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At least 667 records · Page 37

Remote and automated high-throughput powder diffraction measurements enabled by a robotic sample changer at SSRL beamline 2-1

The general-purpose powder diffractometer beamline (BL2-1) at the Stanford Synchrotron Radiation Lightsource (SSRL) is described. The evolution of design and performance of BL2-1 are presented, in addition to current operating specifications, applications and measurement capabilities. Recent developments involve a robotic sample changer enabling high-throughput X-ray diffraction measurements, applicable to mail-in and remote operations. In situ and operando capabilities to measure samples with different form factors ( e.g. capillary, flat plate or thin film, and transmission) and under variable experimental conditions are discussed. Several example datasets and accompanying Rietveld refinements are presented.

43 PARTICLE ACCELERATORS↗

High-resolution in-situ characterization of laser powder bed fusion via transmission X-ray microscopy at X-ray free electron lasers

In this work, we describe the instrumentation used to perform the first operando transmission X-ray microscopy (TXM) and simultaneous X-ray diffraction of laser melting simulating laser powder bed fusion on the XCS instrument at the Linac Coherent Light Source (LCLS) X-ray free-electron laser (XFEL). Our TXM with 40× magnification in the X-ray regime at 11 keV gave spatial resolutions down to 940 nm per line pair, with effective pixel sizes down to 206 nm, image integration times of <100 fs, and frame rates tunable between 2.1 and 119 ns for two probe frames (0.48 GHz to 8.4 MHz). Images were recorded on Zyla and Icarus (UXI) detectors to trade off between spatial resolution and time dynamics. A 1 kW CW IR laser was coupled into the interaction point to conduct pump–probe studies of laser melting and solidification dynamics. Our temporal and spatial resolution with attenuation-based contrast exceeds that currently possible with synchrotron-based high-speed radiography. This system was sensitive to feature velocities of 10–12000 m s −1 but we did not observe any motion in this range in the laser melting of Al6061 alloy. Shockwaves were not observed and hot cracking proceeded at velocities below the detection limits. Pore accumulation was observed between successive shots, indicating that bubble escape mechanisms were not active. With proper experimental design, the spatial resolution, contrast and field of view could be further improved or modified. The increased brightness and narrower bandwidth of the XFEL allowed for this imaging technique and it lays the groundwork for a wide range of operando techniques to study additive manufacturing.

47 OTHER INSTRUMENTATION↗

Background optimization of powder electron diffraction for implementation of the e-PDF technique and study of the local structure of iron oxide nanocrystals

The local structural characterization of iron oxide nanoparticles is explored using a total scattering analysis method known as pair distribution function (PDF) (also known as reduced density function) analysis. The PDF profiles are derived from background-corrected powder electron diffraction patterns (the e-PDF technique). Due to the strong Coulombic interaction between the electron beam and the sample, electron diffraction generally leads to multiple scattering, causing redistribution of intensities towards higher scattering angles and an increased background in the diffraction profile. In addition to this, the electron–specimen interaction gives rise to an undesirable inelastic scattering signal that contributes primarily to the background. The present work demonstrates the efficacy of a pre-treatment of the underlying complex background function, which is a combination of both incoherent multiple and inelastic scatterings that cannot be identical for different electron beam energies. Therefore, two different background subtraction approaches are proposed for the electron diffraction patterns acquired at 80 kV and 300 kV beam energies. From the least-square refinement (small-box modelling), both approaches are found to be very promising, leading to a successful implementation of the e-PDF technique to study the local structure of the considered nanomaterial.

36 MATERIALS SCIENCE↗

Orthorhombic cerium(III) carbonate hydroxide studied by synchrotron powder X-ray diffraction

Cerium(III) carbonate is a precursor material for the synthesis of various Ce-containing compounds. In this work, a synchrotron powder X-ray diffraction study of commercially obtained ‘cerium(III) carbonate hydrate' indicates that multiple Ce-containing phases are present. The majority phase CeCO 3 OH (52.49% wt ) was refined using an orthorhombic Pmcn structure model with a = 5.01019 (2) Å, b = 8.55011 (4) Å and c = 7.31940 (4) Å, which is based on a reported structure for the lanthanoid carbonate mineral ancylite. Additionally, a substantial portion of the precursor material is cubic cerium(IV) oxide (47.12% wt ).

08 HYDROGEN↗

Characterization of Properties of Laser Powder Bed Fusion 3D-Printed Inconel 718 for Centrifugal Turbomachinery Applications

Here, this paper presents the results of a comprehensive effort to characterize the properties of Inconel 718 produced by a form of laser powder bed fusion (LPBF) additive manufacturing (AM) or 3D-printing, subsequently subjected to hot isostatic pressing (HIP) and heat treatment according to standards F3055-14a and AMS 5663, respectively. Material property data, while broadly available for traditional Inconel 718 presentations (e.g. forgings or castings), is currently lacking for the 3D-printed material. It is expected that while limited in size, the experimental data sets presented provide sufficient information to glean the capability of LPBF Inconel 718. These include: 1) Chemical composition, electron backscatter diffraction (EBSD), and x-ray energy dispersive spectroscopy (XEDS) characterization of 3D-printed material structure; 2) Tensile properties — 0.2% yield stress, ultimate stress, modulus of elasticity, and elongation to failure — based on 108 samples, as functions of temperature and sample print orientation; 3) Creep rupture data including the Larson-Miller parameter, based on 21 samples; and 4) High cycle fatigue data based on 21 samples as a function of temperature. Results are compared to available standards and/or data for forged, cast, and other AM Inconel 718. A key observation of this study, based on the EBSD results, is that while the material appears to approach full recrystallization following heat treatment, there is a detectable fraction of the material that does not fully recrystallize, resulting in a material with mechanical properties (e.g. yield stress, creep rupture) measurably lower than those of forgings, but higher than those of castings.

30 DIRECT ENERGY CONVERSION↗

A novel physics-based and data-supported microstructure model for part-scale simulation of laser powder bed fusion of Ti-6Al-4V

The elasto-plastic material behavior, material strength and failure modes of metals fabricated by additive manufacturing technologies are significantly determined by the underlying process-specific microstructure evolution. In this work a novel physics-based and data-supported phenomenological microstructure model for Ti-6Al-4V is proposed that is suitable for the part-scale simulation of laser powder bed fusion processes. The model predicts spatially homogenized phase fractions of the most relevant microstructural species, namely the stable β-phase, the stable α s -phase as well as the metastable Martensite α m -phase, in a physically consistent manner. In particular, the modeled microstructure evolution, in form of diffusion-based and non-diffusional transformations, is a pure consequence of energy and mobility competitions among the different species, without the need for heuristic transformation criteria as often applied in existing models. The mathematically consistent formulation of the evolution equations in rate form renders the model suitable for the practically relevant scenario of temperature- or time-dependent diffusion coefficients, arbitrary temperature profiles, and multiple coexisting phases. Due to its physically motivated foundation, the proposed model requires only a minimal number of free parameters, which are determined in an inverse identification process considering a broad experimental data basis in form of time-temperature transformation diagrams. Subsequently, the predictive ability of the model is demonstrated by means of continuous cooling transformation diagrams, showing that experimentally observed characteristics such as critical cooling rates emerge naturally from the proposed microstructure model, instead of being enforced as heuristic transformation criteria. Eventually, the proposed model is exploited to predict the microstructure evolution for a realistic selective laser melting application scenario and for the cooling/quenching process of a Ti-6Al-4V cube of practically relevant size. Numerical results confirm experimental observations that Martensite is the dominating microstructure species in regimes of high cooling rates, e.g., due to highly localized heat sources or in near-surface domains, while a proper manipulation of the temperature field, e.g., by preheating the base-plate in selective laser melting, can suppress the formation of this metastable phase.

Inverse parameter identification↗

Prediction of microstructure formation in laser powder bed fusion process.

The datasets are results analyzing the predicted microstructures in a single track during the laser powder bed fusion additive manufacturing process. They are the outputs by running the opensource code, muMatScale (The code can be cited at: Yuan, Lang, Fattebert, Jean-Luc, and Sabau, Adrian. (2023, August 03). muMatScale. [Computer software]. https://github.com/lang-yuan/muMatScale. https://doi.org/10.11578/dc.20240112.2.) For each set of data, it contains the time-dependent information of Temperature, Fraction Solid, Grain ID, Grain Angle ( crystallographic orientations by Euler angles), and solute Composition. The dataset can be visualized by Paraview (https://www.paraview.org/ ). The 6 datasets are: 1. Baseline_base1_n4e14_dt20: baseline case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 2. Nuc_n4e15_dt20: case with bulk nucleation density of 4E+15/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 3. Nuc_n4e15_dt50: case with bulk nucleation density of 4E+15/m^3, undercooling of 50K, substrate nucleation density of 1.5E+15/m^3 4. Nuc_n6e15_dt20: case with bulk nucleation density of 4E+16/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 5. Base4_n4e14_dt20: case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 6.0E+15/m^3 6. Base16_n4e14_dt20: case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 2.4E+16/m^3

36 MATERIALS SCIENCE↗

A Co-Registered In-Situ and Ex-Situ Dataset from an Electron Beam Powder Bed Fusion Additive Manufacturing Process (Peregrine v2023-09)

This release contains a co-registered in-situ and ex-situ Peregrine dataset from a single Arcam Q10 Electron Beam Powder Bed Fusion (EB-PBF) Inconel 738 build. These data were collected at the Manufacturing Demonstration Facility (MDF) located at Oak Ridge National Laboratory (ORNL). The dataset includes layer-wise Near Infrared (NIR) in-situ imaging data, in-situ temporal sensor data, ex-situ X-Ray Computed Tomography (X-CT) scans, and the target part geometries. Additionally, anomaly detections produced by a trained Dynamic Segmentation Convolutional Neural Network (DSCNN) are provided.

36 MATERIALS SCIENCE↗

A Co-Registered In-Situ and Ex-Situ Tensile Properties Dataset from a Laser Powder Bed Fusion Additive Manufacturing Process (Peregrine v2023-11)

This release contains a co-registered in-situ and ex-situ Peregrine dataset from five Concept Laser M2 Laser Powder Bed Fusion (L-PBF) stainless steel 316L builds containing 6,299 SS-J3 individually tracked tensile coupons. These data were collected at the Manufacturing Demonstration Facility (MDF) located at Oak Ridge National Laboratory (ORNL). The dataset includes layer-wise visible-light in-situ imaging data, the laser scan paths and parameters, in-situ temporal sensor data, room-temperature static tensile test results, and the target part geometries. Additionally, anomaly detections produced by a modified Dynamic Segmentation Convolutional Neural Network (DSCNN) are provided.

36 MATERIALS SCIENCE↗

A Co-Registered In-Situ and Ex-Situ Dataset from a Laser Powder Bed Fusion Additive Manufacturing Process (Peregrine v2023-10)

This release contains a co-registered in-situ and ex-situ Peregrine dataset from a single Concept Laser M2 Laser Powder Bed Fusion (L-PBF) stainless steel 316L build. These data were collected at the Manufacturing Demonstration Facility (MDF) located at Oak Ridge National Laboratory (ORNL). The dataset includes layer-wise visible-light in-situ imaging data, the laser scan paths and parameters, in-situ temporal sensor data, X-Ray Computed Tomography (X-CT) scans, pycnometry and tensile test results, etched micrographs from selected locations, and the target part geometries. Additionally, anomaly detections produced by a modified Dynamic Segmentation Convolutional Neural Network (DSCNN) are provided.

36 MATERIALS SCIENCE↗

Pressurizing Hagan and SAVY containers to 30-psig (air) to measure the release of analytical cerium oxide test powder

In response to an ESS surrounding the storage of sealed sources at TA-55, personnel from RP-SVS (Radiation Protection Services) and ORI-2 (Operational Readiness & Execution) were approached by ES-55 (Facility System Engineering) to provide technical testing of known nuclear material storage containers. Testing criteria were determined by SB-PF (Safety Basis for Plutonium Facilities). Tests were conducted in conjunction with multiple related projects at the Aerosol Sciences Laboratory (TA-03-0130-0103). An experimental system was quickly developed to deliver a pressure pulse (30-psig) that mimics a sealed source burst scenario. A series of twelve tests was conducted. Six tests were done with two different 5QT SAVY-4000 containers, where each SAVY filter-lid combination was subjected to three successive test insults. Three tests were done with a (0.375" diameter filter) 8Q.T Hagan container, and three tests with a (0.625" diameter filter) 8QT Hagan container. An unused, fresh container filter was used for each tested Hagan container, each receiving only one test insult per filter. Cerium oxide (CeO 2 ) powder was loaded (100 grams per test) into a nozzle in the tested Hagan and SAVY containers, and the nozzle was hard-plumbed to a ball valve and a pressure source. This system was installed into the Los Alamos RRFMC (Respirable Release Measurement Chamber), which is an integrated multipurpose aerosol wind tunnel that satisfies NQA-1 subpart 2.4 for R&D work. The ball valve was fitted with a mechanical linkage for operation from outside the wind tunnel. An aerodynamic particle sizer counted the particle concentrations and size distributions of released aerosol. Respirable aerosol released during the tests was measured and a correction factor for wind tunnel flowrate and internal duct deposition was applied.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Report on Mowry Shale Thermal Maturity Mapping in the Powder River Basin, Wyoming

The Enhanced Oil Recovery Institute (EORI) has completed a map of thermal maturity of the Mowry Shale in the Powder River Basin (PRB). Thermal maturity, the degree to which the total organic carbon in a formation has been transformed from kerogen to producible hydrocarbons due to heat and pressure, is an important measure for not just the quality of a source rock, but also helps for delineating areas more favorable for unconventional drilling. There is a dearth of published Mowry maturity maps available for the PRB and this publication endeavors to provide a detailed map based on a large, public data set covering the Wyoming portion of the PRB. Additional data, currently held confidential by operators in the basin, would be of benefit to future iterations of this map.

02 PETROLEUM↗

The Elevated-Temperature Cyclic Properties of Alloy 316L Manufactured Using Powder Metallurgy Hot Isostatic Pressing

According to developers at the GAIN 2019 microreactors workshop, advanced manufacturing (AM) is needed to fabricate microreactor components. A methodology has not been established to qualify AM for elevated-temperature nuclear construction. A potential approach is to use the wrought design methodology by establishing the AM properties as equivalent to or better than wrought. This investigation aims to understand the relationship between powder metallurgy hot isostatic pressing (PM HIP) and material characteristics for Alloy 316L as they relate to elevated-temperature component design and construction. The elevated-temperature cyclic behavior of Alloy 316L manufactured by PM HIP differs from wrought. Of particular significance is the reduced number of cycles to failure for the PM HIP Alloy 316L compared to wrought. Additional work to identify the microstructural feature that control the elevated-temperature cyclic behavior is needed.

36 MATERIALS SCIENCE↗

The Elevated-Temperature Cyclic Properties of Alloy 316H Fabricated by Powder Metallurgy Hot Isostatic Pressing (Rev.1)

Powder metallurgy hot isostatic pressing (PM HIP), an advanced manufacturing technique, is viewed by the Department of Energy as a “transformational technology” for heavy section manufacturing of nuclear components. Although PM HIP is a mature technology, it has not been qualified in Section III, Division 5 for elevated-temperature nuclear construction. This work seeks to demonstrate a PM HIP qualification method for elevated-temperature nuclear construction that is based on allowable material characteristics. Specifically, the elevated-temperature cyclic properties of PM HIP 316H are investigated. The creep-fatigue properties of PM HIP 316H are significantly degraded compared to those of wrought. Current PM HIP practices are not able to fabricate elevated-temperature nuclear components with creep-fatigue properties that are equivalent to or better than traditional wrought components. A research and development program is proposed for qualifying PM HIP 316H for elevated-temperature nuclear construction.

36 MATERIALS SCIENCE↗

In-Situ Process Monitoring Evaluation and Demonstration using Advanced Characterization with Laser Powder Bed Systems

Oak Ridge National Laboratory’s (ORNL) Manufacturing Demonstration Facility (MDF) worked with EOS Group to evaluate the current in-situ sensor capabilities of an EOS M290 Laser Powder Bed Fusion machine. The M290 was fitted with a 1 Mega-Pixel (MP) grayscale visible-light camera and a 5 MP temporally integrated (TI) near-infrared (NIR) camera. One print from stainless steel (SS) 316 and two from Inconel 625 (IN625) were performed where data including in-situ imaging and a machine log file were captured. These data were subsequently analyzed using a Dynamic Multi-Scale Segmentation Convolutional Neural Network (DMSCNN) trained on user defined classes and correlated to as-printed flaws, in the form of porosity, discovered in X-Ray Computed Tomography (XCT). In Phase I, two indications were detected in-situ and spatially correlated to stochastic lack-of-fusion flaws discovered using XCT. In Phase II, using these links from in-situ signatures to XCT flaw populations, a second neural network (NN) was trained to create a Voxelized Property Prediction Model (VPPM) to predict porosity percentages within the part using only features garnered from the in-situ data from two IN625 complex geometries. The VPPM was able to accurately predict porosity values for IN625 parts with an R 2 value of 0.764.

36 MATERIALS SCIENCE↗

Melt-Pool Dynamics and Microstructure of Mg Alloy WE43 under Laser Powder Bed Fusion Additive Manufacturing Conditions

Magnesium-based alloy WE43 is a state-of-the-art bioresorbable metallic implant material. There is a need for implants with both complex geometries to match the mechanical properties of bone and refined microstructure for controlled resorption. Additive manufacturing (AM) using laser powder bed fusion (LPBF) presents a viable fabrication method for implant applications, as it offers near-net-shape geometrical control, allows for geometry customization based on an individual patient, and fast cooling rates to achieve a refined microstructure. In this study, the laser–alloy interaction is investigated over a range of LPBF-relevant processing conditions to reveal melt-pool dynamics, pore formation, and the microstructure of laser-melted WE43. In situ X-ray imaging reveals distinct laser-induced vapor depression morphology regimes, with minimal pore formation at laser-scan speeds greater than 500 mm/s. Optical and electron microscopy of cross-sectioned laser tracks reveal three distinct microstructural regimes that can be controlled by adjusting laser-scan parameters: columnar, dendritic, and banded microstructures. These regimes are consistent with those predicted by the analytic solidification theory for conduction-mode welding, but not for keyhole-mode tracks. The results provide insight into the fundamental laser–material interactions of the WE43 alloy under AM-processing conditions and are critical for the successful implementation of LPBF-produced WE43 parts in biomedical applications.

36 MATERIALS SCIENCE↗