In the development of high temperature intermetallics involving various aluminides, suicides and Laves phases, it has become evident that it is essential to consider the strong influence of materials processing throughout all stages. The underlying basis for alloy synthesis, processing and the assessment of thermal stability is established by the relevant phase equilibria, the characteristic diffusivities and the possible solidification reaction pathways. In almost all cases the microstructures of the most useful metallic alloys are multiphase assemblies in which the relative phase fractions, compositions and morphologies play key roles in optimizing the performance under high temperature conditions. The microstructure designs are usually tailored for strength, toughness, creep resistance and environmental stability and involve a balance of features derived from mixtures of a ductile phase and intermetallic phases. There is a clear experience that the level of materials processing can only be as sophisticated as the level of knowledge of the phase equilibria and the underlying kinetics. In many of the contemporary intermetallic alloys the phase stability must be considered in terms of multicomponent equilibria and non-stoichiometric intermetallic compositions. Recent developments in several important intermetallic alloy classes illustrate the guidance into alloy design and processing options provided by systematic studies of phase stability.

The Ni3Al-based alloys have been under development at the Oak Ridge National Laboratory (ORNL) and other research institutions in the United States and around the world for the last ten years. The incremental developments of composition, melting process, casting methods, property data, corrosion data, weldability development, and prototype component testing under production-like operating conditions have pushed the ORNL-developed Ni3Al-based alloys closer to commercialization. This paper will present the highlights of incremental technical developments along with the approach and current status of commercialization. It is concluded that cast components are the primary applications of Ni3Al-based alloys, and applications range from heat-treating fixtures to forging dies. It is also concluded that the commercialization process is accelerated when technology is licensed to an organization that can produce the alloy, has component manufacturing capability, and is also a user.

Intermetallic γ-TiAl based alloys (”γ-alloys”) have a great potential to become important materials for advanced applications in aerospace, automotive and related industries. Research and development on γ-alloys have progressed significantly within the last decade. This research has led to a better understanding of the fundamental correlations between alloy composition and microstructure, processing behaviour and mechanical properties. This paper describes the progress in sheet rolling of γ-TiAl based alloys on industrial scale. Employing an advanced hot-rolling process sheets with lengths >1000 mm have been rolled. Furthermore, first results of foil rolling are presented. The mechanical properties of γ-TiAl sheet material with regard to processing route, alloy composition and microstructure are summarized and discussed. Sheet forming by means of superplastic forming and conventional metal forming techniques has successfully been conducted. Different joining techniques have been studied for γ-alloys including solid-state diffusion bonding. The oxidation resistance of γ-alloys is higher than that of Ti-alloys, however, for long-term applications at temperatures >700°C the need for reliable oxidation protective coatings is anticipated. Recent results of cyclic oxidation tests on coated γ-TiAl sheet are presented. Finally, the results of a stability test conducted on a γ-TiAl panel at 750°C are summarized.

Initial microstructure dependence of compactibility at elevated temperature in rapidly solidified Ti-rich TiAl alloy powders produced by plasma rotating electrode process (PREP) has been investigated. There were two kinds of powders with respect to the microstructure. The first one had a surface relief of a martensitic phase, which was referred as M powder. The second one had a dendritic structure, which was referred as D powder. α2+γ microduplex and α2/γ lamellar structures were formed in Mand D powders of the Ti-40 at%Al alloy by heat treatment at 1273 K, respectively. The microduplex structure consisted of γ precipitate in the twin related α2 matrix with the usual orientation relationship. It was difficult to compact the D powder by hot pressing at 1273 K under 50 MPa for 14.4 ks. On the other hand, the M powder was compacted easily by hot pressing with the same condition. The twin related α2 and α2 boundary changed to random ones and the α2 and γ phases were lost the usual orientation relationship in the duplex structure during the hot pressing. In other words, the low energy boundaries were changed to the high energy ones suitable for grain boundary sliding. Dislocations were scarcely observed inside of both the α2 and γ crystal grains. It was concluded that the grain boundary sliding was a predominant deformation mode in the M powder during the hot pressing. D and M powders in Ti-45 and 47 at%Al alloys showed the same tendency as those in Ti-40 at%Al alloy during hot pressing.

With a data base now available on the microstructural characteristics and the deformation, fracture and macroscopic flow behavior of polysynthetically twinned (PST) crystals of γ/α2 TiAl-base alloys, an approach to achieve a good combination of strength, ductility and toughness in γ/α2 TiAl-base alloys was proposed using directional solidification (DS) techniques to produce a columnar grain material with the lamellar orientation aligned parallel to the growth direction. Such alignment of the lamellar microstructure was recently accomplished in γ/α2 TiAl-base alloys of near equiatomic compositions using an appropriately oriented seed crystal from the Ti-Al-Si system.

At the same time, bi-PST crystals, each containing a planar boundary parallel to the loading axis were prepared by directional solidification and diffusion bonding of two PST crystals. Such bi-PST crystals were deformed in tension at room temperature and their deformation behavior was examined in terms of the compatibility requirements imposed at the grain boundary and the interaction of the two component PST crystals.

In this paper, (i) the current status of our DS processing efforts, (ii) some results of microscopic characterization of grain boundaries in diffusion bonded bi-PST crystals and (iii) results of deformation experiments of bi-PST crystals prepared by DS processing and diffusion bonding, will be reported.

Tensile properties of a two-phase γ titanium aluminide with duplex microstructure are tested under different strain rates from 5×10-5 to 5×10-3S-1 at temperature from 1123K to 1273K. It is found that there exists approximate linear relationship between the flow stresses and the logarithm of the strain rate at different temperatures. The strain rate sensitivity can be explained by thermal activation theory, and dislocation climbing is identified as the rate controlling mechanism

For improving the room temperature tensile ductility of direct-cast gamma TiAl sheets without affecting their high-temperature strength, direct sheet casting with T1B2 particle dispersion is employed and conducted. The T1B2 addition and rapid cooling results in the formation of a fine equiaxed grain microstructure with an average grain size of ∼10μm, contributing to the increase in the room temperature ductility to 2.1% with the high-temperature tensile strength kept at about 200MPa. This improvement of room-temperature ductility is attributable to the following fact. The high oxygen content of this material, about 2500wt. ppm, is not harmful to the tensile ductility when the oxygen is in the solid solution of the 0:2 lamellar phase or in oxide particles, which are fine enough not to cause brittleness to the matrix. From these findings, a principle is proposed that oxygen is not harmful to the ductility of gamma TiAl when its microstructure containing oxygen is fine enough.

A two-phase titanium aluminide alloy was systematically doped with carbon to improve its high temperature strength. Solid solutions and precipitates of carbon were formed by different thermal treatments. A fine dispersion of perovskite precipitates was found to be very effective for improving the high temperature strength and creep resistance of the material. The strengthening mechanisms were characterized by flow stresses and activation parameters. The investigations were accompanied by electron microscope observation of the defect structure which was generated during deformation. Special attention was paid on the interaction mechanisms of perfect and twinning dislocations with the carbide precipitates.

The objective of this study is to identify key microstructural parameters which control the mechanical properties of two-phase γ-TiAl alloys with lamellar structures. TiAl alloys with the base composition of Ti-47Al-2Cr-2Nb (at. %) were prepared by arc melting and drop casting, followed by hot extrusion at temperatures above the oc-transus temperature, Tα. The hot extruded materials were then heat treated at various temperatures above and below Tα in order to control microstructural features in these lamellar structures. The mechanical properties of these alloys were determined by tensile testing at temperatures to 1000° C. The tensile elongation at room temperature is strongly dependent on grain size, showing an increase in ductility with decreasing grain size. The strength at room and elevated temperatures is sensitive to interlamellar spacing, showing an increase in strength with decreasing lamellar spacing. Hall-Petch relationships hold well for the yield strength at room and elevated temperatures and for the tensile elongation at room temperature. Tensile elongations of about 5% and yield strengths around 900 MPa are achieved by controlling both colony size and interlamellar spacing. The mechanical properties of the TiAl alloys with controlled lamellar structures produced directly by hot extrusion are much superior to those produced by conventional thermomechanical treatments.

The alloying effect of vanadium upon σ-phase titanium trialuminide has been investigated using materials whose compositions were of the type Al3(Ti,V). Six types of ternary aluminum-titanium-vanadium alloys, ranging from Al3Ti to Al3V at 5 atomic % intervals, have been prepared by arc melting. All the materials showed the D022 tetragonal structure, suggesting vanadium atoms substitute titanium atoms. The 0.2% proof stress increased with increasing vanadium content up to about 10 atomic %, and then decreased toward that of Al3V both at room temperature and at elevated temperatures. Such behavior can be interpreted as substitutional solid solution strengthening.

Transmission electron microscopy (TEM) was used to study the phase transformation in an alloy containing 33Ti-27Nb-40Al (at.%). The results showed that the BCC β phase was present at high temperatures, which ordered to the B2 phase, and finally was martensitically transformed to a plate microstructure during quenching. The plates possessed an orthorhombic crystal structure and a substructure that consisted of both coarse and fine anti-phase domain boundaries (APDBs). These APDBs were consistent with three sublattices that were derived from the inherited site occupancy of the B2 matrix and a subsequent disorder to order transition. The CBED analysis of the plates showed that the site occupancy of this orthorhombic phase was consistent with the Al2NbTi stoichiometry with Al occupying the 8g, Nb the 4c1, and Ti the 4c2 Wyckoff sites.

In an effort to expand the composition range over which Al3Ti is stable, various amounts of niobium were substituted for titanium and processed by melt-spinning. Several samples were annealed both at 600°C and 1000°C for 24 hours. The effects of processing parameters such as wheel speed, the amount of niobium, and annealing temperatures on the structure were investigated by XRD and EXAFS. XRD showed that for all the samples the only structure present was DO22-The DO22 structure was stable even after the high temperature heat treatments. By means of EXAFS, niobium atoms were observed to occupy titanium sites in the DO22 structure. Furthermore, in the unannealed samples, increasing wheel speed of the melt spinning process or the niobium concentration tended to distort the crystal structure. It was observed that Ti EXAFS had different results from the Nb EXAFS beyond their occupying similar sites, which suggested there may exist some composition zones, i.e. rich Nb zone or rich Ti zones, although the structures present were still DO22. The samples were found to experience different distortions as a function of annealing temperatures.

This paper is an inquiry into the relationship between the yield stress and the two length parameters in the fully-lamellar polycrystalline microstructure, the grain-size dCB and the lamellar thickness dLM. Deformation in the multilayer structure is assumed to proceed by dislocations propagating in the formation of a succession of mutually interacting pileups, blocked at the lamellar interfaces and piled-up ultimately against the grain boundary. An important case suggested is a yield stress independent of the grain size, sensitive only to the lamellar spacing.

Polycrystalline stoichiometric Al2Ti was produced via casting or powder metallurgy and further processed yielding material in six conditions. The fracture toughness of the six material conditions was determined from the critical load to initiate cracks with a Vickers indenter. The results show a strong dependence on material condition. Powder processed Al2Ti exhibits the highest fracture toughness value among the material conditions studied.

Polycrystalline non-stoichiometric Al2±yTi1±y and ternary-alloyed Al2Ti + X were prepared in as-cast and cast & annealed conditions. Each material condition exhibited a multiphase microstructure. The composition of the phases present in each alloy was analyzed with SEM/EDS. Fracture toughness values of cast & annealed stoichiometric and non-stoichiometric binary alloys are 20–30% greater than as-cast stoichiometric Al2Ti. For the ternary alloys, the fracture toughness values show a strong dependence on the ternary element used and heat treatment condition. The fracture toughness values of three hot forged ternary alloys were also determined.

Fracture toughness vs. temperature of the cubic (L12), Mn- modified titanium trialuminide (based on Al3Ti) was investigated in air at the temperature range up to 1000°C. Toughness calculated from the maximum load exhibits a broad peak (KQ≈7–10 MPara0,5) at the 200- 500°C temperature range and then decreases with increasing temperature, reaching a room temperature value of ∼4.5 MPam0.5 at 1000°C. However, the work of fracture (γWOF, J/m2) and the stress intensity factor calculated from it (KIWOF) increases continuously with increasing temperature. Fracture modes exhibit a gradual transition from transgranular cleavage at room temperature to predominantly intergranular failure at the 800- 1000°C range.

A range of TiAl-based alloys have been produced by plasma melting either small buttons (1kg samples) or ingots (up to 50kg). Some of the ingots have been atomised. The influence of thermomechanical processing on the microstructure of these materials has been assessed using optical and electron microscopy and the room temperature mechanical properties and creep strengths determined. It has been found that either through appropriate processing and/or through alloy development, it is possible to obtain alloys with room temperature strengths up to 1000MPa. Elongations of about 1% at room temperature have been obtained for alloys with this strength and this is coupled with significant improvements in creep strength over the reference alloy, Ti-48Al-2Mn-2Nb. The influence of the difficulty of slip transfer between gamma and alpha 2 has been assessed as one of the factors limiting ductility. Regions which are low in aluminium, which are present in the atomised powders initiate fracture at very low strains. These results are discussed in terms of the factors that control the strength and fracture behaviour of TiAl-based alloys.

Microstructural development of an extremely fine α2-Ti3Al / γ-TiAl lamellar structure, which was formed by ice water quenching after solution-treatment in a high-temperature α-Ti phase field for a long period of time, was examined during isothermal aging treatment. In an as-quenched Ti-48at.%Al alloy, the massively transformed γ (γm) and untransformed (meaning massively untransformed) fine α2/γ lamellar regions were observed. Fine γ grains, which were similar to γm, were generated both within the fine α2/γ lamellae and at the boundary area between the γm and the fine α2/γ lamellar regions by aging at a low-temperature (1173K) for a short time (180s). Further aging (1.8ks) caused the coarsening of these newly generated fine γ grains. On the other hand, the coarsening of the γ grains occurred by a high-temperature (1323K) aging treatment even for 180s. Fine α2 plates and particles, which were aligned to a particular direction, were observed in the γ grain interiors, indicating that the newly generated γ grains grew at the expense of the fine α2/γ lamellae. It can be considered that the γ grain formation through the fine α2/γ lamellae is closely related to the α2→γ reaction of the α2 plates sandwiched by the γ plates, and needs the fast heating rate enough to overcome the α2/γ → γ/γ lamellae reaction.

At room temperature sheets of γ-TiAl exhibit a higher yield stress in the rolling direction than in the transverse direction. Around 700°C the opposite behavior is observed. The texture mainly consists of a modified cube component. The tetragonal c-axis (001) is aligned in the sheet plane transversely to the rolling direction. Taken into account this special texture and the single crystal yield surface of γ-TiAl we conclude that around 700°C the CRSS of super-dislocations is higher than the CRSS of ordinary dislocations. At RT the relation changes to the opposite.

The alloy Ti-48.6Al-l.9Cr-l.9Nb-IB with an equiaxed γ microstructure, obtained by heat treatment at 1200°C for 4 h, and with a lamellar mi ero structure, obtained by heat treatment at 1380°C for 1 h, is characterized by compression tests and transmission electron microscopy. A lower activity of superdislocations and a more frequent pinning of ordinary dislocations are detected in the lamellar Ti-Al specimens in comparison with the non-lamellar ones during deformation at room temperature. The activity of superdislocations and the pinning of ordinary dislocations are responsible for the differences in yield stress and brittleness between lamellar and non-lamellar Ti-Al. A very high density of ordinary interfacial dislocations is found in the lamellar structure. These influence the activity of superdislocations and the pinning of ordinary dislocations. At high temperature a change in the deformation mechanism occurs. Above the brittle-to-ductile transition, the material is remarkably softer and the mechanical properties are insensitive to the presence of the lamellar interfaces.

Nanocrystalline TiAl powder was formed by the modified HDDR (hydrogenation-disproportion-dehydrogenaton-recombination) method utilizing ball milling in a hydrogen atmosphere. That is, TiAl compound powder decomposed into TiH2 and Al-rich TiAl powders by mechanical grinding in a hydrogen atmosphere (HD process). Dehydrogenaton-recombination (realloying) resulted in the formation of nanocrystalline TiAl powder when heated to about 700 K in an argon atmosphere (DR process). Almost fully dense nanocrystalline TiAl compacts were prepared by a combination of HDDR and hot-pressing at 873 K which is lower than the usual consolidation temperature by about 300 K. The TiAl compact thus made was brittle in the as-pressed state but showed compressive ductility after annealing.