Impact of in Situ Heat Treatment Effects during Laser-Based Powder Bed Fusion of 1.3343 High-Speed Steel with Preheating Temperatures up to 700 °C

For laser-based powder bed fusion (PBF-LB) of high carbon steels, preheated build platforms can reduce thermal stresses and crack formation inside the generated material. Furthermore, the heat distribution during PBF-LB is affected by laser energy input and heat transfer into the surrounding area. Depending on the preheating temperature and the thermal conditions during PBF-LB, thermal gradients and different thermal exposure times of the manufactured layers can lead to in situ heat treatment effects. As a result, gradients in microstructures and properties are observed in the manufactured material. The effects are investigated on AISI M2 high-speed steel (1.3343). Specimens are manufactured at platform preheating temperatures between 200 and 700 °C. Base plate and surface temperatures in the building layer are monitored by thermocouples and pyrometry. Local variations in the material microstructure and properties are determined and the effects of temperature distribution on microstructure and hardness are discussed.     

Influence of Two-Step Heat Treatments on Microstructure and Mechanical Properties of a β-Solidifying Titanium Aluminide Alloy Fabricated via Electron Beam Powder Bed Fusion

Additive manufacturing technologies, particularly electron beam powder bed fusion (PBF-EB/M), are becoming increasingly important for the processing of intermetallic titanium aluminides. This study presents the effects of hot isostatic pressing (HIP) and subsequent two-step heat treatments on the microstructure and mechanical properties of the TNM-B1 alloy (Ti–43.5Al–4Nb–1Mo–0.1B) fabricated via PBF-EB/M. Adequate solution heat treatment temperatures allow the adjustment of fully lamellar (FL) and nearly lamellar (NL-β) microstructures. The specimens are characterized by optical microscopy and scanning electron microscopy (SEM), X-ray computed tomography (CT), X-ray diffraction (XRD), and electron backscatter diffraction (EBSD). The mechanical properties at ambient temperatures are evaluated via tensile testing and subsequent fractography. While lack-of-fusion defects are the main causes of failure in the as-built condition, the mechanical properties in the heat-treated conditions are predominantly controlled by the microstructure. The highest ultimate tensile strength is achieved after HIP due to the elimination of lack-of-fusion defects. The results reveal challenges originating from the PBF-EB/M process, for example, local variations in chemical composition due to aluminum evaporation, which in turn affect the microstructures after heat treatment. For designing suitable heat treatment strategies, particular attention should therefore be paid to the microstructural characteristics associated with additive manufacturing.     

Tap Reactor for Temporally and Spatially Resolved Analysis of the CO2 Methanation Reaction

Chemical energy carriers produced according to power-to-X concepts will play a crucial role in the future energy system. Here, CO₂ methanation is described as one promising route. However, transient operating conditions and the resulting effects on catalyst stability are to be considered. In this contribution, a tap reactor for spatially and temporally resolved analysis of the methanation reaction is presented. The Ni catalyst investigated was implemented as coating. Reaction data as a function of time and reactor coordinate under various operating conditions are presented and discussed. A comparison with simulation data validates the presented tap reactor concept.     

Pumping stations for today's steel degassing requirements

This article focuses on the vacuum equipment used in vacuum degassing (VD) and vacuum oxygen decarburization (VOD) processes. Despite harsh process conditions caused by outgassing and the process gases themselves, there are various pumping principles and designs of vacuum pumps that can be used. Through clever pump selection there is an opportunity to realize substantial energy and operating resource savings on the vacuum pumping side. Last but not least, a new pump series will be presented that further contributes to cost reduction through higher efficiency.     

Locally Adapted Microstructures in an Additively Manufactured Titanium Aluminide Alloy Through Process Parameter Variation and Heat Treatment

Electron beam powder bed fusion (PBF-EB/M) has been attracting great research interest as a promising technology for additive manufacturing of titanium aluminide alloys. However, challenges often arise from the process-induced evaporation of aluminum, which is linked to the PBF-EB/M process parameters. This study applies different volumetric energy densities during PBF-EB/M processing to deliberately adjust the aluminum contents in additively manufactured Ti–43.5Al–4Nb–1Mo–0.1B (TNM-B1) samples. The specimens are subsequently subjected to hot isostatic pressing (HIP) and a two-step heat treatment. The influence of process parameter variation and heat treatments on microstructure and defect distribution are investigated using optical and scanning electron microscopy, as well as X-ray computed tomography (CT). Depending on the aluminum content, shifts in the phase transition temperatures can be identified via differential scanning calorimetry (DSC). It is confirmed that the microstructure after heat treatment is strongly linked to the PBF-EB/M parameters and the associated aluminum evaporation. The feasibility of producing locally adapted microstructures within one component through process parameter variation and subsequent heat treatment can be demonstrated. Thus, fully lamellar and nearly lamellar microstructures in two adjacent component areas can be adjusted, respectively.     

Silane-Mediated Expansion of Domains in Si-Doped κ-Ga2O3 Epitaxy and its Impact on the In-Plane Electronic Conduction

Unintentionally doped (001)-oriented orthorhombic κ-Ga₂O₃ epitaxial films on c-plane sapphire substrates are characterized by the presence of ≈ 10 nm wide columnar rotational domains that can severely inhibit in-plane electronic conduction. Comparing the in- and out-of-plane resistance on well-defined sample geometries, it is experimentally proved that the in-plane resistivity is at least ten times higher than the out-of-plane one. The introduction of silane during metal-organic vapor phase epitaxial growth not only allows for n-type Si extrinsic doping, but also results in the increase of more than one order of magnitude in the domain size (up to ≈ 300 nm) and mobility (highest µ ≈ 10 cm²V⁻¹s⁻¹, with corresponding lowest ρ ≈ 0.2 Ωcm). To qualitatively compare the mean domain dimension in κ-Ga₂O₃ epitaxial films, non-destructive experimental procedures are provided based on X-ray diffraction and Raman spectroscopy. The results of this study pave the way to significantly improved in-plane conduction in κ-Ga₂O₃ and its possible breakthrough in new generation electronics. The set of cross-linked experimental techniques and corresponding interpretation here proposed can apply to a wide range of material systems that suffer/benefit from domain-related functional properties.     

Azide-Modified Poly(diethyl vinylphosphonate) for Straightforward Graft-to Carbon Nanotube Functionalization

Rare-earth metal-mediated group-transfer polymerization (REM-GTP) offers distinctive features over common polymerization techniques, such as living character, a broad scope of functional monomers, high activity, excellent control of the polymeric parameters as well as inherent chain-end functionalization. Through the latter, polymers with reactive end-groups become feasible, opening the pathway for further post-polymerization functionalization. In this study, a straightforward graft-to immobilization of the Michael-type polymer poly(diethyl vinylphosphonate) (PDEVP) on multi-walled carbon nanotubes (MWCNT) is reported. Hence, a customized azide initiator is synthesized and studied in the C H bond activation with various lanthanide-based catalysts and the subsequent polymerization of diethyl vinylphosphonate (DEVP). The successful attachment of the azide end-group is demonstrated via electrospray ionization mass spectrometry (ESI-MS) and the synthesized polymers are subjected to immobilization on multi-walled carbon nanotubes in a graft-to approach. The prepared MWCNT:PDEVP composites are analyzed via thermogravimetric analysis (TGA), elemental analysis (EA), Raman spectroscopy, X-Ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) and the versatility of this approach is shown via the stabilization of MWCNT dispersions in water.     

Impact of Ferroelectric Layer Thickness on Reliability of Back-End-of-Line-Compatible Hafnium Zirconium Oxide Films

Due to its ferroelectricity, hafnium oxide has attracted a lot of attention for ferroelectric memory devices. Amongst different dopant elements, zirconium is found to be beneficial due to the relatively low crystallization temperature of hafnium-zirconium-oxide (HZO), thus it is back-end-of-line (BEoL) compatible. The thickness of HZO has a significant impact on ferroelectric device reliability. High operation temperatures and high endurance are important criteria depending on the application. Herein, various HZO thicknesses (7, 8, and 10 nm) in MFM (metal-ferroelectric-metal) capacitors are investigated at varying operation temperatures (25 to 175 °C) at varying electric fields (±3 to ±5.4 MV cm⁻¹) with respect to polarization, leakage current, endurance, and retention. 7 nm HZO showed promising results with an endurance of 10⁷ cycles, with a low leakage current density, and almost no retention loss after 10 years. Extrapolated results at operation conditions (±2 MV cm⁻¹ and 10 MHz) showed an endurance of 10¹⁰ cycles.