Papers by Author: Florian Pyczak

Abstract: Either at higher temperatures or when a certain alloying element content is exceeded, γ-TiAl alloys contain the β phase (bcc) or its ordered derivate β_o (B2). The relatively soft β phase can facilitate hot deformation, but β_o is detrimental for creep strength and ductility. Thus, knowledge about β_o→β phase transformation is desirable. Surprisingly, even for the binary Ti-Al system it is under discussion whether the ordered β_o phase exists. Also, the effect of alloying elements on the β phase ordering is still unclear. In the present work the ordering of the β phase in binary Ti-(39,42,45)Al and ternary Ti-42Al-2X alloys (X=Fe, Cr, Nb, Ta, Mo) which was experimentally investigated by neutron and high energy X-ray diffraction is compared with the results of first principles calculations using density functional theory. Except for Cr the experimentally determined and the predicted behavior correspond.

Abstract: Metal Matrix Composites (MMCs) are known for their remarkable properties, by combining materials from different classes. Ni-based MMCs are a promising group of heat-resistant materials, targeting aerospace applications. A discontinuously reinforced Inconel X-750/TiC 15 vol.% MMC was proposed for use in lighter, creep resistant turbine elements, with the aim to endure service temperatures up to 1073 K (800 °C). However, their microstructural stability at high temperatures for long periods of time remained to be further investigated. To address this need, specimens were produced by both conventional hot pressing and spark plasma sintering, using powders milled by low and high energy processes, followed by long isothermal aging. The treatments were conducted at 973 and 1073 K, for times between 50 and 1000 hours. The resulting samples were investigated with XRD and EDS techniques for phase analysis. In addition, measurements of hardness were made to monitor changes in mechanical behavior. It was found that, for each different manufacturing process, the amount, distribution and size of γ’ and other precipitates notably vary during the overaging process. Consequently, the amount of elements kept in solid solution also shifted with time. Furthermore, the study shows how distinct initial microstructures, resulting from diverse fabrication processes, differently impact the microstructural stability over long times of exposure to high temperatures.

Abstract: TiAl alloys are increasingly used as a lightweight material, for example in aero engines, which also leads to the requirement for suitable repair techniques. Transient liquid phase bonding is a promising method for the closure of cracks (in non-critical or non-highly loaded areas). The brazing solder Ti-24Ni was investigated for brazing the alloy Ti-45Al-5Nb-0.2B-0.2C (in at. %). After brazing, the joint exhibits different microstructures and phase compositions. The transient liquid phase bonding process was investigated in the middle of the joint region in situ to acquire time resolved information of the phases, their development, and thus the brazing process. These investigations were performed using high-energy X-ray diffraction at the “High-Energy Materials Science” beamline HEMS, located at the synchrotron radiation facility PETRA III at DESY in Hamburg, Germany. For this, we used an induction furnace, which is briefly described here. During the analysis of the diffraction data with Rietveld refinement, the amount of liquid was refined with Gaussian peaks and thus could be quantified. Furthermore, while brazing four different phases occurred in the middle of the joint region over time. Additionally, the degree of ordering of the β_o phase was determined with two ideal stoichiometric phases (completely ordered and disordered). Altogether, the phase composition changed clearly over the first six hours of the brazing process.

Abstract: Titanium aluminides based on the L1₀ ordered g-phase are promising structural light-weight materials for applications in aircraft engines. Typical compositions for γ-TiAl alloys lie in the range Ti-(44-48)Al (at.-%). For high creep resistance, a two-phase microstructure based on lamellar (α₂+γ)-colonies is desirable that may be tuned towards better ductility by introducing pure γ-grains (near lamellar or duplex microstructure).γ-TiAl alloys are often alloyed with niobium for increased oxidation resistance and improved mechanical properties. HEXRD and TEM studies of the alloy Ti-42Al-8.5Nb revealed that the orthorhombic O-phase forms during annealing at 500-650°C. This orthorhombic phase has been known in Nb-rich, Al-lean, α₂-based Ti-aluminides since the late 1980ies (Nb> 12.5 at.-%, Al< 31 at.-%) but the finding in γ-based alloys is new.TEM imaging showed that the O-phase is located within α₂ lamellae of lamellar (α₂+γ)-colonies. O-phase domains and α₂ phase form small columnar crystallites based in the α₂/γ interface. The columnar crystallites grow parallel to the [0001] direction of the α₂ phase and appear as facets when observed along this direction. The evolution of domains and facets with annealing time and the chemical homogeneity of the phases are investigated.The results of STEM imaging show that O-phase domains form during annealing at 550 °C for 8hours or 168 hours. After 168 hours of annealing Nb segregations are observed by EDX mapping within O-phase domains. In comparison, no segregation of niobium is detected after 8 hours of annealing.

Abstract: One strategy to make PM titanium components competitive in terms of mechanical properties is the addition of suitable alloying elements. PM offers the possibility to adapt the alloy composition in order to achieve the required properties. In this study, different alloying elements were introduced into α/β titanium alloys and fatigue behaviour was evaluated. Four-point bending fatigue tests with a stress ratio of 0.2 were performed on specimens manufactured by metal injection moulding (MIM) and shot peening. Results showed an enhanced sintering activity of Ti-6Al-7Nb by adding small amounts of iron. The impact on fatigue properties was evaluated. The increase of oxygen in Ti-6Al-7Nb from 0.15 wt.% to 0.45 wt.% caused a decrease in elongation from 16% to 6%. However the fatigue strength at 10⁷ cycles is just slightly reduced from 450 to 350 MPa. The addition of 0.5 wt.% yttrium powder to gas atomized Ti‑6Al‑4V powder led to a noticeable refinement of the microstructure of the sintered parts, due to the formation of Y₂O₃ particles, which hinder grain growth. In spite of a slightly higher residual porosity, the microstructural refinement increased the fatigue strength at 10⁷ cycles from 450 to 470 MPa. At 10⁶ cycles, the fatigue strength increased even from 705 to 765 MPa. The addition of yttrium did not result in a higher oxygen pick up, which indicates a scavenging of oxygen from the titanium matrix by formation of Y₂O₃ during sintering. Contrary to the fatigue strength results, the scavenging effect led to a decrease in tensile strength of about 70 MPa. The microstructure of fatigue-tested specimens was characterized by using optical and scanning electron microscopy.

Abstract: Ni-based superalloys, in both single and polycrystalline varieties, are extensively used in high pressure turbine blades. But contrary to single crystal variants, the polycrystalline forms present easier manufacturing and offer higher potential for improvement in metal matrix composites (MMCs). To benefit from this opportunity, an Inconel X-750 superalloy reinforced with TiC particles is proposed, having a polycrystalline microstructure and the possibility for weight reduction in turbine elements application. The metallic powder with an addition of 15 vol.% of 3.7 μm_d TiC particles was prepared through low energy mixing, uniaxial pressing and sintering, followed by a triple heat treatment. The microstructure was analyzed with SEM and XRD techniques. Compressive creep tests were performed at 800 °C with 200 MPa, on both original and reinforced alloys. The study shows how the inclusion of a highly compatible particle reinforcement does not only improves the creep resistance, but also reduces the material weight, thus having potential to promote further reduction in the creep rate on turbine blades submitted to centripetal forces.

Abstract: In powder metallurgical processing the sintering process, as well as heat treatments, can drastically influence microstructure formation. In the case of γ-titanium aluminides, it is critical to achieve certain microstructure parameters, such as colony size, porosity and grain boundary morphology in order to obtain appropriate mechanical properties. In this study, the effect of a heat treatment implemented after sintering with the objective of varying the colony size was investigated. Specimens of Ti-45Al-5Nb-0.2B-0.2C prepared by metal injection moulding and uniaxial pressing of feedstock were used to evaluate the tensile and creep properties. Heat treatments conducted at 1350 and 1400 °C for 3 h led to colony sizes of approximately 100 and 200 μm, respectively. Classically, there is an inverse relationship between grain size and creep resistance, nonetheless, for γ-titanium aluminides, the morphology of the colony boundaries was also found to play a role. The larger colony sizes achieved with the heat treatments did not improve the primary creep resistance, which was explained by the change in the morphology of the colony boundaries as they became larger.

Abstract: One of the challenges in PM Ti alloys is to control the impurities level. Oxygen affects the microstructure and the mechanical properties of titanium alloys. Ti-6Al-7Nb is a promising alloy to use in PM due to its outstanding biocompatibility and mechanical properties required for load bearing medical implants. In this work, the influence of the impurities content on the ductility, fatigue resistance and microstructure of Ti-6Al-7Nb alloy processed by metal injection moulding was examined. Tensile and fatigue specimens were manufactured using Ti-6Al-7Nb gas atomized powder. Depending on the thermal treatment time, various oxygen contents were introduced into the specimens. The resulting oxygen content was determined by melt extraction technique. Tensile tests and high cycle four-point bending fatigue tests at room temperature were performed. First studies about the effect of oxygen content on crack initiation and propagation were done by the observation of microstructures and fractured surfaces using light and electron microscopy (SEM).

Abstract: Gas-atomised spherical powders of Ti-45Al-5Nb and Ti-45Al-10Nb alloys were produced using the plasma melting induction guided gas atomisation (PIGA) technique. The phase composition was determined by X-ray diffraction at the synchrotron beamline HEMS at PETRA III (DESY), as well as by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), two dimensional and focused ion beam (FIB) based three dimensional electron back scatter diffraction (EBSD) measurements. Due to the high cooling rates the alloy composition of both alloys consists of hexagonal-close-packed α- and body-centred-cubic β-phase. The α-phase is dominant in the larger powder size fractions. Considerable amounts of the β phase were only found in the powder particle size fractions smaller than 32 μm for the Ti-45Al-5Nballoy and smaller than 45 μm for the Ti-45Al-10Nb. A pronounced dendritic cauliflower-like structure was observed in bigger powder particles of the Ti-45Al-10Nb alloy. This gives proof that diffusion took place during the initial β-grain formation, even though there is no orientation relation between the final grain and the dendrite structure in the powder particles. The presence of dendritic structures showed that the cooling rate during powder atomization was still too low to reach the critical growth rate for a planar solidification. The absence of preferred misorientation angles between α-grains indicates that α-grains are not formed out of already solidified β-grains by a solid state phase transformation.

Abstract: In recent years intermetallic γ-TiAl based alloys with additional amounts of the ternary bcc β Ti(Al,Nb) phase attracted increasing attention due to their improved workability at elevated temperatures. Depending on alloy composition and heat treatment the ductile high-temperature β phase can transform to several ordered phases at lower temperatures. However, currently available phase diagrams of these multiphase alloys are quite uncertain and the precipitation kinetics of some metastable phases is far from understood. In the present study various transformation pathways of the third phase were observed in situ by means of high-energy X-ray diffraction using synchrotron radiation. A Ti-45Al-10Nb (at.%) specimen was subjected to a temperature ramp of repeated heating cycles (700 °C - 1100 °C) with subsequent quenching at different rates. Depending on the quenching rate reversible transformations of the B2-ordered β_o phase to different ω-related phases were observed. The results indicate that the complete transformation from β_o to hexagonal B8₂-ordered ω_o consists of two steps which are both diffusion controlled but proceed with different velocities.