Revealing dynamic processes in laser powder bed fusion with in situ X-ray diffraction at PETRA III.

The high flux combined with the high energy of the monochromatic synchrotron radiation available at modern synchrotron facilities offers vast possibilities for fundamental research on metal processing technologies. Especially in the case of laser powder bed fusion (LPBF), an additive manufacturing technology for the manufacturing of complex-shaped metallic parts, in situ methods are necessary to understand the highly dynamic thermal, mechanical, and metallurgical processes involved in the creation of the parts. At PETRA III, Deutsches Elektronen-Synchrotron, a customized LPBF system featuring all essential functions of an industrial LPBF system, is used for in situ x-ray diffraction research. Three use cases with different experimental setups and research questions are presented to demonstrate research opportunities. First, the influence of substrate pre-heating and a complex scan pattern on the strain and internal stress progression during the manufacturing of Inconel 625 parts is investigated. Second, a study on the nickel-base superalloy CMSX-4 reveals the formation and dissolution of γ' precipitates depending on the scan pattern in different part locations. Third, phase transitions during melting and solidification of an intermetallic γ-TiAl based alloy are examined, and the advantages of using thin platelet-shaped specimens to resolve the phase components are discussed. The presented cases give an overview of in situ x-ray diffraction experiments at PETRA III for research on the LPBF technology and provide information on specific experimental procedures.

Optimization of the Post-Process Heat Treatment Strategy for a Near-α Titanium Base Alloy Produced by Laser Powder Bed Fusion.

During the last decades, titanium alloys have been of great interest for lightweight applications due to their high strength in combination with a low material density. Current research activities focus on the investigation of near-α titanium alloys produced by laser powder bed fusion (LPBF). These alloys are known for their superior tensile strength and high creep resistance. This study focuses on the optimization of post-process heat treatments and the impact on tensile and creep strength of a LPBF produced Ti6242S alloy. Therefore, a variety of annealing steps were conducted to gain knowledge about the decomposition process of the non-equilibrium as-built microstructure and the arising influence on the mechanical properties. Components made of Ti6242S and produced by LPBF reveal an extraordinarily high ultimate tensile strength of about 1530 MPa at room temperature, but show a low elongation at fracture (A5 = 4.3%). Based on microstructure-property relationships, this study recommends precise heat treatments on how to improve the desired mechanical properties in terms of strength, ductility as well as creep resistance. Moreover, this study shows a triplex heat treatment, which enhances the elongation at fracture (A5) to 16.5%, while the ultimate tensile strength is still at 1100 MPa.

Thermal Expansion of a Multiphase Intermetallic Ti-Al-Nb-Mo Alloy Studied by High-Energy X-ray Diffraction.

Intermetallic γ-TiAl-based alloys are lightweight materials for high-temperature applications, e.g., in the aerospace and automotive industries. They can replace much heavier Ni-based alloys at operating temperatures up to 750 °C. Advanced variants of this alloy class enable processing routes that include hot forming. These alloys consist of three relevant crystallographic phases (γ-TiAl, α2-Ti3Al, ßo-TiAl) that transform into each other at different temperatures. For thermo-mechanical treatments as well as for adjusting alloy properties required under service conditions, the knowledge of the thermal expansion behavior of these phases is important. Therefore, thermal expansion coefficients were determined for the relevant phases in a Ti-Al-Nb-Mo alloy for temperatures up to 1100 °C using high-energy X-ray diffraction.

Geometrical model for calculating the effect of surface morphology on total x-ray output of medical x-ray tubes.

PURPOSE: Correlation of characteristic surface appearance and surface roughness with measured air kerma (kinetic energy released in air) reduction of tungsten-rhenium (WRe) stationary anode surfaces. METHODS: A stationary anode test system was developed and used to alter nine initially ground sample surfaces through thermal cycling at high temperatures. A geometrical model based on high resolution surface data was implemented to correlate the measured reduction of the air kerma rate with the changing surface appearance of the samples. In addition to the nine thermally cycled samples, three samples received synthetic surface structuring to prove the applicability of the model to nonconventional surface alterations. Representative surface data and surface roughness values were acquired by laser scanning confocal microscopy. RESULTS: After thermal cycling in the stationary anode test system, the samples showed surface features comparable to rotating anodes after long-time operation. The established model enables the appearance of characteristic surface features like crack networks, pitting, and local melting to be linked to the local x-ray output at 100 kV tube voltage ,10° anode take off angle and 2 mm of added Al filtration. The results from the conducted air kerma measurements were compared to the predicted total x-ray output reduction from the geometrical model and show, on average, less than 10 % error within the 12 tested samples. In certain boundaries, the calculated surface roughness Ra showed a linear correlation with the measured air kerma reduction when samples were having comparable damaging characteristics and similar operation parameters. The orientation of the surface features had a strong impact on the measured air kerma rate which was shown by testing synthetically structured surfaces. CONCLUSIONS: The geometrical model used herein considers and describes the effect of individual surface features on the x-ray output. In close boundaries arithmetic surface roughness Ra was found to be a useful characteristic value on estimating the effect of surface damage on total x-ray output.

An Advanced TiAl Alloy for High-Performance Racing Applications.

Requirements and strict regulations for high-performance racing applications involve the use of new and innovative lightweight structural materials. Therefore, intermetallic γ-TiAl-based alloys enable new opportunities in the field due to their lower density compared to commonly used Ni-base superalloys. In this study, a ß-solidifying TiAl alloy was examined toward its use as structural material for inlet and outlet valves. The nominal composition of the investigated TNM alloy is Ti-43.5Al-4Nb-1Mo-0.1B (in at%), which enables an excellent formability at elevated temperatures due to the presence of bcc ß-phase. Different hot-extrusion tests on an industrial scale were conducted on the cast and hot isostatic pressed material to determine the ideal microstructure for the respective racing application. To simulate these operation conditions, hot tensile tests, as well as rotational bending tests, at room temperature were conducted. With a higher degree of deformation, an increasing strength and fatigue limit was obtained, as well as a significant increment of ductility. The fracture surfaces of the rotational bending test specimens were analyzed using scanning electron microscopy, revealing the relationship between crack initiation and microstructural constituents. The results of this study show that the mechanical performance of extruded TiAl material can be tailored via optimizing the degree of hot-extrusion.

Heat Treatments and Critical Quenching Rates in Additively Manufactured Al-Si-Mg Alloys.

Laser powder-bed fusion (LPBF) has significantly gained in importance and has become one of the major fabrication techniques within metal additive manufacturing. The fast cooling rates achieved in LPBF due to a relatively small melt pool on a much larger component or substrate, acting as heat sink, result in fine-grained microstructures and high oversaturation of alloying elements in the α-aluminum. Al-Si-Mg alloys thus can be effectively precipitation hardened. Moreover, the solidified material undergoes an intrinsic heat treatment, whilst the layers above are irradiated and the elevated temperature in the built chamber starts the clustering process of alloying elements directly after a scan track is fabricated. These silicon-magnesium clusters were observed with atom probe tomography in as-built samples. Similar beneficial clustering behavior at higher temperatures is known from the direct-aging approach in cast samples, whereby the artificial aging is performed immediately after solution annealing and quenching. Transferring this approach to LPBF samples as a possible post-heat treatment revealed that even after direct aging, the outstanding hardness of the as-built condition could, at best, be met, but for most instances it was significantly lower. Our investigations showed that LPBF Al-Si-Mg exhibited a high dependency on the quenching rate, which is significantly more pronounced than in cast reference samples, requiring two to three times higher quenching rate after solution annealing to yield similar hardness results. This suggests that due to the finer microstructure and the shorter diffusion path in Al-Si-Mg fabricated by LPBF, it is more challenging to achieve a metastable oversaturation necessary for precipitation hardening. This may be especially problematic in larger components.

Microstructural Evolution and Mechanical Properties of an Advanced γ-TiAl Based Alloy Processed by Spark Plasma Sintering.

Intermetallic γ-TiAl based alloys are innovative lightweight structural high-temperature materials used in aerospace and automotive applications due to already established industrial-scale processing routes, like casting and hot-working, i.e., forging. A promising alternative method of production, regarding manufacturing of near net-shape components, goes over the powder metallurgy route, more precisely by densification of TiAl powder via spark plasma sintering. In this study, gas atomized powder from the 4th generation TNM alloy, Ti-43.5Al-4Nb-1Mo-0.1B (in at.%), was densified and the microstructure was investigated by means of electron microscopy and X-ray diffraction. The sintered microstructure exhibits lamellar α2-Ti3Al /γ-TiAl colonies surrounded by globular γ- and ordered ßo-TiAl phase. The coarse lamellar spacing stems from the low cooling rate after densification at sintering temperature. Against this background, subsequent heat treatments were designed to decrease the lamellar widths by a factor of ten. Accompanying, tensile tests and creep experiments at different temperatures revealed that the modified almost fully lamellar microstructure is enhanced in strength and creep resistance, where a small volume fraction of globular γ-phase provides ductility at ambient temperatures.

Thermal Expansion and Other Thermodynamic Properties of α2-Ti3Al and γ-TiAl Intermetallic Phases from First Principles Methods.

Anisotropic thermal expansion coefficients of tetragonal γ -TiAl and hexagonal α 2 -Ti3Al phases were calculated using first principles methods. Two approaches with different computational costs and degrees of freedom were proposed. The predicted values were compared with available experimental data showing that for γ -TiAl, the more computational demanding method with decoupled impact of volume and temperature effects on the cell shape leads to significantly better results than that with only ground-state optimised unit cell geometry. In the case of the α 2 -Ti3Al phase, both approaches yielded comparable results. Additionally, heat capacity and bulk modulus were evaluated as functions of temperature for both phases, and were fitted to provide an analytical formula which can be further used.

Correlative microscopy of a carbide-free bainitic steel.

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite-austenite (M-A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M-A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation.

Advancement of Compositional and Microstructural Design of Intermetallic γ-TiAl Based Alloys Determined by Atom Probe Tomography.

Advanced intermetallic alloys based on the γ-TiAl phase have become widely regarded as most promising candidates to replace heavier Ni-base superalloys as materials for high-temperature structural components, due to their facilitating properties of high creep and oxidation resistance in combination with a low density. Particularly, recently developed alloying concepts based on a ß-solidification pathway, such as the so-called TNM alloy, which are already incorporated in aircraft engines, have emerged offering the advantage of being processible using near-conventional methods and the option to attain balanced mechanical properties via subsequent heat-treatment. Development trends for the improvement of alloying concepts, especially dealing with issues regarding alloying element distribution, nano-scale phase characterization, phase stability, and phase formation mechanisms demand the utilization of high-resolution techniques, mainly due to the multi-phase nature of advanced TiAl alloys. Atom probe tomography (APT) offers unique possibilities of characterizing chemical compositions with a high spatial resolution and has, therefore, been widely used in recent years with the aim of understanding the materials constitution and appearing basic phenomena on the atomic scale and applying these findings to alloy development. This review, thus, aims at summarizing scientific works regarding the application of atom probe tomography towards the understanding and further development of intermetallic TiAl alloys.