Microstructure and high-temperature mechanical behavior of the NiAl–27 at.% Cr intermetallic composite

A NiAl–27 at.% Cr composite material was prepared by a powder metallurgical route, involving argon atomization and consolidation by hot isostatic pressing at 1350°C for 4 h at 400 MPa. The consolidated material exhibited a fine-grained microstructure consisting of a fine dispersion of Cr particles of about 1.7 μm in a NiAl matrix. The mechanical behavior at temperatures ranging from 650 to 1100°C was investigated by tensile-strain-rate-change tests. Analysis of the strain–stress data with both power law creep and Garofalo’s hyperbolic sine relation shows the transition to a low stress exponent creep regime with decreasing stress and/or increasing testing temperature. The measured activation energy for deformation of 300 kJ/mol is consistent with the activation energy for Ni self-diffusion in Ni–50Al. Experiments with coarse grain sizes established that the creep rate is independent of grain size which suggests that the deformation mechanisms must be associated with the motion of lattice dislocations.     

Study of the martensitic transformation in the Co–9 at % Al alloy

Phase transformations in the Co–9 at % Al have been investigated after slow furnace cooling. It has been shown that the structure and phase composition of the alloy after slow cooling do not correspond to the equilibrium phase diagram of the alloy of this chemical composition. It has been established that the α → ε martensitic transformation does not require overcooling and occurs even during a slow cooling of the alloy. It has been found that the formation of 4H modulated martensite is a specific feature of the binary alloys of cobalt and is not connected with the rate of their cooling. The Curie temperatures for the B2, α, and ε phases have been determined.     

A comparison of the plastic behaviour of Fe3Al and Fe3Si in the temperature range of 300–973 K

The plastic behaviour of Fe₃Al and Fe₃Si is compared in view of the different diffusivities of Fe atoms in these intermetallic phases. In case of Fe₃Al serrated yielding and vanishing strain rate sensitivity (S) in a range of intermediate temperatures (T=400–800 K) indicates some kind of dynamic strain aging effect. In spite of the higher diffusivity of Fe in Fe₃Si, serrations and S ⩽ 0 have been found only in a small temperature interval around 800 K. Possible reasons are discussed using experimental information on the temperature and strain rate dependences of the critical resolved shear stress and on the slip line development measured and observed during compression tests in vacuum (300–973 K) on near stoichiometric Fe₃Al single and polycrystals and Fe₃Si single crystals. In addition the coarsening of D0₃ domains (in case of Fe₃Al) during TEM in situ heating has been observed.     

Metastable phase formation during the decomposition of Fe–20 at.% Mo

The early stages of the isothermal decomposition of an Fe–20 at.% Mo alloy at 500°C have been studied by means of atom-probe (AP) and field-ion microscopy (FIM), as well as high-resolution (HREM) and conventional (CTEM) transmission electron microscopy. CTEM reveals a characteristic modulated structure oriented along the 〈100〉-type directions of the b.c.c. matrix. Electron diffraction patterns show satellite-like intensities close to the fundamental reflections in 〈100〉-type directions, indicating an approximate 6 nm characteristic length scale of the decomposition microstructure. FIM and HREM reveal precipitates about 2 nm in size with a b.c.c. structure formed coherently within the matrix. AP analyses show these precipitates to consist of almost pure Mo. The size misfit between the Mo-rich precipitates and the Fe-rich matrix causes large coherency strains, resulting in precipitate alignment along 〈100〉-type directions. The Mo-rich b.c.c. solid solution precipitates in a metastable equilibrium with the Fe-rich b.c.c. matrix, whereas the formation of the equilibrium intermetallic phases is kinetically suppressed. A coherent metastable miscibility gap between the Fe-rich and the Mo-rich b.c.c. solid solution is assessed by incorporating a continuum elasticity strain-energy term into the Gibbs free energy.     

Reaction-sintering of intermetallic alloys of the Ni–Al–Mo system

A powder metallurgy route has been used for producing binary and ternary alloys of the Ni–Al–Mo system. Elemental powder mixtures were compacted and, then, sintered in a dilatometer. In this way the dimensional changes involved with thermally induced transformations could be followed during continuous heating runs up to the sintering temperatures. Sintering was assisted by the formation of a liquid phase, promoted by the heat output coming from the intermetallic phase formation reactions. The amount of liquid phase and the efficiency of sintering was highly dependent on the heating rate. A threshold value for optimal densification was identified for some compositions. The effect of other processing parameters, such as pre-sintering compaction pressure and sintering atmosphere has been considered too. The characterisation of the final products was mainly based on X-ray diffraction analyses. The microstructural parameters and the phase composition of the sintered materials were evaluated. On the basis of these results it is possible to draw some conclusions concerning the main phenomena occurring during the sintering process.     

Effect of Zn Additions on the Oxidation of Cu–2 at.% Al and Cu–4 at.% Al Alloys in 1 atm O2 at 800 °C

Four ternary Cu–Zn–Al alloys containing 5 or 10 at.% Zn and 2 or 4 at.% Al plus an alloy containing 2 at.% Al and 15 at.% Zn have been oxidized at 800 °C in 1 atm O₂, and their behavior has been compared with that of the corresponding binary Cu–Zn and Cu–Al alloys. For the alloy containing 4 at.% Al, which is already able to form external alumina scales, the addition of Zn is only effective in reducing the mass gain during the fast, initial-oxidation stage. Conversely, the addition of 15 at.% Zn to Cu–2Al is able to prevent the formation of external scales containing mixtures of the Cu and Al oxides, resulting in the formation of external alumina scales after an initial stage of faster rate, producing a limited third-element effect. Finally, the addition of Al to both Cu–5Zn and Cu–10Zn is able to prevent the internal oxidation of Zn, producing a kind of reversed third-element effect. Possible mechanisms for these effects are examined on the basis of general treatments concerning the scaling behavior of ternary alloys.     

Precipitation mechanism of an MoNi type intermetallic phase in W–27.0at.%Mo–35.6at.%Ni–17.6at.%Fe

For W–27.0Mo–35.6Ni–17.6Fe (at.%) sintered at 1500 °C for 240 min, an MoNi type intermetallic phase was formed during cooling, when either a water-quenching or furnace-cooling practice was employed. For the water-quenched specimen, a quasi-eutectic reaction took place, wherein the intermetallic phase precipitated directly from a eutectic liquid phase, which was super-saturated with W and Mo, in the form of a lamellar structure along with the Ni-based matrix phase. Accordingly, the intermetallic phase was located primarily in the interstices between the grains of the Ni-based matrix phase. On the other hand, for the furnace-cooled specimen, the intermetallic phase was formed by the peritectoid reaction between the Ni-based matrix phase and the W–Mo grains. The intermetallic phase thus existed primarily at the boundaries between the Ni-based matrix phase and the W–Mo grains.     

Phases and evolution of microstructures in Ti–60 at.% Al

The formation and stability of Al-rich Ti–Al phases is reviewed and the kinetics of the phase transformations and evolution of lamellar TiAl + r-TiAl₂ microstructures is discussed. For this a couple of Ti–60 at.% Al alloys were processed by different techniques to generate different initial microstructures. The kinetics were studied by annealing the differently processed alloys for 1, 10, 100 and 1000 h at temperatures between 800 and 1000 °C and then analysing the quenched microstructures by optical, scanning electron, and transmission electron microscopy. In addition, in situ heating and cooling experiments using differential thermal analysis and transmission electron microscopy were performed to verify the results obtained for the quenched samples. The results conclusively show why the metastable phases h-TiAl₂ and Ti₃Al₅ form. The stability and transformation of the metastable phases have been determined in dependence on time and temperature and the kinetics of the two different mechanisms by which the stable phase r-TiAl₂ forms have been established. The effects of differing initial microstructures on the evolution of the microstructure with time and temperature are discussed.     

Competitive Effect of Water Vapor and Oxygen on the Oxidation of Fe–5 wt.% Al Alloy at 1073 K

The effect of oxygen on the oxidation of Fe–5wt.% Al alloy was investigated at 1073 K in N2–12.2 vol.% H₂O, O₂–12.2 vol.% H₂O, and N₂–O₂–12.2 vol.% H₂O with various amounts of oxygen. The results showed S-shaped oxidation curves that consisted of three stages: slow-incubation, rapid transition, and relatively slow oxidation. The amount of oxidation increased with increasing oxygen contents up to 0.9 vol.% O₂ and then rapidly decreased. On the oxygen-rich side, a slow incubation oxidation stage was observed and its duration increased with increasing oxygen content. The extent of oxidation decreased gradually with decreasing oxygen content from the critical value and the incubation period disappeared. In the transient period, Fe₂O₃ was formed on the lean oxygen-content side and elongated voids were formed in the outer Fe₃O₄ and FeO layer. It was suggested that the differences in the morphology of Fe₂O₃ formed on the surface affected by the dissociation and gas-transport process due to differences in oxygen partial pressure at the gas–scale interface.     

Phase decomposition of the γ phase in a Mn–30 at.% Cu alloy during aging

The phase decomposition process of γ phase in a Mn–30 at.% Cu alloy, when aged at 723 K from 2 to 50 h, is investigated with electrical resistivity and magnetic susceptibility measurement. In conjunction with the antiferro-magnetic transition of the Mn-rich regions during cooling to room temperature from the aging temperature, the temperature coefficient of electrical resistivity shows a continuous increase in a certain temperature range. The temperature where the coefficient has the maximum increasing rate is defined as the T_N temperature of the Mn-rich regions. It was found that the T_N temperature was 20–30 K higher than the concomitant f.c.c.–f.c.t. transformation temperature T_t, determined with the minima of Young’s modulus in the aged samples. The increment of temperature coefficient of electrical resistivity involved in the magnetic transition is used to estimate the changes of volume fraction for Mn-rich regions vs aging time. At the same time, the paramagnetic feature above the spin-freezing transition temperature for quenched Cu-rich alloys is summarized, and the Mn concentration in Cu-rich regions of aged samples is calculated. It should be noted that Mn and Cu-rich regions had already formed in the 2 h-aged Mn–30 at.% Cu sample, and longer aging further enriched Mn or Cu, while the volume fraction of Mn-rich regions decreased slightly with aging time. Electrical resistivity measurement sensitive to Mn-rich regions and the magnetic susceptibility measurement for Cu-rich regions have shown the compositional heterogeneity in decomposed phases. TEM observation confirms the interconnectivity of the two regions in the aged microstructure. All the results support the hypothesis that the decomposition of γ phase in Mn–Cu alloys proceeds in the spinodal manner.     

Effect of Nb on the high temperature oxidation of Ti–(0–50 at.%)Al

The oxidation behavior of Ti–Nb, Ti₃Al–Nb and TiAl–Nb (Nb: 0–30 at.%) has been investigated at 1173 K in air. When Nb is in solid solution with TiO₂, the addition of Nb can improve the oxidation resistance of the alloys by impeding mass transfer in TiO₂. However, Nb decreases the oxidation resistance when the amount of Nb is too high and forms TiNb₂O₇ or AlNbO₄ phases in the scale.     

Experimental investigation of phase equilibria in the Ru–Fe–Al system at 1473 K

The low-Al part of the ternary Ru–Fe–Al phase diagram at 1473 K is established in this work. Due to the very promising properties of B2 ruthenium aluminide, the investigation of the B2 region of this system is of special interest. The experimental work includes diffusion methods, as well as quenching of annealed single-phase and two-phase alloys. The results of the different methods are in good agreement. Optical and scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction are used to investigate the samples. It is shown in this work that a three-component B2 phase exists over a wide composition range.     

Electrochemical formation of La–Al intermetallic compounds in fluoride melts

The electrochemical formation of La-Al alloys in LiF-CaF₂ molten salt on a molybdenum electrode at 1123 K was investigated by electrochemical techniques,such as cyclic voltammetry,square-wave voltammetry and open-circuit chronopotentiometry.The formation signals of four types of Al-La intermetallic compounds were observed.The Al-La alloy was obtained through galvanostatic electrolysis at 2.5 A·cm^-2 for 3 h.The phase composition and microstructure of the electrolytic product...     

Atom probe tomography investigation of heterogeneous short-range ordering in the ‘komplex’ phase state (K-state) of Fe–18Al (at.%)

We study an Fe–18Al (at.%) alloy after various thermal treatments at different times (24–336 h) and temperatures (250–1100 °C) to determine the nature of the so-called ‘komplex’ phase state (or “K-state”), which is common to other alloy systems having compositions at the boundaries of known order-disorder transitions and is characterised by heterogeneous short-range-ordering (SRO). This has been done by direct observation using atom probe tomography (APT), which reveals that nano-sized, ordered regions/particles do not exist. Also, by employing shell-based analysis of the three-dimensional atomic positions, we have determined chemically sensitive, generalised multicomponent short-range order (GM-SRO) parameters, which are compared with published pairwise SRO parameters derived from bulk, volume-averaged measurement techniques (e.g. X-ray and neutron scattering, Mössbauer spectroscopy) and combined ab-initio and Monte Carlo simulations. This analysis procedure has general relevance for other alloy systems where quantitative chemical-structure evaluation of local atomic environments is required to understand ordering and partial ordering phenomena that affect physical and mechanical properties.     

Theoretical Analysis of Anomalies in High-Temperature Oxidation of Fe–Cr, Fe–Ni, and Fe–Ni–Cr Alloys

The following anomalies are theoretically analyzed: weakening of the protective ability of dense Cr₂O₃ film during its long-term thermal exposure (because of iron oxidation under the film); lowering of the heat resistance of Fe–Cr and Fe–Ni–Cr alloys during the oxidation (800°C) with an increase in the chromium content over 40 at. %; improving of the protective ability of the films formed at Fe–Ni alloys because of nickel oxidation under the dense FeO film; and the internal oxidation of the Fe 30Ni alloys under the FeO films with the internal formation of FeO oxides and spinel of NiFe₂O₄ type. It is shown that these anomalies can be explained, and the composition of the most heat-resistant alloys calculated, if one takes into account that associates with significantly stronger interatomic bonds than those in ideal solutions can form in solid solutions and cause unlimited solubility of the metallic components in each other.     

Growth morphology and crystallography of precipitate in a new high-temperature structural intermetallic Ti–40Al–10Fe

Based on TiAl alloys bearing high levels of Nb, which are prospective high-temperature intermetallics, a new dual-phase alloy (Ti–40Al–10Fe (at%)) with precipitate growth direction close to the slipping plane normal of the matrix was developed. Transmission electron microscopy revealed that the annealed alloy was composed of equiaxed grains of τ₂-TiAl₂Fe and γ-TiAl phases. Aging treatment at 1000 °C produced polygon-shaped γ-TiAl precipitate from the τ₂-TiAl₂Fe matrix. The precipitation reaction of the face-centered cubic structure of τ₂-TiAl₂Fe into the ordered face-centered tetragonal structure of γ-TiAl phase was systematically investigated in terms of crystallographic features, including mutual orientation relationship, growth direction, habit plane, side facets, and interfacial dislocation structure. The observed growth direction <973> was close to the normal of the slip plane {111}, with a discrepancy angle of ∼20°. Thus, the observed two-phase microstructure might significantly improve strengthening. It could also be quantitatively controlled by selection of precipitate and matrix with phase structures and lattice parameters that meet a certain requirement.