The purpose of this research was to characterize the oxidation behavior of several model (TiAl, TiAl-Nb, TiAl-Cr, TiAl-Cr-Nb) and engineering alloys (XD, K5, Alloy 7, WMS) after long-term isothermal exposure (∼7000 h) at 704°C, and after shorter time exposure (∼1000 h) at 800°C in air. High-resolution field emission and microprobe scanning electron microscopy were used to characterize the scales formed on these alloys. Similarities and differences observed in the scales are correlated with the various ternary and quaternary microalloying additions.

L12 modified titanium trialuminides have been prepared by replacing 9at.% of the aluminum in Al3Ti with chromium and/or iron. The materials were recrystallized into single phase polycrystals after isothermal forging resulting in an average grain diameter of about 40μm. Lattice parameter of the material containing 9 at.% chromium or 9 at.% iron, are 0.3959nm and 0.3939nm, respectively. The lattice parameters varied linearly with composition between these values for additions of both chromium and iron. Uniaxial compression tests were performed at temperatures ranging from 293K to 1300K. The yield strength is not sensitive to chemical composition within the range of compositions tested. Flow stress serrations of a few % were observed at temperatures around 600K, where intermittent drops in flow stress started immediately after yielding and continued to the end. These serrations were observed up to about 800K. At 900K and above the materials became fully deformable. Quasi steady state flow and strain softening were observed at 1200K and 1300K, respectively, due to dynamic recrystallization.

The temperature, TP, and the stress, σP, at which the yield stress of γ-TiAl alloys peaks are influenced by factors such as alloy composition and load orientation. Available data indicates that in the absence of adequate heat treatments, TP and σP are shifted towards values significantly higher than those of samples pre-annealed in order to precipitate interstitial atoms. Conditions under which precipitation influences the anomalous regime are revealed by dedicated tests. In addition to pointing out the clear effect of interstitials, these tests suggest that further ordering may contribute to the strength of Al-rich γ-TiAl.

Recent Monte-Carlo simulations of order relaxations in L12-ordered Ni3Al reproduced the simultaneous action of two processes as experimentally observed by residual resistometry. It was shown that the fast process is related to the fast annihilation/creation of nearest neighbour antisite pairs. These findings are now strongly corroborated by a new supercell approach of ab initio quantum mechanical calculations describing the simultaneous displacement of Ni and Al atoms on their way to their respective antisite positions. Studies of single jumps suggest that such a cooperative migration of Ni and Al is necessary in order to prevent Al antisites from jumping back into their regular position. Relaxation of neighbouring atoms was taken into account. Thus, a minimum migration barrier of about 3 eV was derived which together with the calculated formation enthalpy of a Ni vacancy of 1.5 eV amounts to 4.5 eV, in remarkable agreement with the high activation enthalpy of 4.6 eV as observed experimentally.

γ-T1AI (Cr, Mo, Si, B) specimens with two different fine lamellar microstructures were produced by vacuum arc melting followed by a two-stage heat treatment. The average lamellar spacing was determined to be 200 nm and 25–50 nm, respectively. Creep tests at 700°C showed a very strong primary creep for both samples. After annealing for 24 hours at 1000 °C the primary creep for both materials is significantly decreased. The steady-state creep for the specimens with the wider lamellar spacing appears to be similar to the creep behavior prior to annealing while the creep rate of the material with the previously smaller lamellar spacing is significantly higher. Optical microscopy and TEM-studies show that the microstructure of the specimens with the wider lamellar specing is nearly unchanged, whereas the previously finer material was completely recrystallized to a globular microstructure with a low creep resistance. The dissolution of the fine lamellar microstructure was also observed during creep tests at 800 °C as manifested in an acceleration of the creep rate. It is concluded that extremely fine lamellar microstructures come along with a very high dislocation density and internal stresses which causes the observed high primary creep. The microstructure has a composition far away from the thermodynamical equilibrium which leads to a dissolution of the structure even at relatively low temperatures close to the intended operating temperature of γ-T1AI structural parts. As a consequence this limits the benefit of fine lamellar microstructures on the creep behavior.

We have investigated an effect of hydrogen gas-charging on the microstructure and the mechanical property of a Ti-49at.%Al alloy. After hydrogen-charging performed under an atmospheric pressure of hydrogen gas at 1023K for 3 hours, the alloy with γ-single phase has become completely brittle, while this hydrogen-induced embrittlement is suppressed for that with (γ+α2) two-phase microstructure composed of lath-precipitates in the γ matrix. A significant microstructural change was found to occur for the two-phase alloy (approximately 340ppm hydrogen in the alloy); a thin amorphous layers with a few nm thickness appear at the preexisting γ/α2 interfaces in the lath-precipitates after hydrogen-charging. In-situ TEM observation confirmed that the amorphous region transforms to a nano-crystalline state after heating to 1000K at which the hydrogen could be removed (degassed), indicating that the amorphous phase is not a binary Ti-Al phase but a ternary Ti-Al-H one. This, in turn, suggests that the γ/α2 interface in the lath packets act as the most preferential sites for hydrogen storage. Therefore, the scavenging is expected to occur effectively for the microstructure composed of γ-α2 fine lamellae in which a large number of γ/α2 interfaces exist. It is worthwhile mentioning that the fine-scale of the lamellae makes it possible to have a large number of interfaces for a given volume of the α2 phase.

The Knoop microhardness anisotropy of single crystal NiAl, a B2 intermetallic compound, was investigated on the (001) plane at indentation test loads from 25 to 500 g. An energy balance analysis was applied to analyze the indentation size effect (ISE). The load independent, orientation independent Knoop microhardness was determined to be 220 kg/mm2 for the (100) plane of NiAl.

Plastic deformation behavior and substructures in Ni3Nb single crystals were examined focusing on the operative deformation twin systems. Three twinning systems were operative depending on crystal orientation. The twinning behavior was discussed comparing with that in pure hcp metals. Microcracks initiated at the twin intersection. A large number of twin intersections were analyzed and classified into several types.

A preliminary study on the phase relations in Al-Mo-Ti-X quaternary systems in the vicinity of Ti-trialuminide phases is carried out with various additives X= Mn, Cr, Fe, Ni and Ag. In the Al-Mo-Ti ternary system, a bcc-phase field extends from the Ti-Mo edge to high Al region at high temperatures and it equilibrates with a DO22-Al3Ti phase containing a large amount of Mo. It is found that, by additions of X= Mn, Cr, Fe or Ni, an L12-(Al, X)3 Ti phase appears near the two-phase region composed of the DO22-Al3 Ti and bcc phases in the Al-Mo-Ti ternary system. By heat treatment at 1223 K, the bcc phase of quaternary alloys decomposes into the A15-Mo3Al, DO22, L12 and/or σ phases, and no voids are observed. The mechanical properties of these alloys are also investigated by Vickers hardness.

Gas nitridation of TiAl based alloys in an ammonia atmosphere was carried out in the present work. The nitride layers were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The evaluation of the surface hardness and wear resistance was performed to compare with those of the non-nitrided alloys. It is concluded that the nitride layers are composed of Ti2AlN as the inward-growing layer and TiN as the outward-growing layer. The nitridation temperature and time were two major factors influencing the thickness of the nitride layers of the alloys. The high temperature nitridation raised the surface hardness and the wear resistance of the TiAl based alloys markedly. The tribological behaviors of the nitrided alloys were also discussed.

Tungsten (W) doped γ-TiAl is one of promising alloys among many other proposed TiAl base alloys, for the purpose of structural applications at elevated temperatures. Ingots of W doped γ-TiAl were produced by plasma arc melting, followed by homogenizing heat treatment and isothermal forging to control their microstructures. The phase stability of W doped γ-TiAl has been studied quantitatively, using the specimens quenched from 1273 K. Equilibrium compositions of consisting phases were analyzed by means of EDS analysis in a TEM. An isothermal cross section of the Ti-Al-W ternary phase diagram at 1273K has been proposed based on the experimental observations. Small amounts of W addition (< 1at%) to Ti-48at%Al cause a phase shift from α2+γ to α2+β+γ, which suggests that W is the strongest β stabilizer among transition metals, such as Cr and Mo. Mechanical property measurements of W doped γ-TiAl show that the high temperature tensile strength has been improved by the W addition. Relationships between the microstructures and the mechanical properties of W doped γ-TiAl have been discussed.

Minimum creep rates as a function of stress have been obtained for Ti-48Al binary alloy with a near gamma and a fully lamellar microstructure. TEM investigation reveals that deformation structures in both microstructures are dominated by jogged screw 1/2[110] dislocations in γ phase. A modif ied jogged screw model is adopted to predict minimum creep rates where the rate controlling step is assumed to be the non-conservative motion of 1/2[110] unit dislocations. In the case of equiaxed microstructure where the deformation was mostly uniform, the creep rates predicted by this model were in agreement with experimental values. Conversely, deformation in lamellar microstructures were highly inhomogeneous where the density of jogged 1/2[110] unit dislocations were seen in varying proportions depending on the width of the γ laths. The creep rates and stress exponents in these microstructures is explained in terms of active volume fractions of γ laths participating in deformation for a given applied stress.

In view of the possibility of the E21-type intermetallic compound as a strengthener in austenitic alloys at high temperatures, mechanical properties and microstructures of the γ / κ two-phase alloys in the Fe-Mn-Al-C system were investigated. Alloy compositions with more than 1.5wt% C were selected in order to stabilize the γ / κ two-phase microstructure in the high temperature regime exceeding 873K. During furnace cooling after the homogenization treatment, κ phase precipitates on the γ grain boundary, which results in the poor tensile ductility. In these alloys, tensile yield strength at 873K and 1073K increases with increasing κ phase volume fraction. Applying ageing treatment at 1073K after the solid solution treatment followed by water quenching causes the formation of a uniform γ / κ lamellar microstructure, and the remarkable improvement of ductility was achieved. The addition of Cr, which is expected to improve the oxidation resistance, reduces the phase stability of κ phase, and leads to the formation of Cr7C3 carbide and β-Mn phase with more than 5.5wt.% Cr addition.

The high melting temperature and oxidation resistance of the Mo5SiB2 (T2) phase and multiphase microstructures incorporating the T2 phase in the Mo-Si-B system have motivated further studies for applications in very high temperature environments. Since the long term microstructural stability is determined by diffusional processes, diffusion couples consisting of binary boride and silicide phases have been examined in order to evaluate the kinetics of T2 phase development and the relative diffusivities controlling the kinetics. Long term annealing (500 hrs) of the Mo5Si3/Mo2B diffusion couple yields the phase sequence of Mo5Si3/Mo3Si/T2/Mo2B at 1600°C. This indicates that the T2 phase initiates and grows from the Mo2B side to a thickness of about 32μm and the Mo3Si phase initiates and grows from the Mo5Si3 side to a thickness of about 15μm. Other annealing treatments allow for an analysis of the diffusion kinetics based upon the layer thickening and composition profile measurements. To identify the crystallographic growth direction of T2 on Mo2B, a wedge shaped TEM sample with very thin leading edge was prepared. Microstructure images indicate that the growth mode of the T2 phase is columnar. There is a clear tendency for the growth of T2 to be approximately normal to c-axis.

Ir-based refractory superalloys with an fcc and L12 two-phase structure similar to that in Ni-based superalloys but with considerably higher melting temperatures are proposed. First, the microstructure and strength are shown for several kinds of binary alloys. Then, the effect that the third element and the combination of Ni-Al with an fcc and L12 two-phase structure in binary alloys had on the lattice misfit, microstructure, and strength was investigated. The precipitation-hardening effect in Ir-based alloys was investigated and discussed in terms of precipitate morphology and lattice misfit. The creep properties of Ir-based alloys were also investigated.

A Laves phase strengthened NiAl-Ta-Cr alloy (IP 75) has been developed for structural applications in gas turbines as well as in heat exchangers. It has a lower density and a higher thermal conductivity as well as a higher melting point than conventional superalloys. Different methods for alloy production have been established including investment casting (IC) and a powder metallurgical method (PM). Creep properties have been determined in compression and tension. Tension tests up to 10000 hours were performed at 900 °C and 1000 °C for both PM and IC materials. The oxidation behavior of the PM and IC material was studied for up to 1000 hours by thermogravimetry in air at constant temperature between 600 °C and 1300 °C. The results are compared with results obtained from long-term isothermal and cyclic oxidation experiments in air at 1200 °C for 17900 hours. Microstructures and scales were examined by light optical and scanning microscopy, X-ray powder diffraction and electron probe microanalysis.

For applications at ultrahigh temperatures the multiphase microstructural options that can be developed in the Mo-Si-B system have demonstrated an effective and attractive balance of essential characteristics. The coexistence of the high melting point (>2100°C) ternary intermetallic Mo5SiB2 (T2) phase with Mo provides a useful option for in-situ toughening. A further enhancement is available from a precipitation reaction of Mo within the T2 phase that develops due to the temperature dependence of the solubility behavior of the T2 phase. However, direct access to Mo+T2 microstructures is not possible in ingot castings due to solidification segregation reactions that yield nonequilibrium boride and silicide phases with sluggish dissolution. Alternate routes involving rapid solidification of powders are effective in suppressing the segregation induced phases. The processing and microstructure options can also be augmented by selected refractory metal substitutional alloying, such as the incorporation of Nb, that alters the solubility of the T2 phase and the relative phase stability to yield solidification of two phase refractory solid solution + T2 structures directly. The observed alloying trends highlight the role of atomic size in influencing the relative stability of the T2 phase. A key component of the overall microstructural control and long term microstructural stability is determined by the kinetics of diffusional processes. The analysis of selected diffusion couples involving binary boride and silicide phases has been used to assess the relative diffusivities in the T2 phase and coexisting phases over the range of solubility and to provide a basis for the examination of the kinetics of reactions involved in coatings and oxidation.

This paper presents the results of a study of the effects of temperature on fatigue crack growth in Ti-47A1–2Cr-2Mn + 0.8 Vol. %TiB2 gamma titanium aluminide intermetallics. Fatigue crack growth rate data are presented for the cast lamellar microstructure at 25,450 and 750°C. The trends in the fatigue crack growth rate data are explained by considering the combined effects of crack-tip deformation mechanisms and oxide-induced crack closure. Faster fatigue crack growth rates at 450°C are attributed to the high incidence of irreversible deformation-induced twinning, while slower crack growth rates at 700°C are due to increased deformation by slip and the effects of crack-tip shielding provided by oxide-induced wedging, which is analyzed using a modified Dugdale-Barenblatt model.

Intermetallic titanium aluminides based on γ(TiAl) are prone to cleavage fracture on low index lattice planes. Unfavourably oriented grains may therefore provide easy crack paths so that the cracks can rapidly grow to a length which is critical for failure. The effect of crack tip plasticity on crack propagation in γ(TiAl) was investigated by conventional and high-resolution electron microscopy. Crack tip shielding due to mechanical twinning was recognized as toughening mechanism, which occur at the atomic scale and apparently is capable to stabilize fastly growing cracks. The potential of the mechanism will be discussed in the context of novel design concepts for improving the strength properties of γ-base titanium aluminide alloys.

The present study is concerned with the processing, microstructural characterization, mechanical and tribological properties of fine-grained Fe-25Al-10Ti intermetallic alloy. The alloy was synthesized from elemental powders by mechanical alloying in an attritor-type ball milling system for 100 h, followed by hot isostatic pressing (HIP). After HIP treatment at 1073 K under an ultra-high pressure of 980 MPa, fully dense compacts with a grain size of about 200 nm were produced. Mechanical properties were evaluated by compression tests from room temperature to 1073 K. At room temperature, the alloy exhibits yield strength as high as 2.4 GPa, together with considerable rupture strain of 0.16. The yield strength decreases monotonically with increasing test temperature with no positive temperature dependence observed. The grain growth after high temperature deformation is not severe, indicating that the alloy has a relatively high thermal stability. Finally, tribological properties of the alloy were evaluated by using a ball-on-disk type wear tester and compared with those for gray cast iron, a currently used material for automotive brake rotors.