Integrated High-Throughput and Machine Learning Methods to Accelerate Discovery of Molten Salt Corrosion-Resistant Alloys.

Insufficient availability of molten salt corrosion-resistant alloys severely limits the fruition of a variety of promising molten salt technologies that could otherwise have significant societal impacts. To accelerate alloy development for molten salt applications and develop fundamental understanding of corrosion in these environments, here an integrated approach is presented using a set of high-throughput (HTP) alloy synthesis, corrosion testing, and modeling coupled with automated characterization and machine learning. By using this approach, a broad range of CrFeMnNi alloys are evaluated for their corrosion resistances in molten salt simultaneously demonstrating that corrosion-resistant alloy development can be accelerated by 2 to 3 orders of magnitude. Based on the obtained results, a sacrificial protection mechanism is unveiled in the corrosion of CrFeMnNi alloys in molten salts which can be applied to protect the less unstable elements in the alloy from being depleted, and provided new insights on the design of high-temperature molten salt corrosion-resistant alloys.

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.

Understanding Deformation Behavior in Uniaxial Tensile Tests of Steel Specimens at Varying Strain Rates.

Uniaxial tensile tests are routinely conducted to obtain stress-strain data for forming applications. It is important to understand the deformation behavior of test specimens at plastic strains, temperatures, and strain rates typically encountered in metal forming processes. In this study, the Johnson-Cook (J-C) flow stress model was used to describe the constitutive behavior of ASTM International (ASTM) A 1008 steel specimens during uniaxial tensile tests at three different average strain rates (10-5 s-¹, 10-³ s-¹, and 10-¹ s-¹). The digital image correlation (DIC) technique was used for displacement and strain measurement, and two-dimensional (2D) infrared (IR) imaging was employed for temperature measurement. Separate optimization studies involving relevant finite element (FE) modeling with appropriate measured data yielded optimum values of convective heat transfer coefficients, J-C parameters, and inelastic heat fraction variables. FE modeling employing these optimum parameter values was then used to study the mechanical behavior. While FE predictions matched measured strain localization and thermal field very well in the intermediate- and low-rate experiments, the high-rate test showed narrower strain localization and a sharper temperature peak in the experiment. Possible use of a higher steel thermal conductivity value and/or exclusion of material inhomogeneities may have resulted in discrepancies between computed and measured temperature and strain fields. The study shows that an optimized set of parameters obtained with a controlled test could be reasonably applied for other tests conducted at very different strain rates.

Assessment of Martensitic Transformation Paths Based on Transformation Potential Calculations.

Transformation potentials for two different martensitic transformation paths are calculated and compared to experimentally measured austenite textures of an SAE 201 stainless steel. The authors conclude that the γ → ε → α' transformation path is a better match than the γ → α' transformation path, based on comparison of the texture evolution and transformation potentials. However, significant plastic deformation is also observed in these samples which occurs simultaneously with the transformation. The values of transformation potentials also demonstrate that the transformation path may also be a function of crystal orientation and stress state, in addition to the effect of stacking fault energy (SFE).

Assessment of bias errors caused by texture and sampling methods in diffraction-based steel phase measurements.

Many advanced high-strength steels rely on a metastable austenite phase for improvements in strength and formability. To date, no method has demonstrated the ability to provide accurate austenite phase fraction measurements in textured steels. Several techniques have been proposed, such as averaging the intensity of several peaks and/or summation of intensity from several sample orientations. The series of numerical experiments performed in this work sought to quantify the effects of texture on the measurement of the austenite phase fraction, with an emphasis on techniques suitable for laboratory X-ray diffraction. Simulated diffraction profiles were created with the following variables: texture components for the ferrite and austenite phases, the sharpness of each of the texture components, the number of peaks used for averaging in the phase fraction calculation, and the sampling scheme used for sample orientation summation in the phase fraction calculation. The resulting phase fraction calculations showed that texture, the number of peak pairs and the sampling method have a drastic effect on phase fraction measurements, causing significant bias errors. Hexagonal grids produced minimal bias errors and demonstrated a robust method of measuring phase fractions in textured materials.

In Situ Structural Characterization of Ageing Kinetics in Aluminum Alloy 2024 across Angstrom-to-Micrometer Length Scales.

The precipitate structure and precipitation kinetics in an Al-Cu-Mg alloy (AA2024) aged at 190 °C, 208 °C, and 226 °C have been studied using ex situ Transmission Electron Microscopy (TEM) and in situ synchrotron-based, combined ultra-small angle X-ray scattering, small angle X-ray scattering (SAXS), and wide angle X-ray scattering (WAXS) across a length scale from sub-Angstrom to several micrometers. TEM brings information concerning the nature, morphology, and size of the precipitates while SAXS and WAXS provide qualitative and quantitative information concerning the time-dependent size and volume fraction evolution of the precipitates at different stages of the precipitation sequence. Within the experimental time resolution, precipitation at these ageing temperatures involves dissolution of nanometer-sized small clusters and formation of the planar S phase precipitates. Using a three-parameter scattering model constructed on the basis of TEM results, we established the temperature-dependent kinetics for the cluster-dissolution and S-phase formation processes simultaneously. These two processes are shown to have different kinetic rates, with the cluster-dissolution rate approximately double the S-phase formation rate. We identified a dissolution activation energy at (149.5 ± 14.6) kJ mol-1, which translates to (1.55 ± 0.15) eV/atom, as well as an activation energy for the formation of S precipitates at (129.2 ± 5.4) kJ mol-1, i.e. (1.33 ± 0.06) eV/atom. Importantly, the SAXS/WAXS results show the absence of an intermediate Guinier-Preston Bagaryatsky 2 (GPB2)/S″ phase in the samples under the experimental ageing conditions. These results are further validated by precipitation simulations that are based on Langer-Schwartz theory and a Kampmann-Wagner numerical method.

Anodic Dissolution of Aluminum in the Aluminum Chloride-1-Ethyl-3-methylimidazolium Chloride Ionic Liquid.

The anodic dissolution of aluminum metal was investigated in the Lewis acidic chloroaluminate ionic liquid, aluminum chloride-1-ethyl-3-methylimidazolium chloride. The investigation was conducted on aluminum rotating disk electrodes as a function of potential, ionic liquid composition, and temperature. Two different dissolution mechanisms were realized. At modest overpotentials, dissolution takes place under mixed kinetic-mass transport control. However, as the overpotential is increased to induce higher dissolution rates and/or the ionic liquid is made more acidic, the dissolution reaction transitions to a potential-independent passivation-like process ascribed to the formation of a porous solid layer of AlCl3(s). At a fixed temperature and composition, the limiting passivation current density displays Levich behavior and also scales linearly with the concentration of AlCl4 - in the ionic liquid. The heterogeneous kinetics of the Al dissolution reaction were measured in the active dissolution potential regime. The exchange current densities were independent of the composition of the ionic liquid, and the anodic transfer coefficients were close to zero and seemed to be independent of the Al grain size.

Forming limit prediction using a self-consistent crystal plasticity framework: a case study for body-centered cubic materials.

A rate-dependent self-consistent crystal plasticity model was incorporated with the Marciniak-Kuczynski model in order to study the effects of anisotropy on the forming limits of BCC materials. The computational speed of the model was improved by a factor of 24 when running the simulations for several strain paths in parallel. This speed-up enabled a comprehensive investigation of the forming limits of various BCC textures, such as γ, σ, α, η and ϵ fibers and a uniform (random) texture. These simulations demonstrate that the crystallographic texture has significant (both positive and negative) effects on the resulting forming limit diagrams. For example, the γ fiber texture, which is often sought through thermo-mechanical processing due to a high r-value, had the highest forming limit in the balanced biaxial strain path but the lowest forming limit under the plane strain path among the textures under consideration. A systematic investigation based on the results produced by the current model, referred to as 'VPSC-FLD', suggests that the r-value does not serve as a good measure of forming limit strain. However, model predictions show a degree of correlation between the r-value and the forming limit stress.

Thermally-activated constitutive model including dislocation interactions, aging and recovery for strain path dependence of solid solution strengthened alloys: Application to AA5754-O.

A thermally-activated constitutive model is developed based on dislocation interactions, crystallographic orientations and microstructural evolution to describe the elasto-plastic stress-strain behavior during multi-axial loading. The aim is to contribute to the quantification of complex strain path response in solid solution strengthened alloys. In detail, dislocation/dislocation interactions are incorporated in the model to quantify latent and kinematic hardening phenomena during loading path changes. Dislocation density-based constitutive relations are included to account for dislocation features such as dislocation forests, walls and channels. Moreover specifically, dislocation/solute atom interactions are also considered in order to account for both dynamic and static strain aging as well as static recovery. The model is validated against multiple multi-axial data sets for AA5754-O with changes of loading path and various degrees of pre-strain and time intervals between tests.