Surface chemistry in Ti-6Al-4V feedstock as influenced by powder reuse in electron beam additive manufacturing.

X-ray photoelectron spectroscopy (XPS) as well as scanning and transmission electron microscopy (SEM/TEM) analysis was carried out on four Ti-6Al-4V powders used in electron beam powder-bed fusion (PBF-EB) production environments: virgin low oxygen (0.080 wt% O), reused medium oxygen (0.140 wt% O), reused high oxygen (0.186 wt% O), and virgin high oxygen (0.180 wt% O). The two objectives of this comparative analyses were to (1) investigate high oxygen containing Grade 23 Ti-6Al-4V powders which were further oxidized as a function of reuse and (2) comparing the two virgin Grade 23 and Grade 5 powders of similar oxygen content. The microstructure of the low oxygen virgin Grade 23 powder was consistent with martensitic α' microstructure, whereas the reused powder displayed tempered α/ß Widmänstatten microstructure. XPS revealed a decrease in TiO2 at the surface of the reused powders with an increase in Al2O3. This trend is energetically favorable at the temperatures and pressures in PBF-EB machines, and it is consistent with the thermodynamics of Al2O3 vs. TiO2 reactions. An unexpected amount of nitrogen was measured on the titanium powder, with a general increase in nitride on the surface of the particles as a function of reuse in the Grade 23 powder.

Small Punch Testing to Estimate the Tensile and Fracture Properties of Additively Manufactured Ti-6Al-4V.

Small punch (SP) testing is a methodology that uses tiny disks (generally 8 mm in diameter and 0.5 mm thick) to estimate mechanical properties of metallic materials, such as tensile properties, fracture toughness, and ductile-to-brittle transition temperature. Empirical correlations are typically used to infer conventional mechanical properties from characteristic forces and displacements obtained from the test record. The majority of the available literature relates to SP testing of steels, while relatively little is available for other metallic materials. At NIST in Boulder, Colorado, we conducted SP tests on additively manufactured (AM) Ti-6Al-4V with different processing parameters and heat treatment conditions. Force/punch displacement curves appeared different than those typically reported for conventionally manufactured steels, and correlations with tensile and fracture parameters were generally weaker than those published for steel samples. It appears that the application of the SP technique (characterized by a biaxial loading mode) to materials with high anisotropy such as AM materials may be somewhat problematic and therefore of limited applicability.

Impact of grain orientation and phase on Volta potential differences in an additively manufactured titanium alloy.

This work introduces a method for co-localized multi-modal imaging of sub-µm features in an additively manufactured (AM) titanium alloy. Ti-6Al-4V parts manufactured by electron beam melting powder bed fusion were subjected to hot isostatic pressing to seal internal porosity and machined to remove contour-hatch interfaces. Electron microscopy and atomic force microscopy-based techniques (electron backscatter diffraction and scanning Kelvin probe force microscopy) were used to measure and categorize the effects of crystallographic texture, misorientation, and phase content on the relative differences in the Volta potential of α-Ti and ß-Ti phases. Given the tunability of additive manufacturing processes, recommendations for texture and phase control are discussed. In particular, our findings indicate that the potential for micro-galvanic corrosion initiation can be regulated in AM Ti-6Al-4V parts by minimizing both the total area of {111} prior-ß grains and the number of contact points between {111} ß grains and α laths that originate from {001} prior-ß grains.

Texture evolution as a function of scan strategy and build height in electron beam melted Ti-6Al-4V.

Metal additive manufacturing (AM) enables customizable, on-demand parts, allowing for new designs and improved engineering performance. Yet, the ability to control AM metal alloy microstructures (i.e., grain morphology, crystallographic texture, and phase content) is lacking. This work performs corroborative neutron diffraction and large-scale electron backscatter diffraction (EBSD) measurements to assess crystallographic texture in electron beam melted (EBM) Ti-6Al-4V as a function of scan strategy and build height. Texture components for one raster and two spot melt scan strategies were evaluated using a triclinic specimen symmetry to capture all possible texture components, which were found to be considerably different than previously reported values from studies employing orthotropic specimen symmetry. This finding highlights the importance of a standard method and best practice for assessing textures produced by AM. Texture was found to vary between scan strategies, but changed minimally as a function of build height. Parent phase ß-Ti reconstructions obtained from as-built crystallographic orientations revealed spot melt scan strategies produced finer equiaxed/columnar grains with clear 001 ß build direction fiber textures, whereas the raster scan strategy produced large columnar grains and a weaker 001 ß build direction fiber texture. The observed grain morphologies agree with those predicted by solidification theory for the thermal gradients and solidification velocities experienced during the build process. The presence of a strong 001 ß fiber orientation (typical of cubic solidification) produced by spot melting was found to correlate with a previously unreported 01 1 ¯ 2 α fiber texture in the as-built condition and colony microstructures. The 01 1 ¯ 2 α fiber texture was weakly observed for the raster scan strategy, and 001 ß oriented grains preferentially transformed into α' martensite with orientations between 1 1 ¯ 00 α and 11 2 ¯ 0 α . This shift in product α-Ti orientations has not yet been reported, and further work is recommended to understand these crystallographic signatures in the context of solid-state phase transformations. The presence of the 01 1 ¯ 2 α fiber texture is proposed as a useful diagnostic for evaluating the solidification or transformed microstructure condition (e.g., grain morphology and texture) of Ti-6Al-4V AM builds via accessible techniques like laboratory X-ray diffraction.

MAUD Rietveld Refinement Software for Neutron Diffraction Texture Studies of Single­ and Dual­Phase Materials.

This work presents a detailed instructional demonstration using the Rietveld refinement software MAUD for evaluating the crystallographic texture of single- and dual-phase materials, as applied to High-Pressure-Preferred-Orientation (HIPPO) neutron diffraction data obtained at Los Alamos National Laboratory (LANL) and electron backscatter diffraction (EBSD) pole figures on Ti-6Al-4V produced by additive manufacturing. This work addresses a number of hidden challenges intrinsic to Rietveld refinement and operation of the software to improve users' experiences when using MAUD. A systematic evaluation of each step in the MAUD refinement process is described, focusing on devising a consistent refinement process for any version of MAUD and any material system, while also calling out required updates to previously developed processes. A number of possible issues users may encounter are documented and explained, along with a multilayered assessment for validating when a MAUD refinement procedure is finished for any dataset. A brief discussion on appropriate sample symmetries is also included to highlight possible oversimplifications of the texture data extracted from MAUD. Included in the appendix of this work are two systematic walkthroughs applying the process described. Files for these walkthroughs can be found at the data repository located at: https://doi.org/10.18434/mds2-2400.

Effects of laser-energy density and build orientation on the structure-property relationships in as-built Inconel 718 manufactured by laser powder bed fusion.

This study investigates the effects of build orientation and laser-energy density on the pore structure, microstructure, and tensile properties of Inconel 718 manufactured by laser powder bed fusion. Three different build conditions were selected for comparison based on previous research (namely, the conditions that resulted in the worst and best fatigue lifetimes): 0° build orientation and 38 J/mm3 laser-energy density, 0° build orientation and 62 J/mm3 laser-energy density, and 60° build orientation and 62 J/mm3 laser-energy density. Differences in porosity were measured between each build condition. In terms of microstructure, all three conditions exhibited a predominantly <001> texture in the build direction, grains elongated in the build direction, and a sub-grain structure oriented with the build direction that consisted of dislocation networks decorated with nano-scale precipitates. Build orientation (0° versus 60° with respect to the build plate) produced a difference in yield strength due to anisotropic grain morphology and effective grain size. The low laser-energy density specimens showed a significant decrease in all mechanical properties compared to the high laser-energy density specimens because the amount (6.91% by volume) and size of the lack-of-fusion porosity (from insufficient melting) sur-passed a level at which microstructure (the grain and sub-grain structure) no longer governs quasi-static mechanical properties. This work provides insight that could enable the tunability of structure-property relationships in as-built Inconel 718 by optimizing laser-energy density and build orientation.