effect of grain boundary precipitate spacing is most significant to the crack propagation stage of stress corrosion. These results indicate that improved properties for Al-Mg-Zn type alloys could be attained by a desirable combination of matrix and grain boundary structure.     

The effect of fe additions on the embrittlement of Cu-Bi alloys

The effect of iron additions on the embrittlement of Cu-Bi alloys was studied by monitoring the ductility and grain boundary chemistry of embrittled specimens as a function of iron content. Mechanical properties improved for the same embrittling heat treatment as the bulk iron level increased, and this was correlated with a decrease in bismuth segregation to the grain boundaries. No iron was detected segregated to the boundaries, and several possible mechanisms were proposed to explain the beneficial effect of the iron additions. It was also found that approximately 70 min at 530°C is required to attain equilibrium for segregation of bismuth to the grain boundaries, and a diffusion coefficient derived from this data was found to be reasonable for bulk diffusion of bismuth in copper.     

The effect of fe additions on the embrittlement of Cu-Bi alloys

The effect of iron additions on the embrittlement of Cu-Bi alloys was studied by monitoring the ductility and grain boundary chemistry of embrittled specimens as a function of iron content. Mechanical properties improved for the same embrittling heat treatment as the bulk iron level increased, and this was correlated with a decrease in bismuth segregation to the grain boundaries. No iron was detected segregated to the boundaries, and several possible mechanisms were proposed to explain the beneficial effect of the iron additions. It was also found that approximately 70 min at 530°C is required to attain equilibrium for segregation of bismuth to the grain boundaries, and a diffusion coefficient derived from this data was found to be reasonable for bulk diffusion of bismuth in copper.     

Anneal hardening and flow softening in beta zirconiumniobium alloys

The flow properties of β-Zr-Nb (Cb) alloys were investigated by means of compression testing in the strain rate range 10^-1 to 10^-5 s^-1 and from 725 to 1025°C. The flow curves obtained on Zr-Nb alloys containing 10, 15 and 20 pct Nb exhibited flow softening, and the magnitude of this effect decreased as the temperature was increased. All three alloys also exhibited anneal hardening, i.e. an increase in flow stress at 825°C with annealing time at 1000°C. Neither the flow softening, nor the anneal hardening could be associated with environmental effects, as in Zr-Mo alloys, nor could they be attributed to texture changes or to the occurrence of dynamic recrystallization. On the basis of X-ray and microprobe investigations, as well as grain size measurements, it is concluded that the anneal hardening is due to the combined effect of grain growth and the formation of solute clusters during annealing. The occurrence of flow softening is attributed to the destruction of the solute clusters by straining. Stress-strain curves were also determined for Zr-2.5 pct Nb. Unlike the high Nb alloys, these materials exhibited neither flow softening nor anneal hardening. The flow stresses were found to be highly strain rate dependent, with stress sensitivities of about 5.5 for yielding and 4.5 for steady state flow.     

Effects of hydrogen on some mechanical properties of vanadium-titanium alloys

The effect of hydrogen on the strength and ductility of V-Ti alloys was investigated from 78 to 300 K. Alloy softening which was observed at low temperatures for V-Ti alloys containing 5 at. pct of titanium or less was mitigated by the addition of hydrogen, and low temperature hardening took place. Hydrogen embrittlement, as measured by reduction of area, was observed in both the hydride forming V-1Ti alloy and some nonhydride forming V-Ti alloys. In alloys containing 10 at. pct of titanium the addition of hydrogen caused low temperature embrittlement, the range of which increased as the hydrogen concentration was increased. Failure of the severely embrittled alloys was found to be initiated transgranularly for the hydride forming V-1Ti alloy and intergranularly for alloys which did not form hydrides. A possible reason for this difference in crack initiation is discussed.     

The Effect of Phosphorus Content on the Hydrogen Stress Cracking of High Strength 4130 Steel

A series of four 4130 base steels with various phosphorus concentrations was subjected to cathodic charging to determine the effect of P on hydrogen stress cracking resistance. Static fatigue curves for several different yield strengths were obtained for each alloy. At high yield strengths under applied loads of 60 to 80 pct of the yield, 50 ppm P (bulk concentration) was enough to provide sufficient grain boundary P for an impurity-hydrogen interaction which produced intergranular fracture along prior austenite grain boundaries. Decreasing yield strength and applied stress caused a transition in fracture mode to transgranular while the resistance to hydrogen stress cracking increased with decreasing P. Microhardness measurements of prior austenite grain boundaries were made to establish the role of P. The role of P is not apparently related to its capacity as a strengthening element but more probably as a hydrogen recombination poison. Grain boundary hardness measurements for low temperature tempers (200 °C) appear to be valid while those at 500 °C were not.     

Indentation loading studies of acoustic emission from temper and hydrogen embrittled A533B steel

Isothermal tempering at 500 °C (within the region rendering low alloy steels susceptible to reversible temper embrittlement) induced acoustic emission activity in A533B steel during indentation loading. Samples, when sectioned, were found to contain small (∼10 μm long) MnS inclusions, some of which had debonded from the matrix material when they were near the indentations. Hydrogen charging prior to testing greatly enhanced the acoustic emission activity. It also resulted in the formation of small (∼20 to 200 μm) microcracks in samples tempered at 500 °C. These microcracks, when examined by optical metallography, appear to have propagated along prior austenite grain boundaries, consistent with fractographic observations of temper embrittlement in other low alloy steels. Many were nucleated by MnS inclusion debonding and all were confined to within a few hundred micrometers of the sample surface and within two or three indenter diameters from the indent. It is proposed that trace impurities (P, As, Sb, Sn) diffuse during the 500 °C temper to both the MnS inclusion interfaces and the prior austenite grain boundaries, reducing local cohesive strength. The tensile field created by the indenter debonds inclusions to form crack nuclei. Moderate acoustic emission results. In the absence of hydrogen these void nuclei may grow but do not coalesce to form observable cracks. The prior austenite grain boundaries, which in contrast to the dispersed inclusions can provide continuous crack paths, are not sufficiently temper embrittled to fracture without the assistance of hydrogen at these stresses. Hydrogen charging induces a high hydrogen concentration in a surface layer of the sample. This reduces further the grain boundary cohesion, and cracks initiated at inclusions are able to propagate along continuous grain boundary paths, generating additional energetic acoustic emission signals. This process can continue after unloading the indenter due to hydrogen diffusion to the residual stress field.     

The hydrogen embrittlement of Fe-Ni martensites

Iron alloys containing 20 and 30 pct Ni and 3 to 4 cu cm H per 100 g metal have been subjected to slow strain-rate tensile tests in a study of hydrogen embrittlement. In the lower nickel massive martensite alloy, embrittlement is manifest as the cracking of prior austenite grain boundaries and is severe at room temperature but less marked at -196°C; while in the higher nickel acicular martensite alloy, the embrittlement observed at 20°C does not occur at —196°C. Hydrogen embrittlement in these materials is believed to be the result of high hydrogen contents in the vicinity of the prior austenite grain boundaries combined with stress concentrations caused by boundary perturbations which result from the impact of the martensite shears. During deformation, microcracks form and propagate in the prior austenite grain boundaries, probably assisted by internal hydrogen pressure and the lowering of crack surface energy by hydrogen adsorption. The temperature dependence and the effect of the type of martensite on the embrittlement can be explained by their effects on the hydrogen content and stress concentrations at prior austenite grain boundaries during deformation.     

Auger electron spectroscopy study of grain boundary segregation in alloy K-500: Part I. Behavior in as-processed state

Increased interest has been paid to grain boundary segregation in alloy K-500 due to severe intergranular cracking recently observed in forged bars. However, little systematic study of this segregation has been performed so far. A detailed auger electron spectroscopy (AES) study of grain boundary segregation in alloy K-500 has been carried out as a function of alloy chemistry. To determine C segregation, the C and O contamination rates in a vacuum chamber were measured and the necessary condition for C grain boundary segregation determination was established. It has been found that severe C, Al, and Cu segregation to grain boundaries occurred and depended on alloy chemistry. High bulk Ni and low bulk Al promoted C and Al grain boundary segregation, and low bulk Ni and high bulk Al significantly enhanced Cu segregation to grain boundaries. The depth profiles of intergranularly segregated elements also showed different features for high and low Ni content alloys. In high Ni alloys, C and Al levels dropped continuously as a function of distance from the grain boundaries but the Cu level dropped only slightly. In low Ni alloys, the Al and C levels rose from relatively low grain boundary levels to a peak at a certain distance from the grain boundary where the high grain boundary Cu level dramatically dropped. Transmission electron microscope (TEM) observation revealed a grain boundaryγ′-depleted zone followed by a region with coarser and denserγ′ particles in low Ni and high Al alloys but quite uniformly distributedγ′ particles with no depleted zone in high Ni and low Al alloys. These can be explained by the observed segregation behavior. The occurrence of Cu segregation is explained according to available theories about surface segregation in binary Ni-Cu alloys, and the segregation of C and Al to grain boundaries is suggested to be probably due to their interaction with Ni and Cu.     

Preparation and properties of fine grain β- CuAlNi strain- memory alloys

A method has been developed to produce grain sizes as small as 5 μm in alloys of β-CuAlNi. The alloys were of eutectoid composition and a procedure was developed for determining the composition of a eutectoid alloy having any required value for transition temperature (M _s ). The thermo-mechanical treatment involved two sequential stages of warm rolling followed by recrystallization. The alloys produced were single phase β-type with no second phase being present. Characteristic two-stage stress-strain curves were obtained for most of the specimens. It was generally found that the tensile strength and strain to failure increased with decreasing grain size according to a Hall-Petch type relationship down to a grain size of 5 μm. A fracture strength of 1200 MPa and a fracture strain of 10 pct were obtained in the best alloy. It was found that the major recovery mode, whether pseudoelastic or strain-memory, did not have any significant effect on the total recovery obtained. Recovery properties were not affected significantly by decreasing grain size, and 86 pct recovery could still be obtained at a grain size of around 10 μm. Grain refinement improved the fatigue life considerably, possibly due to the high ultimate fracture stress and ductile fracture mode. A fatigue life of 275,000 cycles could be obtained for an applied stress of 330 MPa and a steady state strain of 0.7 pct. At fine-grain sizes most of the fractures were due to transgranular-type brittle fracture and micro void-type ductile fracture, depending on the alloy composition. It was suggested that the difference between the alloys was due to differences in oxygen segregation at the grain boundaries.     

Precipitation hardening of aluminum alloys

The author’s charge was to discuss recent trends in research and development on precipitation hardened aluminum alloys and to indicate where research is needed. This will be done for three areas: fatigue, properties of grain boundaries and interfaces, and stability of precipitates at elevated temperatures. Present strong precipitation hardened aluminum alloys do not have high endurance limits. One problem is that the small GP zones are cut by the dislocations giving rise to highly localized deformation which aids fatigue crack initiation. A duplex structure with relatively large uniformly spaced precipitates to give more homogeneous deformation plus small precipitates to give high yield strength is a promising approach. The structures of precipitation hardened aluminum base alloys are essentially controlled by the stabilities of the various precipitates and the interfacial energies. Precipitates with high interfacial energies tend to precipitate preferentially at grain boundaries giving embrittlement. Low interfacial energy means easy nucleation, a uniform precipitate distribution, and resistance to coarsening at elevated temperatures. For elevated temperature use, the precipitate must be stable at elevated temperatures. Precipitation hardened aluminum alloys do not have good elevated temperature properties because the hardening precipitates normally used, GP zones, are not stable at elevated temperatures. Thus a low interfacial energy, ductile precipitate, which is stable at elevated temperatures, is needed for aluminum. Possibilities for achieving such precipitates will be discussed. This paper is based on an invited presentation made at a symposium on “Advances in the Physical Metallurgy of Aluminum Alloys” held at the Spring Meeting of TMS-IMD in Philadelphia, Pennsylvania, on May 29 to June 1, 1973. The symposium was co-sponsored by the Physical Metallurgy Committee and the Non-Ferrous Metals Committee of TMS-IMD.     

The effect of grain boundaries on the athermal stress of tantalum and tantalum-tungsten alloys

The temperature dependence of the yield stress of polycrystalline Ta, Ta-2.47 wt pct W (Ta-2.5W), and Ta-9.80 wt pct W (Ta-10W) was measured to study the effect of grain boundaries and tungsten concentration on athermal strength components. Compression tests were performed over a temperature range from 77 to 1223 K at strain rates of 10⁻⁴ and 10⁻¹ s⁻¹. The test results show that the yield stress of Ta becomes independent of temperature above about 400 K, indicating an “athermal” regime. In contrast, the temperature dependence of yield stress was still significant for Ta-10W up to the maximum test temperature. An analysis of the test data using single-crystal data in conjunction with Taylor factors was performed to assess the effect of grain boundaries on the athermal component of flow stress at 600 K. The results indicated that the long-range athermal stress at the yield point due to grain boundaries is approximately 13 to 41 MPa for the study materials and decreases with an increase in tungsten concentration. These results are discussed with regard to constitutive modeling of flow stress.     

Influence of Grain Size and Age-Hardening on Dislocation Pile-Ups and Tensile Fracture for a Ti-AI Alloy

In an aged Ti-8.6 wt pct Al alloy macroscopic embrittlement occurs with increasing grain size and degree of age hardening. The influence of the grain sizeL on the true fracture strain can be described by εF ∼L-¹ Tensile crack nucleation is caused microscopically by strong dislocation pile-ups which crack the grain boundaries. Using transmission electron microscopy and equations from the dislocation theory, an experimental method was developed to determine quantitatively the shear stress concentrations at the grain boundaries which are produced by the dislocation pile-ups and cause crack nucleation. The experimental results show that for all investigated grain sizes and degrees of age hardening a critical local stress t* _C ≈ 38 GPa leads to crack nucleation. Based on this result equations were derived which describe the combined influence of grain size and age hardening on the true fracture strain and on the true fracture stress. These equations show a good agreement with the tensile test results.     

Constitutive behavior of tantalum and tantalum-tungsten alloys

The effects of strain rate, temperature, and tungsten alloying on the yield stress and the strainhardening behavior of tantalum were investigated. The yield and flow stresses of unalloyed Ta and tantalum-tungsten alloys were found to exhibit very high rate sensitivities, while the hardening rates in Ta and Ta-W alloys were found to be insensitive to strain rate and temperature at lower temperatures or at higher strain rates. This behavior is consistent with the observation that overcoming the intrinsic Peierls stress is shown to be the rate-controlling mechanism in these materials at low temperatures. The dependence of yield stress on temperature and strain rate was found to decrease, while the strain-hardening rate increased with tungsten alloying content. The mechanical threshold stress (MTS) model was adopted to model the stress-strain behavior of unalloyed Ta and the Ta-W alloys. Parameters for the constitutive relations for Ta and the Ta-W alloys were derived for the MTS model, the Johnson—Cook (JC), and the Zerilli-Armstrong (ZA) models. The results of this study substantiate the applicability of these models for describing the high strain-rate deformation of Ta and Ta-W alloys. The JC and ZA models, however, due to their use of a power strain-hardening law, were found to yield constitutive relations for Ta and Ta-W alloys that are strongly dependent on the range of strains for which the models were optimized.     

The effect of reactive metal additions on grain boundary embrittlement in 18Ni200 maraging steel

Maraging steel can be embrittled by slowly cooling between 1850° and 1400°F from elevated temperatures (>2200°F). The object of this work was to examine the effect of various refining and hardening additions on the slow cooling embrittlement response of 18Ni200 maraging steel. Small refining additions of magnesium give a partial but significant reduction of embrittlement that is caused by grain boundary precipitates. Ca, B, and Zr did not have this beneficial effect. Of the hardening elements studied, only titanium could be associated with the embrittlement. Titanium was otherwise the best hardening addition, judged from its combined effect on the yield strength and toughness of normally annealed plus aged material.     

Precipitation of austenite particles at grain boundaries during aging of Fe-Mn-Ni steel

Precipitation of austenite particles at grain and lath boundaries after aging treatment of a Fe-8Mn-7Ni alloy was investigated by selected area electron diffraction (SAD), X-ray energy dispersive spectrometry (EDS) in a scanning transmission electron microscope (STEM), and high-resolution (HRTEM) analysis. High spatial-resolution (2 to 5 nm) EDS analysis revealed no significant segregation of alloying elements at grain boundaries but the precipitation of very fine particles of Mn- and Ni-rich phase. Detailed EDS, SAD, and HRTEM analyses all confirmed that these particles are austenite phase, which have a Kurdjumov-Sachs (K-S) orientation relationship with one of the adjacent grain. The concentration of Mn and Ni in austenite, measured by EDS, varied from ∼15 pct to a maximum of ∼30 pct. Low-voltage scanning electron microscopy (SEM) fractographs also revealed the presence of very fine, second-phase precipitates on the fracture surface of the embrittled alloys.