Microstructural, microhardness and electrochemical properties of heat-treated LENS in-situ synthesized Ti-Al-x(Mo, Si) alloys.

So as to explore the opportunity of property enhancement of TiAl-based alloys, studies of microstructural evolution after processing with heat treatments are to be expected. Therefore, the objective of this present study is to investigate how additions of silicon (Si) and molybdenum (Mo) as alloying elements affects the microstructure, microhardness, corrosion behaviour, and wear properties of Ti-Al-x(Mo, Si) alloys made from constituent elemental powders through in-situ alloying laser engineered net shaping (LENS) technique. The influence of the feed rate of Si powder (0.1 rpm, 0.2 rpm and 0.3 rpm) on Ti-Al-xMo was studied at 0.1 rpm and 0.2 rpm Mo feed rate, respectively. Heat treatment at 1200 °C for 15, 30, and 60 min was performed after LENS in-situ alloying, and furnace cooling (FC) was the final step. The microstructure of the produced alloys was analyzed via Scanning electron microscopy (SEM) fitted with energy dispersive spectroscopy (EDS). Using a tribometer and a potentiodynamic polarization test, the alloys' wear characteristics and corrosion behaviour were studied. Based on the results, it was noticed that microhardness values decrease after heat treatment for all the samples produced. Owing to the combined effects of Mo and Si, both the ßo-TiAl and ζ-Ti5Si3 phases lead to solid precipitation hardening and solution strengthening at the grain boundaries. The XRD analysis confirmed γ, α2, α, ßo and ζ-Ti5Si3 phases occurrence in the as-built alloys. The LENS fabricated alloys demonstrated improved wear properties and marginally change in corrosion behavior after heat treatment.

Electron Beam Powder Bed Fusion of Ti-48Al-2Cr-2Nb Open Porous Scaffold for Biomedical Applications: Process Parameters, Adhesion, and Proliferation of NIH-3T3 Cells.

Titanium aluminide (TiAl)-based intermetallics, especially Ti-48Al-2Cr-2Nb, are a well-established class of materials for producing bulky components using the electron beam powder bed fusion (EB-PBF) process. The biological properties of Ti-48Al-2Cr-2Nb alloy have been rarely investigated, specifically using complex cellular structures. This work investigates the viability and proliferation of NIH-3T3 fibroblasts on Ti-48Al-2Cr-2Nb dodecahedral open scaffolds manufactured by the EB-PBF process. A process parameter optimization is carried out to produce a fully dense part. Then scaffolds are produced and characterized using different techniques, including scanning electron microscopy and X-ray tomography. In vitro viability tests are performed with NIH-3T3 cells after incubation for 1, 4, and 7 days. The results show that Ti-48Al-2Cr-2Nb represents a promising new entry in the biomaterial field.

On the Microstructural Evolution and Cracking Behavior of a Titanium Aluminide Alloy During Selective Laser Melting.

Selective laser melting of Ti-48Al-2Cr-2Nb usually ends up with serious cracking. The cracking mechanism, however, remains elusive. In this study, both bulk samples and samples containing only several layers were prepared and investigated. It is shown that a freshly built layer is dominated by single α2 phase. γ started to form from α2 during subsequent thermal cycling due to reheating effects and its volume fraction increased continuously with increased thermal cycles. The γ phase contains higher geometrically necessary dislocation (GND) density than α2. This could be due to its relatively lower hardness and higher thermal expansion coefficient, which made it easier to deform under stresses. With higher GND and thus probably higher distortion energy, the γ experienced more extensive recrystallization than α2 during reheating. Cracks are more liable to initiate from the interior of α2 or the γ/α2 interfaces, which could be due to incompatible deformation between the two phases.

Microstructure of TiAl Capsules Processed by Electron Beam Powder Bed Fusion Followed by Post-Hot Isostatic Pressing.

The microstructures of intermetallic γ-titanium aluminide (TiAl) alloys are subjected to a certain degree of Al evaporation when processed by electron beam powder bed fusion (EB-PBF). The magnitude of the Al-loss is mainly correlated with the process parameters, and highly energetic parameters produce significant Al evaporation. The Al-loss leads to different microstructures, including the formation of inhomogeneous banded structures, thus negatively affecting its mechanical performance. For this reason, the current work deals with creating EB-PBFed TiAl capsules with the inner part produced using only the pre-heating step and melting parameters with low energetic parameters applying high beam speed from 5000 to 3000 mm/s. This approach is investigated to reduce the Al-loss and microstructure inhomogeneity after hot isostatic pressing (HIP). The results showed that the HIP treatment effectively densified the capsules obtaining a relative density of around 100%. After HIP, the capsules produced with the inner part melted at 3000 mm/s presented a lower area shrinkage (around 6.6%) compared to the capsules produced using only the pre-heating step in the core part (around 20.7%). The different magnitudes of shrinkage derived from different levels of residual porosity consolidated during the HIP process. The HIPed capsules exhibited the presence of previous particle boundaries (PPBs), covered by α2 phases. Notably, applying low energetic parameters to melt the core partially eliminates the particles' surface, thus reducing the PPBs formation. In this case, the capsules melted with low energetic parameters (3000 mm/s) exhibited α2 concentration of 3.5% and an average size of 13 µm compared to the capsules produced with the pre-heating step in the inner part with an α2 around 5.7% and an average size around 23 µm. Moreover, the Al-loss of the capsules was drastically limited, as determined by X-ray fluorescence (XRF) analysis. More in detail, the capsules produced with the pre-heating step reported an atomic percentage of Al of 48.75, while using low energetic melting parameters led to 48.36. This result was interesting, considering that the massive samples produced with standard parameters (so more energetic ones) revealed atomic Al percentage from 48.04 to 47.70. Finally, the recycled small particles showed a higher fraction of α2 phases with respect to the coarse particles, as determined by X-ray diffraction (XRD).

Influence of Combined Heat Treatment and Hot Isostatic Pressure (HT-HIP) on Titanium Aluminide Processed by L-PBF.

Postprocessing is essential for improving titanium aluminide (TiAl) microstructure and part quality after using the laser powder bed fusion (L-PBF) method. It has been reported that Ti-48Al-2Cr-2Nb (%at) processed by L-PBF has internal defects and low fracture toughness. Microstructure control by heat treatment (HT) showed a significant improvement in the ductility of the material. Alternatively, hot isostatic pressing (HIPing) could be applied to reduce the residual stresses and internal defects formed during the L-PBF. Combining the benefits of these two subsequent processes into a single predetermined process is appealing for Ti-48Al-2Cr-2Nb (%at) to minimize cost. This work presents a novel strategy to postprocess L-PBF TiAl by applying combined heat treatment and hot isostatic pressing in one process, namely HT-HIP. The process includes three cycles with different conditions (i.e., temperature, time, and pressure). These conditions were determined to achieve improved part quality and microstructure. The results show that the tensile residual stresses decreased from a peak of 249 MPa in the as-built sample to compressive stresses that peaked at -90 MPa after the HT-HIP process. The number and size of internal defects could be greatly reduced. The defects were transformed into a regular spherical shape, which is good in terms of fatigue strength. Additionally, a duplex microstructure with lamellar α2/γ colonies could be introduced for better ductility. Different levels of duplex microstructure could be achieved along with the process cycles. The grain structure using EBSD analysis showed refined equiaxed grains, which demonstrate better strength after the HT-HIP process. Twinning boundaries were also observed in the HT-HIP sample. The grain orientation tendency to the build direction significantly reduced after the HT-HIP process. The nanoindentation test was applied to evaluate the nanohardness of the as-built and HT-HIP samples. It could be demonstrated that the nanohardness is dependent on the formed phases and lamellar density inside the grains. The mean hardness value was 8.19 GPa for the as-built sample, while it was 5.48 GPa for the HT-HIP sample.

Nanoindentation and Structural Analysis of Sintered TiAl(100-x)-xTaN Composites at Room Temperature.

The nanohardness, elastic modulus, anti-wear, and deformability characteristics of TiAl(100-x)-xTaN composites containing 0, 2, 4, 6, 8, and 10 wt.% of TaN were investigated via nanoindentation technique in the present study. The TiAl(100-x)-xTaN composites were successfully fabricated via the spark plasma sintering technique (SPS). The microstructure and phase formation of the TiAl sample constitute a duplex structure of γ and lamellar colonies, and TiAl2, α-Ti, and TiAl phases, respectively. The addition of TaN results in a complex phase formation and pseudo duplex structure. The depth-sensing indentation evaluation of properties was carried out at an ambient temperature through a Berkovich indenter at a prescribed load of 100 mN and a holding time of 10 s. The nanoindentation result showed that the nanohardness and elastic modulus characteristics increased as the TaN addition increased but exhibited a slight drop when the reinforcement was beyond 8 wt.%. At increasing TaN addition, the yield strain (HEr), yield pressure (H3Er2), and elastic recovery index (WeWt) increased, while the plasticity index (WpWt) and the ratio of plastic and elastic work (RPE) reduced. The best mechanical properties were attained at the 8 wt.%TaN addition.

Optimization of the Dry Turning Process of Ti48Al2Cr2Nb Aluminide Based on the Cutting Tool Configuration.

Titanium aluminides are one of the most promising materials in aeronautical and automotive applications. However, their low machinability makes the processing of these alloys quite difficult under sustainability conditions, specially without lubrication. The current study focuses on the turning process of the Ti48Al2Cr2Nb gamma titanium aluminide under dry conditions. As far as we are aware, dry cutting is the most sustainable feature, although it has not been traditionally applied on titanium aluminides due to the accelerated tool wear that the material promotes. The main novelty of this work consists of providing a simple solution for reducing the tool wear based on the inclination of the cutting insert, what is evaluated in terms of tool wear and tool life, cutting forces, cutting temperature, surface integrity of the machined part, as well as its microhardness and microstructural effects. The results shown here clearly point out a better performance of the machining process. This fact could be understood if we take into consideration that an increment of the clearance angle from 6.3° to 11.6° and 15° increases the tool life by five and six times, respectively, using efficient cutting speeds, whose values have increased by 50% with respect to the original cutting conditions. This improvement is explained according to the reduction in the cutting temperature and friction forces in the flank face of the tool. In addition, the use of uncoated carbide inserts may lead to a better behaviour than the coated ones, considering the results obtained for a PVD TiAlN + AlCr2O3 coated insert herein researched.

Development of TiAl-Si Alloys-A Review.

This paper describes the effect of silicon on the manufacturing process, structure, phase composition, and selected properties of titanium aluminide alloys. The experimental generation of TiAl-Si alloys is composed of titanium aluminide (TiAl, Ti3Al or TiAl3) matrix reinforced by hard and heat-resistant titanium silicides (especially Ti5Si3). The alloys are characterized by wear resistance comparable with tool steels, high hardness, and very good resistance to oxidation at high temperatures (up to 1000 °C), but also low room-temperature ductility, as is typical also for other intermetallic materials. These alloys had been successfully prepared by the means of powder metallurgical routes and melting metallurgy methods.

Er,Cr:YSGG laser surface treatment of gamma titanium aluminide: Scanning electron microscopy-energy-dispersive X-ray spectrometer analysis, wettability and Eikenella corrodens and Aggregatibacter actinomycetemcomitans bacteria count-in vitro study.

Dental implants play an important role in oral health. Titanium dental implants must endure the complex microflora environment of the oral cavity. Moreover, bacterial infections have been considered as one of the most important factors of implant failure. The issue of dental improvement through modification of chemical composition and surface treatment has received considerable critical attention. γ-TiAl as a novo biocompatible material revealed a slower corrosion rate in biological media rather Ti-6Al-4V. The objective of this study is to investigate the effect of Er,Cr:YSGG laser on γ-TiAl in comparison with sandblasted and acid-etched samples as the control groups and machined samples.Wettability, surface roughness, surface topography, scanning electron microscopy-energy dispersive X-ray spectrometer analysis of surface and subsurface of samples were investigated and bacteria counts of two periodontal bacterial strains (Aggregatibacter actinomycetemcomitans and Eikenella corrodens) were evaluated on the Er,Cr:YSGG laser surface-treated sandblasted and acid-etched and machined samples.The results of this investigation show that Er,Cr:YSGG laser surface treatment affects surface roughness, surface topography, wettability, chemical composition of the surface and bacteria count. Scanning electron microscopy-energy dispersive X-ray spectrometer analysis of the sample revealed the increment of titanium and oxygen content and reduction of aluminum content in the surface and subsurface layer. A. actinomycetemcomitans and E. corrodens count were found from the lowest level to highest in the sandblasted and acid-etched samples, laser samples and machined samples, respectively.Using controlled parameters of Er,Cr:YSGG laser ensured no significant adverse alteration. The findings to emerge from this study revealed the significant correlation between microbial count and wettability. Furthermore, the contact angle strongly correlated with surface roughness.

Fabrication of Metal Matrix Composite by Laser Metal Deposition-A New Process Approach by Direct Dry Injection of Nanopowders.

Laser Metal Deposition (LMD) offers new perspectives for the fabrication of metal matrix nanocomposites (MMnCs). Current methods to produce MMnCs by LMD systematically involve the premixing of the nanopowders and the micropowders or require in-situ strategies, thereby restricting the possibilities to adjust the nature, content and location of the nano-reinforcement during printing. The objective of this study is to overcome such restrictions and propose a new process approach by direct injection of nanoparticles into a metallic matrix. Alumina (n-Al2O3) nanoparticles were introduced into a titanium matrix by using two different direct dry injection modes in order to locally increase the hardness. Energy dispersive X-ray spectroscopy (EDS) analyses validate the successful incorporation of the n-Al2O3 at chosen locations. Optical and high resolution transmission electron microscopic (HR-TEM) observations as well as X-ray diffraction (XRD) analyses indicate that n-Al2O3 powders are partly or totally dissolved into the Ti melted pool leading to the in-situ formation of a composite consisting of fine α2 lamellar microstructure within a Ti matrix and a solid solution with oxygen. Mechanical tests show a significant increase in hardness with the increase of injected n-Al2O3 amount. A maximum of 620 HV was measured that is almost 4 times higher than the pure LMD-printed Ti structure.

A New Mechanism of Dynamic Phase Transformations in An Isothermal Forged Beta-Gamma Intermetallic Alloy.

A new mechanism of dynamic phase transformations of α2 ↔ γ in an isothermally forged γ-TiAl-based alloy that occur simultaneously during a short-term exposure at 1000 °C is identified in this study. In the heating process, γ phase significantly decreases through a phase transformation of γ → α2, while new γ lamellae are precipitated in the interior of equiaxed grains of α2 phase through a phase transformation of α2 → γ. The reasons for the presence of these two inverse phase transformations α2 ↔ γ occurring simultaneously are discussed.

Structure Determination of Er Doped Ti-Al-Nb Alloy by Neutron Diffraction Analysis.

Neutron diffraction experiments with both conventional powder diffraction setup and under in-situ compressive loading were conducted to investigate the structural origins of large strength and toughness enhancements in Ti-16Al-27Nb alloy after Er addition. The primary phase is determined to be the ordered B2 structure form, in agreement with the previous electron microscopy study. Lattice strains of {210} and {100} planes were measured as a function of applied stress, and elastic anisotropy was found for both, and strong plastic nonlinearity was discovered for (210) reflection. The grain refinement during plastic deformation was proposed by both the 2D diffraction intensity distribution and SEM observations, while stress-induced martensitic phase transition was not observed in this study. It is believed that the activation of different slip systems and grain refinement might be the structural origin of the novel mechanical properties of this alloy.

In situ synchrotron research of phase formation in mechanically activated 3Ti†+†Al powder composition during high-temperature synthesis under the condition of heating with high-frequency electromagnetic fields.

An in situ synchrotron study of the specific features of the phase formation dynamics in mechanically activated 16 wt% Al + Ti powder composition is described, the high-temperature synthesis being carried out under the condition of high volume inflammation by means of inductive heating. The kinetics of the phase formation were registered with an experimental complex, especially designed, constructed and adjusted for the method of dynamic diffraction analysis in synchrotron radiation beams. It has been experimentally in situ shown that increasing the time of mechanical activation of the initial powder mixture reduces the temperature at which components start to react and the time of realization of the high-temperature synthesis. With the latter set at 1 min of mechanical activation, the temperature of the reaction in the mixture is T = 603°C; at 3 min of mechanical activation, T = 442°C; and at 7 min, T = 359°C. The maximum burning temperatures are: for 1 min of mechanical activation, Tmax = 1080°C; for 3 min, Tmax = 1003°C; and for 7 min, Tmax = 820°C. It was found that formation of both stable compounds Ti3Al, TiAl3, TiAl2, TiAl and metastable phases Ti9Al23, Ti5Al11, Ti2Al5, Ti3Al5 occurs at the stage of primary structure formation, before the system goes to thermal explosion. High-temperature synthesis of a mixture of the studied composition takes place without formation of a liquid phase, in the solid-phase combustion mode. It was found that the increase in the time of mechanical activation of the initial powder mixture contributes to the formation of a product with a dominant content of intermetallic compound Ti3Al. By synthesis of the powder mixture of composition 16 wt% Al + Ti, mechanically activated for 7 min, the content of Ti3Al in the final product was found to be 68%.

Effect of Energy Input on Microstructure and Mechanical Properties of Titanium Aluminide Alloy Fabricated by the Additive Manufacturing Process of Electron Beam Melting.

Titanium aluminides qualify adequately for advanced aero-engine applications in place of conventional nickel based superalloys. The combination of high temperature properties and lower density gives an edge to the titanium aluminide alloys. Nevertheless, challenges remain on how to process these essentially intermetallic alloys in to an actual product. Electron Beam Melting (EBM), an Additive Manufacturing Method, can build complex shaped solid parts from a given feedstock powder, thus overcoming the shortcomings of the conventional processing techniques such as machining and forging. The amount of energy supplied by the electron beam has considerable influence on the final build quality in the EBM process. Energy input is decided by the beam voltage, beam scan speed, beam current, and track offset distance. In the current work, beam current and track offset were varied to reflect three levels of energy input. Microstructural and mechanical properties were evaluated for these samples. The microstructure gradually coarsened from top to bottom along the build direction. Whereas higher energy favored lath microstructure, lower energy tended toward equiaxed grains. Computed tomography analysis revealed a greater amount of porosity in low energy samples. In addition, the lack of bonding defects led to premature failure in the tension test of low energy samples. Increase in energy to a medium level largely cancelled out the porosity, thereby increasing the strength. However, this trend did not continue with the high energy samples. Electron microscopy and X-ray diffraction investigations were carried out to understand this non-linear behavior of the strength in the three samples. Overall, the results of this work suggest that the input energy should be considered primarily whenever any new alloy system has to be processed through the EBM route.

Stable Speckle Patterns for Nano-scale Strain Mapping up to 700 °C.

The digital image correlation (DIC) of speckle patterns obtained by vapour-assisted gold remodelling at 200 - 350 °C has already been used to map plastic strains with submicron resolution. However, it has not so far proved possible to use such patterns for testing at high temperatures. Here we demonstrate how a gold speckle pattern can be made that is stable at 700 °C, to study deformation in a commercial TiAl alloy (Ti-45Al-2Nb-2Mn(at%)-0.8 vol% TiB2). The pattern is made up of a uniformly sized random array of Au islands as small as 15 nm in diameter, depending on reconstruction parameters, with a sufficiently small spacing to be suitable for nano-scale, nDIC, strain mapping at a subset size of 60 × 60 nm2. It can be used at temperatures up to 700 °C for many hours, for high cycle fatigue testing for instance. There is good particle attachment to the substrate. It can withstand ultra-sound cleaning, is thermally stable and has a high atomic number contrast for topography-free backscatter electron imaging.

A Model for Creep and Creep Damage in the γ-Titanium Aluminide Ti-45Al-2Mn-2Nb.

Gamma titanium aluminides (γ-TiAl) display significantly improved high temperature mechanical properties over conventional titanium alloys. Due to their low densities, these alloys are increasingly becoming strong candidates to replace nickel-base superalloys in future gas turbine aeroengine components. To determine the safe operating life of such components, a good understanding of their creep properties is essential. Of particular importance to gas turbine component design is the ability to accurately predict the rate of accumulation of creep strain to ensure that excessive deformation does not occur during the component's service life and to quantify the effects of creep on fatigue life. The theta (θ) projection technique is an illustrative example of a creep curve method which has, in this paper, been utilised to accurately represent the creep behaviour of the γ-TiAl alloy Ti -45Al-2Mn-2Nb. Furthermore, a continuum damage approach based on the θ-projection method has also been used to represent tertiary creep damage and accurately predict creep rupture.