Microstructural and dimensional stabilities of a potential γ/γ′-α(Mo) directionally solidified eutectic superalloy under cyclic thermal exposure to 1000° C

A potential heat-resistant ductile eutectic composite,/-, in the Ni-Al-Mo ternary system has been thermally cycled in the temperature range 200 to 1000° C for up to 1000 cycles in an attempt to examine dimensional as well as microstructural stability of the composite under thermal fatigue conditions. The composite examined has two types of initial microstructure; in one, blocky -Ni₃Al encircles individual-Mo fibres (as-grown condition) whereas in the other, is in the form of fine cuboidal particles uniformly distributed in an Ni-rich fcc matrix (heat-treated condition). Dilatometric measurements upon temperature cycling show that the composite is stable against thermal ratchetting irrespective of initial microstructural conditions. However, the cycling induces microstructural change, which is characterized by segmentation of-Mo fibres or formation of a detrimental brittle phase identified as an intermetallic-NiMo that consumes-Mo fibres whether the fibres are encircled by or not. Post-cycling tensile tests at room temperature show that the fibre damage in the former has no fatal effect on tensile strength and ductility. A beneficial effect of the-encircling configuration is discussed on the basis of the recognition of a peritecto-eutectoid reaction:++ that has been disregarded.     

Effect of retained austenite on the microstructure and mechanical properties of martensitic precipitation hardening stainless steel

The effect of retained austenite () on the microstructure and mechanical properties of a martensitic precipitation hardening stainless steel was experimentally investigated, whose chemical composition was Fe-1.8Cu-15.9Cr-7.3Ni-1.2Mo-0.08Nb-low C, N (mass%). The microstructures of all specimens consist of a typical lath martensite with interlath films of the retained , which is not reverted with aging. Cu-rich precipitates which may contribute to precipitation hardening can not clearly be observed. The tensile properties and Charpy absorbed energy are linearly approximated to the amount of retained as follows: 0.2% Y.S. (MPa) = 1192.3 – 13.6 × %, T.S. (MPa) = 1250.1 – 9.3 × %, El. (%) = 12.16 + 0.43 × %, R.A. (%) = 64.25 + 0.14 × %, and A.E. (J) = 72.5 + 0.8 × %. The introduction of retained is not beneficial to the fatigue limit. An excellent combinations of strength, ductility and toughness obtained in the present work is attributed to the introduction of retained and also to the chemical composition of the specimen used.     

Stress-induced phase transformations in a hot-deformed two-phase (α2+γ) TiAl alloy

Stress-induced 2, 2 and 9R phase transformations in a hot-deformed Ti–45 at% Al–10 at% Nb alloy have been investigated using high-resolution transmission electron microscopy. The 2 phase transformation is an interface-related process. The interfacial superdislocations emitted from the misoriented semicoherent 2– interface react with each other or with the moving dislocations in the phase, resulting in the formation of the 2 phase. The nucleation of the 2 phase transformation takes place either at the 2– interfaces or at the stacking faults on the basal plane of 2 phase, and the growth of plate is accomplished by the moving of a/61 0 1 0 Shockley partials on alternate basal plane (0 0 0 1)2. The 9R structure was usually found to form at incoherent twin or pseudotwin boundaries. During deformation the interfacial Shockley partial dislocations of these incoherent twin and pseudotwin boundaries may glide on (1 1 1) planes into the matrix, resulting in the formation of 9R structure. The interfaces (including 2– and – interfaces) as well as the crystallographic orientation relationship between the as-received or stress-induced 2, and 9R phase have been analysed. The mechanisms for the stress-induced 2, 2 and 9R phase transformations were also discussed. © 1998 Chapman & Hall     

The Ni3Al-Ni3Cr-Ni3Ru section of the Ni-Cr-Al-Ru system

An investigation is reported of the 75 at% nickel section of the Ni-Cr-Al-Ru system at 1523 and 1273 K. Constitutional data obtained by electron probe microanalysis, X-ray diffraction and microscopical examination are presented as partial isothermal sections. At 1523 K, the major part of the section consists of phase, while the aluminium-rich region contains a and+ region; the extent of the solid solution of chromium and ruthenium in totals ~ 4 at%. The ruthenium-rich corner of the section shows a two-phase region consisting of + ruthenium-rich solid solution. At 1273 K the,+ and + ruthenium regions increase in extent. The/ mismatch values in the equilibrated alloys studied lie in the range ~ –0.08 to –0.39%. Constitutional features of as-cast alloys are also reported.     

The Ni3Al-Ni3Cr-Ni3Mo section of the Ni-Cr-Al-Mo system

An investigation is reported of the constitution of the 75 at % nickel section of the Ni-Cr-Al-Mo system in the temperature range 1523 to 1073 K. Alloys in the region 10 to 20 at % Al were annealed at 1523, 1273, and 1073 K, respectively, and subjected to electron microprobe analysis, X-ray diffraction, and microscopical and hardness examination. Constitutional data are presented as partial isothermal sections and as vertical sections. At 1523 K the section consists only of fields containing ,+ and , the last mentioned phase being predominant. With decreasing temperature the and + fields increase in extent. Also, the NiMo and Ni₃Mo phases were encountered in the ternary Ni-Al-Mo alloy studied. The quaternary + alloys showed small lattice mismatch values, i.e. up to 0.25%. Raft like morphologies of were found in the quaternary alloys, resulting from directional coarsening. Observations of as-cast structures are also reported.     

Grain refinement of a TiAl alloy by heat treatment through near gamma transformation

Casting of TiAl alloys is receiving more and more research because of its relatively low cost. One problem with this technology is that the coarse microstructure developed during solidification is harmful to material properties. Thus it is essential to seek an approach to refining the cast microstructure and this approach may also be applicable to cast components. In this study, a novel heat treatment route is proposed to obtain a fine fully lamellar structure from a cast TiAl alloy with a grain size of 1000 m. This route consists of three steps, namely pretreatment to have a feathery structure, annealing in the + region to have a fine near gamma structure and solution treatment to develop a fully lamellar structure with a grain size of 30 m.     

The constitution of the Ni-Al-Ru system

The constitution of the Ni-Al-Ru system has been investigated in the range 0 to 50 at% Al. Isothermal sections at 1523 and 1273 K have been determined using microstructural observations, electron probe microanalysis and X-ray diffraction. The phases present were: nickel-based solid solution (); (based on Ni₃Al); solid solutions based on NiAl and RuAl, respectively (designated ₁ and ₂), and ruthenium-based solid solution (Ru). The maximum solubility of Ru in was 5 at%. ₁, and ₂ show extensive range of solubilities, namely up to 20at% Ru in ₁ and up to 25 to 35 at% Ni in ₂. Three-phase equilibrium between , ₂ and (Ru) existed at 1523 and 1273 K. Also at 1523 K, three-phase equilibria existed between , and ₁ and ,₁ and ₂, while at 1273 K, the equilibria were between , ₁,₂ and , , ₂ indicating the occurrence of a reaction +₁, +₂ at a temperature between 1523 and 1273 K. Liquidus features have been deduced from data on as-solidified structures. Lattice parameter data and hardnesses are also reported.     

The effective surface energy of brittle materials

The effective surface energy of four brittle materials, alumina, poly(methylmethacrylate), glass, and graphite, is calculated from load/deflection curves of notched bars deformed in three-point bending. Two of the methods, which are commonly used in fracture mechanics studies,viz the modified Griffith treatment and the compliance analysis method, are concerned with the effective surface energy at the initiation of fracture, _I . The third method, the work of fracture test, is concerned with the mean effective surface energy over the whole fracture process, _F . The two estimates of _I give consistent values, and there is no systematic variation of _I with notch depth. Values of _F decrease with increasing notch depth as the fracture process becomes more controlled. For alumina _{I F} . For PMMA and glass _I > _F because of a multiplicity of crack sources during fracture initiation. For graphite _I < _F because of subsidiary cracking as fracture proceeds.     

Elevated temperature deformation behaviour of multi-phase Ni-20 at % Al-30 at % Fe and its constituent phases

The mechanical behaviour of the multi-phase ( + /) alloy Ni-20 at % Al-30 at % Fe and alloys similar to its constituent and / phases, Ni-30 at % Al-20 at % Fe and Ni-12 at % Al-40 at % Fe, respectively, were investigated. When tested in tension at 300 K, the alloys exhibited 20%, 2% and 28% elongation, respectively. At elevated test temperatures (700, 900 and 1100 K), the multi-phase alloy exhibited increased ductility, reaching an elongation in excess of 70% at 1100 K without necking or fracture. Similarly, the alloy demonstrated increased ductility with increasing test temperatures. In contrast, the / alloy showed greatly reduced ductility with increasing temperature and was quite brittle both at 900 and 1100 K. Thus, whilst at room temperature the / phase improved the ductility of the + / aggregate, at elevated temperatures the phase alleviated the brittleness of the / phase, thereby preventing any embrittlement of the multi-phase alloy over the temperature range 300–1100 K. Also, whilst the phase improved the room-temperature strength of the multi-phase alloy, at elevated temperatures where the phase is known to be weak, the / phase improved the strength of the multi-phase alloy up to 900 K, beyond which the strength deteriorated due to disordering and lack of anomalous strengthening in the / component.     

Morphological and crystallographic features of γ-γ′ Ni-Al and Ni-Al-Ti two-phase bicrystals

Several- Ni-Al and Ni-Al-Ti two-phase bicrystals were made by the solid-state diffusion couple method. Each couple consisted of a-phase single crystal and a pure-Ni polycrystal, and was annealed at 1473 K in an Ar gas atmosphere. Single crystal layers of-phase with uniform thickness always grow into the parent-phase single crystals. The resultant/ interface has no voids or facets regardless of the orientation of interface and the chemical composition of the-phase. Porosity formation due to the Kirkendall effect is observed in the diffused region. Concentration profiles exhibit nearly constant gradients in-phase. The orientation relationship between both phases is found to be 001//001, that is, the-phase grows epitaxially along the crystal orientation of-phase.     

Precipitation in Ni-Co-Al alloys

Continuous precipitation of in Ni-Co-Al alloys has been studied using X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The precipitation sequence is observed to be a change of morphology from spheres cube plates. The lattice parameter mismatch is of the order of 0.3%. The particle growth rate has been determined over a range of temperatures for alloys containing a range of cobalt contents from 0 to 55 at %. In all cases the particle size varies att ^1/3 and the particle number density ast ^–1. The growth rate varies very little with increasing volume fraction of . The measured particle growth rate decreases with increasing cobalt content, probably as a result of partitioning of cobalt between particle and matrix. Electron micro-probe analysis, volume fraction measurements and X-ray analyses were used to determine the ( + ) boundary in the Ni-Co-Al ternary system at temperatures between 973 and 1073 K. It is clear from the position of the boundary that a significant beneficial effect of cobalt is in decreasing the solubility of the phase in for any temperature up to 1073 K. Histograms of particle size were constructed and compared with both the Lifshitz-Slyozov-Wagner and the Lifshitz-Slyozov encounter modified (LSEM) predicted distributions. The LSEM theory for particle coarsening was shown to be a much better fit to the experimental particle size distributions.     

The influence of ageing on the stability of β-γ/γ′ derived microstructures in Ni-Al-Cr-(Co) alloys

Multiphase Ni-Al-(Fe)-(Cr)-(Co)-based intermetallics with (B2)- (A1)/(L1₂), - or - microstructures can exhibit significant room-temperature tensile ductility. In the case of Ni-Al-Cr-based alloys, microstructural development is complicated by the precipitation of -Cr, which can supplant the -phase during ageing of three-phase -/ microstructures. An investigation of the stability, during ageing, of cast Ni-Al-Cr-(Co) alloys with microstructures derived from -/ is reported. In the as-cast condition, the materials investigated consisted of a dendritic matrix containing L1₀ type martensite and interdendritic /. Extensive intra- and interdendritic -Cr precipitation was also observed. The stability during ageing of the interdendritic / microstructure is also considered and transformation of the L1₀ martensite is examined.     

Flow-stress recovery of nickel-aluminium alloys

Flow-stress recovery measurements along with structural observations using electron microscopy have been carried out on room-temperature prestrained alloys of Ni-11.9, 13.1 and 13.5 at.% Al aged at 735° C. These alloys contained respectively 0, 5, and 8 vol% Ni₃Al) in a fine dispersion. Samples were recovered at and below the ageing temperature for times ranging from 0.1 to 100 h. The influence of volume fraction of , distribution, amount of prestrain and recovery temperature on recovery kinetics was investigated.Results for samples recovered at 735° C showed a large fractional recovery (about 30%) following the first 0.1 h anneal for all samples. About 50 to 70% of the flow stress is recovered at the end of 100 h recovery anneals. The changes in dislocation structure agreed quantitatively with the changes in flow stress.Interpretation of the data in terms of a network growth model of recovery show the solid solution alloy to agree with theory for long recovery times (t>10 h) whereas the -strengthened alloys deviate considerably from the simple model.     

Effects of carbon content on microstructures and magnetic properties of annealed or solution treated Fe-Cr-Ni-C alloys

The correlations between microstructures and magnetic properties were studied in four Fe-17.5 mass%Cr-2.0 mass%Ni-Xmass%C (X = 0.3–0.6) alloys. Each alloy consisted of ferromagnetic and M₂₃C₆ carbide phases by step-annealing at 1053 K and 848 K. The number of the M₂₃C₆ carbide particles increased with the carbon content, and this microstructural variation caused a deterioration of the soft magnetic properties. On the other hand, the alloy with 0.3 mass% carbon content consisted of ferromagnetic and paramagnetic retained structures after solution treatment at 1473 K. The amount of the stable structure increased with the carbon content, while the amount of the structure decreased. This microstructural variation caused a decrease in the relative permeability, _r, and the stabilization of the paramagnetic property to low temperatures below room temperature. The temperature stability of the _r values was closely related to the martensite start temperature, M _s. From an equation for the estimation of M _s from the chemical compositions of the phase, the M _s's of the alloys with 0.3, 0.4, 0.5 and 0.6 mass%C were estimated to be 326, 289, 241 and 216 K respectively. These values were consistent with the M _s's expected from the microstructures and temperature dependences of the _r values.     

Abundance of 766.6 and 1001 keV γ-Quanta in the 238U Decay Chain

The abundances of 63.3, 185.7, 766.6, 1001 keV -quanta in the ²³⁸U decay chain, determinedby semiconductor -ray spectrometry of metallic uranium foil, are 4.2, 48, 0.39, and 1.12%, respectively.The abundance of 766.6 and 1001 keV -ray quanta is higher than the generally accepted values by a factor of 1.9.     

Brittle fracture of polycrystalline tungsten

A comparative study of the brittle fracture of three varieties of polycrystalline tungsten has been carried out using mainly impact tests, scanning electron microscopy and Auger spectroscopy. It indicates the occurrence of two modes of brittle fracture, namely cleavage and intergranular fractures, whose proportions depend on temperature and on phosphorus segregation at the grain boundaries. Scanning Auger images indicate unambiguously that phosphorus is only located on the intergranular surfaces. No phosphorus is observed on cleavage planes. Fracture surfaces are the result of the propagation of a crack through the whole sample. As the propagation follows the path which requires the lowest expenditure of energy, it depends both on a geometrical factor and on the respective values of the cleavage (_cl) and intergranular (_l) works of fracture. Our results indicate an increase in _cl and _l with temperature (the effect being more marked in the case of _cl) and a large decrease in _l with phosphorus segregation at the grain boundaries. This impurity produces an intergranular embrittlement of the tungsten.     

Study on the α2/γ interfacial structures in a two-phase (α2?+?γ) alloy deformed at elevated temperature

The details of structure modification on ₂/ interface induced by deformation in a hot-deformed Ti-45Al-10Nb alloy were investigated by conventional and high-resolution transmission electron microscopy. A new type of dislocation ledge containing 1/3[111] partials was identified. The Burgers vectors of these dislocation ledges were determined to be 1/2[110] or 1/2101]. The formation mechanism of this new type of dislocation ledge is discussed. Also, two types of hot deformation induced ₂/ interfaces, coherent interfaces with high density of ledges and misoriented semi-coherent ₂/ interfacial boundaries were observed. For the misoriented semi-coherent ₂ interfaces, the density of dislocation ledges in these interfaces increases with the misoriented angle between the (111) and (0001) planes, and 1/3[111] partial dislocations were involved in all the dislocation ledges. The formation mechanism of these deformation-induced ₂/ interfaces were discussed related to the role of ₂/ interfaces adjusting the deformation as a dislocation sink absorbing the slipping dislocations in the phase. Moreover, misoriented semi-coherent ₂ interface related deformation twinning and structure transformation induced by deformation were analyzed and discussed related to the role of ₂/ interfaces as a dislocation source during deformation.     

Magnetic field dependence of the density of states of YBa2Cu3O6.95: Implications for the vortex structure

The total specific heat of YBa₂Cu₃O_6.95 single crystals includes contributions from phonons and spin-1/2 particles, as well as electronic contributions. The electronic specific heat is described by a quadratic term T² in zero field and a linear term [(0)+(H)]T which is increased when a magnetic field H is applied perpendicular to the CuO₂ planes. In agreement with d-wave superconductivity, we find that _n/T_c and (H)_n(H/H_c2)^1/2, where _n is the coefficient of the normal-state linear term. The H^1/2 dependence of the density of states at the Fermi level was predicted by G. Volovik for lines of nodes in the gap: the quasiparticles which contribute to this density of states are close to the nodes in momentum space and are located outside the vortex core.     

Heat Inputs to Sub-mK Temperature Cryostats and Experiments from γ-Radiation and Cosmic Ray Muons

We measured the spectrum of energies deposited by -radiation, emanating from radioactive materials in the laboratory that houses our mK cryostat, and by cosmic ray muons. This allows us to quantify the heat input that adversely affects the lowest temperature accessible in sub-mK experiments. We use our nuclear stage, stage plate and experimental cell as a prototype model system, and calculate the power deposited due to low energy (below 2.65 MeV) background radiation quanta (~20 pW). This is significantly less than the power (~120 pW) deposited in the nuclear and experimental stages by muons. Installation of a 5 cm thick lead wall around the cryostat reduced the energy due to the flux of quanta by a factor of ~10 to ~2 pW, and the number of quanta by a factor of ~20. The lower energy, soft cosmic ray component was also affected by introducing the same thickness of lead, reducing the overall count of cosmic ray derived particles by ~15% and the heat leak to ~100 pW.     

Electronic specific heat of La2−xSrxCu1−yMyO4(M=Ga,Zn): Impurity effects on a D-wave superconductor

The electronic specific heat C_el was studied in Ga- and Zn-doped La_2–xSr_xCuO₄ (0.16x0.22) at T10K. Partial substitution of Ga or Zn for Cu suppresses T_c and revives the T-linear electronic specific heat, T, markedly. The (y)/n vs T_c/T_c0 relation for Zn-doped samples with x0.2 is in good agreement with the theoretical one for resonant impurity scattering in a d-wave superconductor, while those for Ga-doped samples and for Zn-doped samples with x 0.2 deviate slightly from the theoretical curve. The deviation will be discussed in relation to changes in the magnetic properties of 3d electrons.