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At least 343 records · Page 19

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DOE OSTI2022

High-Magnification Faraday Rotation Imaging and Analysis of X-pinch Implosion Dynamics

An X-pinch load driven by an intense current pulse (>100 kA in ~100 ns) can result in the formation of a small radius, runaway compressional micro-pinch. A micro-pinch is characterized by a hot (>1 keV), current-driven (>100 kA), high-density plasma column (near solid density) with a small neck diameter (1–10 μm), a short axial extent (<1 mm), and a short duration (.1 ns). With material pressures often well into the multi-Mbar regime, a micro-pinch plasma often radiates an intense, sub-ns burst of sub-keV to multi-keV x-rays. A low-density coronal plasma immediately surrounding the dense plasma neck could potentially shunt current away from the neck and thus reduce the magnetic drive pressure applied to the neck. To study the current distribution in the coronal plasma throughout the implosion process, a Faraday rotation imaging diagnostic (1064 nm) capable of producing simultaneous high-magnification polarimetric and interferometric images has been developed for the 1-MA, 100-ns MAIZE facility at the University of Michigan. Designed with a variable magnification (1–10×), this diagnostic achieves a spatial resolution of approximately 35 μm, which is useful for resolving the ~100-μm-scale coronal plasma region immediately surrounding the dense core. Combined with the corresponding interferogram, which provides the radial density distribution in the low-density coronal plasma, the measured rotation can be used to diagnose the delivery of the driver current, and thus the magnetic drive pressure, to the micro-pinch plasma as it approaches minimal radius. Using this technique on MAIZE, we have measured

Dowhan, G. V.↗

DOE OSTI2022

Transuranium Sulfide via the Boron Chalcogen Mixture Method and Reversible Water Uptake in the NaCu T S 3 Family

The behavior of 5f electrons in soft ligand environments makes actinides, and especially transuranium chalcogenides, an intriguing class of materials for fundamental studies. Due to the affinity of actinides for oxygen, however, it is a challenge to synthesize actinide chalcogenides using non-metallic reagents. Using the Boron Chalcogen Mixture (BCM) method, we achieved the synthesis of the transuranium sulfide NaCuNpS 3 starting from the oxide reagent, NpO 2 . Via the same synthetic route, the isostructural composition of NaCuUS 3 was synthesized and the material contrasted with NaCuNpS 3 . Single crystals of the U-analog, NaCuUS 3 , were found to undergo an unexpected reversible hydration process to form NaCuUS 3 ·xH 2 O (x ≈ 1.5). Here, a large combination of techniques was used to fully characterize the structure, hydration process, and electronic structures, specifically a combination of single crystal, powder, high temperature powder X-ray diffraction, extended X-ray ab-sorption fine structure, infrared, and inductively coupled plasma spectroscopies, thermogravimetric analysis, and density functional theory calculations. The outcome of these analyses enabled us to determine the composition of NaCuUS 3 ·xH 2 O and obtain a structural model that demonstrated the retention of the local structure within the [CuUS 3 ] – layers throughout the hydration-dehydration process. Band structure, density of states, and Bader charge calculations for NaCuUS 3 , NaCu-US 3 ·xH 2 O, and NaCuNpS 3 along with X-ray absorption near edge structure, UV-vis-NIR and work function measurements on ACuUS 3 (A = Na, K, and Rb) and NaCuUS 3 ·xH 2 O samples were carried out to demonstrate that electronic properties arise from the [CuTS 3 ] – layers and show surprisingly little dependence on the interlayer distance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Understanding the effects of fabrication process on BaZr 0.9 Y 0.1 O 3– δ grain-boundary chemistry using atom probe tomography

Proton-conducting oxides, such as BaZr 0.9 Y 0.1 O 3–δ (BZY10), are receiving significant scientific attention for application in a variety of electrochemical applications. It has been shown that the synthesis route has a significant effect on the ionic behavior of these materials, especially the grain boundaries (GB). In this study, laser-pulsed atom probe tomography (APT) is used to characterize the GB chemistry of BZY10 samples prepared by four different methods: (1) spark plasma sintering (SPS), (2) conventional sintering followed by high-temperature annealing (HT), (3) conventional sintering with NiO used as a sintering aid (SSR-Ni), and (4) solid-state reactive sintering of oxide precursor powders with NiO as a reactive sintering aid (SSRS-Ni). Oxygen depletion (corresponding to oxygen vacancy accumulation) was observed at every GB in this study, consistent with the positive space-charge GB region commonly assigned to these materials. In contrast to the consistent trends associated with oxygen depletion, cation constituents showed varying segregation/depletion behaviors. The samples that used NiO revealed Ni preferentially segregating to the GB. The most common impurities in BZY10 are Al, Fe, Mg, Si, and Sr, all of which generally accumulate at GBs. In order to quantify these chemical trends, the APT method was optimized for this material supplemented with understanding from density functional theory (DFT). Finally, this APT study reveals the complexity of BZY10 GB chemistry and shows that even adjacent GBs in the same material can sometimes show surprisingly different GB chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Simple thermal vapor deposition process for and characterization of n-type indium oxysulfide thin films

The search continues for alternative nontoxic n-type electron transport layers in optoelectronic thin-film devices. Indium oxysulfide, In 2 (O,S) 3 , represents one promising material for this application, especially when paired with chalcogenide absorber layers. The ternary nature of the composition allows for electrical conductivity and optical bandgap tuning by tailoring the sulfur to oxygen ratio in the oxysulfide alloy. However, thin films of In 2 (O,S) 3 are typically deposited only by chemical bath deposition or plasma-enhanced atomic layer deposition. Here we report deposition of thin films of In 2 (O,S) 3 in a custom-built thermal reactor using only water vapor and hydrogen sulfide as the coreactants. This advance is enabled by the use of a recently reported, highly reactive indium formamidinate precursor. As shown by x-ray photoelectron spectroscopy, the composition can be tuned from pure In 2 (O,S) 3 to pure In 2 S 3 by varying the ratio of cycles employing water or hydrogen sulfide. The oxygen to the sulfur ratio in the film can be controlled by altering the dose sequence, although films typically contain more sulfur than would be expected naively from the percentage of hydrogen sulfide doses in the deposition recipe. Rutherford backscattering spectrometry confirms the composition is sulfur-rich relative to the dosing ratio. Structural characterization indicates films are relatively amorphous in nature. Electrically, these films offer reasonably constant electron mobility at different O:S ratios, with an electron concentration tunable over 4 orders of magnitude. These oxysulfide films possess a higher indirect bandgap than their oxygen-free indium sulfide counterparts, indicating higher transmittance to blue light. These indium oxysulfide films may be suitable candidates for electron transport layers in thin-film solar cells where their wider bandgap might result in higher optical transparency and thus short circuit current density, while the tunability of their conduction band offset with an absorber layer may result in higher open circuit voltage.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Thermal transport modeling of laser-irradiated spheres

Thermal transport of uniformly laser-irradiated spheres of various materials is investigated computationally. One-dimensional simulations of low- to mid-Z materials (Be, Al, and Cu) are performed to evaluate the impact of nonlocal electron transport on experimental observables under laser intensities of relevance to direct-drive inertial confinement fusion. Here we compare thermal transport models of different levels of fidelity: flux-limited Spitzer–Harm diffusion, the Schurtz–Nicolai–Busquet (SNB) reduced-order nonlocal model, and a Fokker–Planck description. Spitzer–Harm diffusion with different flux-limiter factors are compared with different implementations of the SNB model in the HYDRA radiation hydrodynamics code. Under the conditions of interest, the peak heat flux in the thermal front with the SNB model shows good agreement with Fokker–Planck calculations, with the largest errors below 10% at 10 15 W/cm 2 laser intensity. From HYDRA-SNB simulations, two experimentally relevant effects are observed from nonlocal heat transport when compared to flux-limited Spitzer–Harm modeling: coronal temperatures are cooler due to reduced heat fluxes in the expanding plasma and (for mid-Z materials) x-ray emissions are enhanced due to preheating in the dense plasma.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2020

A versatile and low-cost chip-to-world interface: enabling ICP-MS characterization of isotachophoretically separated lanthanides on a microfluidic device

Microfluidics offer novel and state-of-the-art pathways to process materials. Microfluidic systems drastically reduce timeframes and costs associated with traditional lab-scale efforts in the area of analytical sample preparations. The challenge arises in effectively connecting microfluidics to off-chip analysis tools to accurately characterize samples after treatment on-chip. Here, a fused silica microfluidic device (MFD) is connected to a fused-silica capillary in order to create a world-to-chip connection between the MFD and an inductively coupled plasma mass spectrometer (ICP-MS). Specifically, this is demonstrated by utilizing isotachophoresis (ITP) on a microfluidic chip to separate samples containing up to 14 lanthanides into elementally pure bands. The separated sample is successfully transferred across a 7 nL dead space at the microchip-capillary junction, such that separation resolution is maintained and even increased through the interface and into the ICP-MS, where the elemental composition of the separated sample is analysed. Lanthanide samples of varying composition are detected using ICP-MS, demonstrating this versatile and cost-effective approach that does not degrade the separation quality achieved on the MFD. This simple and inexpensive connection enables fast, low-cost sample preparation immediately prior to injection into an ICP-MS or other analytical instruments.

Lackey, Hope E.↗

DOE OSTI2026

A tutorial on high-order harmonic generation in atoms, molecules, and condensed matter

This tutorial introduces strong-field-driven high-order harmonics, their experimental generation and characterization techniques, and their main applications including attosecond pulse generation and ultrafast spectroscopy of the target material. We begin from the use of atomic targets, where the first high-order harmonic generation (HHG) experiments were realized in the late 1980s. Then, we briefly discuss the basics of the microscopic generation mechanism and how various steps of the mechanism were exploited in applications such as generating isolated attosecond pulses and probing molecular orbitals. We introduce and describe the standard experimental approaches for condensed phase HHG, where we discuss unique technical challenges of the use of solid-state materials, such as the mitigation of plasma formation and laser damage. We cover the fundamentals of high-harmonic spectroscopy in condensed matter systems, such as wide bandgap dielectrics, semiconductors, liquid media, and 2D-crystals. We provide some examples of rapidly emerging spectroscopic capabilities, such as for probing crystal symmetries, Berry phases, and associated non-trivial topological properties of the source material. Finally, we provide an overview of the research field, including some of the challenges, opportunities, and open questions.

Attosecond pulses↗

DOE OSTI2020

High Heat Flux Testing of Castellated Graphite Plasma- Facing Components

As part of the recovery project of the National Spherical Tokamak Experiment–Upgrade (NSTX-U), the divertor plasma-facing components (PFCs) were redesigned to handle significantly higher heat fluxes and longer pulse lengths than NSTX. The design process resulted in a castellated, graphite PFC tile. To verify the thermal performance of this design, dedicated electron beam, high heat flux (HHF) testing was carried out on a de-optimized mock-up PFC target. These tests demonstrated that the tile design is itself robust to large, localized thermal gradients. No mechanical damage to the mock-up was observed during HHF testing, though the actual PFC tile mechanical tie-down was not tested. Rather, when the surface temperature exceeded the sublimation temperature of graphite, carbon blooms from the mock-up tile surface were observed. Finally, this resulted in 1 to 2 mm of surface material ablating from the mock-up after repeated, highly localized electron beam exposures.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Solid-state reaction mediated microstructural evolution in a spark plasma sintered in situ Ti–B 4 C composite

For this study, a novel porosity-free in situ Ti–B 4 C composite was fabricated via spark plasma sintering (SPS). Detailed analysis of the phase evolution, coupling results from XRM, XRD and SEM-EBSD-EDS, indicate that primarily TiB 2 precipitates formed due to the in-situ reactions between the boron-carbide and titanium powders. The precipitation of TiB 2 resulted in the formation of a graphitic C-rich thin layer circumscribing the partially reacted B 4 C particles. Further progression of the in-situ reaction leads to the out-diffusion of the excess carbon from the B 4 C particles, across the graphite and TiB 2 phases, forming TiC upon reacting with the titanium matrix. Therefore, the final microstructure primarily consisted of TiB 2 , TiC, and partially reacted B 4 C phases, with small amounts of TiB, α-Ti, and graphite. Furthermore, the microstructure in these SPS processed in situ composites appeared to be the product of a solid-state Ti–B 4 C diffusion couple, substantially different from their fusion-based additively manufactured counterparts. Nano-indentation tests revealed a remarkably high average hardness of ~25 GPa for this SPS-processed Ti–B 4 C composite and comparable (with literature) phase-specific hardness and modulus values for the constituent TiB 2 , TiC, and B 4 C phases.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Thermal gradient effect on helium and self-interstitial transport in tungsten

First-wall materials in a fusion reactor are expected to withstand harsh conditions, with high heat and particle fluxes that modify the materials microstructure. These fluxes will create strong gradients of temperature and concentration of diverse species. Besides the He ash and the hydrogenic species, neutron particles generated in the fusion reaction will collide with the material creating intrinsic defects, such as vacancies, self-interstitials atoms (SIAs), and clusters of such point defects. These defects and the He atoms will then migrate in the presence of the aforementioned gradients. In this study, we use nonequilibrium molecular dynamics to analyze the transport of He and SIAs in the presence of a thermal gradient in tungsten. We observe that, in all cases, the defects and impurity atoms tend to migrate toward the hot regions of the tungsten sample. The resulting species concentration profiles are exponential distributions, rising toward the hot regions of the sample, in agreement with irreversible thermodynamics analysis. For both He atoms and SIAs, we find that the resulting species flux is directed opposite to the heat flux, indicating that species transport is governed by a Soret effect (thermal-gradient-driven diffusion) characterized by a negative heat of transport that drives species diffusion uphill (from the cooler to the hot regions of the sample). Here, we demonstrate that the steady-state species profiles obtained accounting for the Soret effect vary significantly from those where temperature-gradient-driven transport is not considered and discuss the implications of such a Soret effect on the response to plasma exposure of plasma-facing tungsten.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Electron beam injection from a hollow cathode plasma into a downstream reactive environment: Characterization of secondary plasma production and Si 3 N 4 and Si etching

A material etching system was developed by combining beam electron injection from a direct current (DC) hollow-cathode (HC) electron source with the downstream reactive environment of a remote CF 4 /O 2 low temperature plasma. The energy of the injected beam electrons is controlled using an acceleration electrode biased positively relative to the HC Argon discharge. For an acceleration voltage greater than the ionization potential of Ar, the extracted primary electrons can produce a secondary plasma in the process chamber. We characterized the properties of the secondary plasma by performing Langmuir probe measurements of the electron energy probability function (EEPF) 2.5 cm below the extraction ring. The data indicate the existence of two major groups of electrons, including electrons with a primary beam electron energy which varies as the acceleration voltage is varied, along with low energy electrons produced by ionization of the Ar gas atoms in the process chamber by the injected beam electrons. When combining the HC Ar beam electron with a remote CF 4 /O 2 electron cyclotron wave resonance (ECWR) plasma, the EEPF of both the low energy plasma electron and beam electron components decreases. Additionally, we studied surface etching of Si3N4 and poly-crystalline Si (poly-Si) thin films as a function of process parameters, including the acceleration voltage (0-70 V), discharge current of the HC discharge (1-2 A), pressure (2- 100 mTorr), source to substrate distance (2.5 to 5 cm), and feed gas composition (with or without CF 4 /O 2 ). The direction of the incident beam electrons was perpendicular to the surface. Si 3 N 4 and poly-crystalline silicon etching are seen and indicate an electronneutral synergy effect. No/little remote plasma spontaneous etching was observed for the conditions used in this study, and the etching is confined to the substrate area irradiated by the injected beam electrons. The electron etched Si 3 N 4 surface etching rate profile distribution is confined within a ~30 mm diameter circle, which is slightly broader than the area for which poly-Si etching is seen, and coincides closely with the spatial profile of beam electrons as determined by the Langmuir probe measurements. The magnitude of poly-Si etching rate is by a factor of two times smaller than the Si 3 N 4 etching rate. In this paper, we discuss possible explanations of the data and the role of surface charging.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2026

NanoPSD: A software for automatic detection of Nano-Particle Shape Distribution in electron microscopy images

Accurate quantification of the size and morphology of nanoparticles from electron microscopy (EM) images is essential to understand growth mechanisms, surface reactivity, and functional behavior in nanoscale materials. Manual analysis remains slow, subjective, and difficult to reproduce in large datasets. We introduce NanoPSD (Nano-Particle Shape Distribution), an open-source and fully automated framework for quantitative particle detection and morphology analysis from EM images. NanoPSD integrates adaptive contrast enhancement, polarity-agnostic scale-bar detection, Optical Character Recognition (OCR)-based calibration, and classical segmentation via Otsu thresholding with morphological refinement. Particle contours are used to extract geometric descriptors, including equivalent circular diameter, aspect ratio, circularity, and solidity, enabling automated classification into spherical, rod-like, and aggregate morphologies. The framework supports both single-image and batch processing, generating publication-quality visualizations, LaTeX-ready tables, and structured comma-separated values (CSV) datasets. As a demonstration, we applied NanoPSD to plasma-synthesized nanoparticle samples diagnosed via transmission electron microscopy (TEM). The code produced statistically robust size and morphology distributions spanning a few to tens of nanometers with minimal user supervision. The pipeline demonstrates high reproducibility and scalability, processing large image collections with consistent calibration and output formatting. Its modular design enables seamless integration of future deep-learning-based segmentation models, providing a pathway toward intelligent, data-driven electron microscopy analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Numerical benchmark of transient pressure-driven metallic melt flows

Fluid dynamics simulations of melting and crater formation at the surface of a copper cathode exposed to high plasma heat fluxes and pressure gradients are presented. The predicted deformations of the free surface and the temperature evolution inside the metal are benchmarked against previously published simulations. Despite the physical model being entirely hydrodynamic and ignoring a variety of plasma–surface interaction processes, the results are also shown to be remarkably consistent with the predictions of more advanced models, as well as experimental data. This provides a sound basis for future applications of similar models to studies of transient surface melting and droplet ejection from metallic plasma-facing components after disruptions.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Directional amorphization of covalently-bonded solids: A generalized deformation mechanism in extreme loading

Shock compression subjects materials to a unique regime of high quasi-hydrostatic pressure and coupled shear stresses for durations on the order of 1–10 nanoseconds for laser-driven loading of samples. There is, additionally, an attendant temperature increase due to the shock and the mechanisms of plastic deformation in metals whereby dislocations, twins, and phase transitions nucleate and propagate at velocities near the sound speed. Covalently bonded materials have, by virtue of the directionality of their bonds, great difficulty in responding by conventional plastic deformation to this extreme regime of shock compression. Here, we propose that the shear from shock compression induces amorphization, as observed in Si, Ge, B4C, SiC, and olivine ((Mg, Fe) 2 SO 4 ) and that this is a general deformation mechanism in a broad class of covalently bonded materials. The crystalline structure transforms to amorphous along regions of maximum shear stress, forming nanoscale bands, and thereby relaxing the shear component of the imposed shock stress. This process is usually preceded by the emission and propagation of a critical concentration of dislocations.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Novel data interpretation method for DIII-D divertor retarding field energy analyzer with 3-D particle-in-cell simulations

A novel data interpretation process that utilizes comprehensive particle-in-cell (PIC) simulations is developed for the new retarding field energy analyzer (RFEA) currently being constructed at DIII-D for the lower divertor using the Divertor Material Evaluation System. Furthermore, this probe is expected to survive a heat load of up to 100 MW/m 2 for up to 5 s and reliably measure the main ion temperature (T i ) on the divertor target ranging from 10 to 200 eV. These extreme conditions posed significant engineering limitations on the probe geometry, thus extensive validation work has been performed. The conventional fitting method for the RFEA I–V characteristics is based on a simplified 1-D model without considering the ion space charge inside the probe cavity and may not be sufficient for probes designed for the DIII-D divertor environment. In this article, a more realistic description of the particle propagation process within the RFEA cavity is achieved by including both 3-D geometric effects and ion space charge in the PIC simulations, and the capability to reconstruct the ion energy distribution functions is demonstrated with reasonable consistency.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Surface Finishing and Coating Parameters Impact on Additively Manufactured Binder-Jetted Steel–Bronze Composites

In this paper, electroless nickel plating is explored for the protection of binder-jetting-based additively manufactured (AM) composite materials. Electroless nickel plating was attempted on binder-jetted composites composed of stainless steel and bronze, resulting in differences in the physicochemical properties. We investigated the impact of surface finishing, plating solution chemistry, and plating parameters to attain a wide range of surface morphologies and roughness levels. We employed the Keyence microscope to quantitatively evaluate dramatically different surface properties before and after the coating of AM composites. Scanning electron microscopy revealed a wide range of microstructural properties in relation to each combination of surface finishing and coating parameters. We studied chempolishing, plasma cleaning, and organic cleaning as the surface preparation methods prior to coating. We found that surface preparation dictated the surface roughness. Taguchi statistical analysis was performed to investigate the relative strength of experimental factors and interconnectedness among process parameters to attain optimum coating qualities. The quantitative impacts of phosphorous level, temperature, surface preparation, and time factor on the roughness of the nickel-plated surface were 17.95%, 8.2%, 50.02%, and 13.21%, respectively. On the other hand, the quantitative impacts of phosphorous level, temperature, surface preparation, and time factor on the thickness of nickel plating were 35.12%, 41.40%, 3.87%, and 18.24%, respectively. The optimum combination of the factors’ level projected the lowest roughness of Ra at 7.76 µm. The optimum combination of the factors’ level projected the maximum achievable thickness of ~149 µm. This paper provides insights into coating process for overcoming the sensitivity of AM composites in hazardous application spaces via robust coating.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Pretreatment of Bituminous Coal By-Products for the Hydrometallurgical Extraction of Rare Earth Elements

Low-temperature plasma (LTP) oxidation has been widely used to study the mineralogy of the mineral matter existing in coal sources. The current study investigated the potential of LTP oxidation as a pre-treatment method to improve rare earth element (REE) leachability from coal and its by-products. Representative density-fractionated samples of Baker and Fire Clay coarse refuse seam materials were ground to a top size of 180 µm and subjected to low-temperature plasma oxidation. Subsequently, the treated samples were leached at 1% w/v solids concentration and 75 °C for 5 h using (i) de-ionized (DI) water, (ii) 0.1 mol/L of ammonium sulfate, and (iii) 1.2 mol/L of sulfuric acid. It was determined that LTP treatment improved REE leaching characteristics, especially the leaching of heavy REEs (HREE), existing in the lighter density fractions of the Baker seam coarse refuse material. For instance, the HREE recovery for the 1.6 specific gravity (SG) float fraction increased from 8% to 33% using 0.1 mol/L of ammonium sulfate solution after 32 h of LTP treatment. This finding indicated that HREEs associated with the organic matter were released by the LTP treatment and adsorbed onto the surfaces of highly negative charged mineral matter and was exchanged with ammonium to allow their recovery. Similarly, when using 1.2 mol/L of sulfuric acid, the HREE recovery increased from 23% to 53% for the 1.6 SG float fraction. Interestingly, LTP oxidation did not provide significant improvement in REE recovery from the 2.2 sink density fractions, which was likely due to its lower organic content. No significant benefits were observed when treating the Fire Clay coarse refuse material, which was likely due to the lack of organic affinity and the difficult-to-leach REE minerals associated with the coal source such as monazite, xenotime, and zircon. Conversely, high-temperature oxidation within a temperature range of 600–750 °C significantly improved REE leaching characteristics for both coal sources. Improvement in REE recovery was due to decarbonization of the material, clay dehydroxylation and subsequent conversion of liberated REE-bearing minerals into a more leachable form. However, increasing the temperature above 800 °C decreased REE recovery due to the conversion of meta-kaolinite into mullite, which is chemically stable.

58 GEOSCIENCES↗

DOE OSTI2023

Development of process parameters and post-build conditions for qualification of LPBF 316 SS

To harness the potential of laser powder bed fusion (LPBF) 316H stainless steel (SS) for use in advanced nuclear reactors, extensive research efforts are needed to develop optimal laser processing parameters and appropriate heat treatments, taking into account various manufacturing platforms and locations. Furthermore, it is crucial to assess the material properties in environments relevant to reactor operating conditions. In collaboration with Oak Ridge National Laboratory (ORNL) and Los Alamos National Laboratory (LANL), Argonne National Laboratory (ANL) is dedicated to gaining insights into how the manufacturing process and post-build treatments impact the performance of LPBF 316H SS. This report provides an overview of ANL's research findings for FY23, focusing on LPBF 316H SS produced using a Renishaw AM400 laser system. Specifically, our research has concentrated on three key areas: 1) Optimum laser processing parameters: Leveraging the high-throughput printing technology, we systematically varied the laser power, exposure time and point distance within the same build. By measuring the as-printed porosity, we identified an optimum printing parameter window that produced materials with near-complete density; 2) Post-built treatment development: Materials printed with the optimum laser parameters underwent treatments including stress relief, solution annealing, and hot isostatic pressing. Subsequently, we fabricated tension, creep, and fatigue specimens from materials subjected to these different conditions. Over the next year, a series of scoping tests will be conducted to facilitate the selection of the most suitable post-build treatment condition; 3) Thermal aging effects on microstructure and properties: thermal aging at 550°C, 650°C and 750°C was conducted on LPBF 316H SS specimens up to 2500 h. Microstructural characterization was performed with electron microscopy, and the evolution of the dislocation cell structures and secondary phases was studied. Microhardness tests and tension tests were conducted to quantify changes in mechanical properties. The results revealed that the aged LPBF 316H SS exhibited a high density of Cr-rich and Mo-rich fine precipitates within grains due to the presence of a high density of dislocations and the globally distributed dislocation cell structures, which served as heterogeneous nucleation sites for secondary phases. Along grain boundaries, a Mo-Cr-rich phase, observed in 750°C-aged conditions, displayed significant thermal coarsening. Throughout the aging process, various mechanisms, including stress relaxation, dislocation cell structure recovery, solution hardening, and precipitation hardening, competed to influence materials strength. These results contribute towards establishing the technical basis for qualifying LPBF 316H SS for advanced nuclear reactor applications.

36 MATERIALS SCIENCE↗