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DOE OSTI2025

Post-build stress-relief optimization for laser powder bed fusion 316H stainless steel

Nuclear energy remains a critical component of a diversified and efficient energy portfolio, offering reliable, high-capacity, and low-carbon power. However, in the U.S., aging infrastructure and the slow qualification and deployment of advanced materials and manufacturing techniques hinder progress in next-generation reactor technologies. This study explores the application of laser powder bed fusion (LPBF) additive manufacturing for stainless steel 316H, with a focus on optimizing post-build heat treatments to enhance material properties for high-temperature nuclear applications. The research targets the optimization of stress-relief temperatures to alleviate postbuild residual stresses, ensuring improvements in the microstructural corelated properties. A series of microstructural and mechanical evaluations were performed on LPBF-printed SS-316H samples which were subjected to annealing at temperatures varying between 650 °C and 850 °C. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses revealed that increasing the heattreatment temperature accelerated dislocation recovery. Vickers microhardness measurements showed an initial reduction in values, followed by stabilization over extended durations at all the temperatures. While higher temperatures facilitated faster recovery, they also promoted carbide precipitation along grain and solidification cell boundaries, narrowing the safe processing window. In contrast, heat treatment at 650°C preserved the cellular substructure and enabled controlled carbide precipitation over time. In conclusion, these findings highlight the importance of time–temperature optimization and suggest that 650°C for up to 2 h provides the most favorable balance between recovery and carbide control for a stress-relief treatment.

316 stainless steel↗

DOE OSTI2023

Novel materials irradiation and pre-characterization plans for high-power targetry applications

The multi-megawatt proton beams that will be employed at future accelerator complexes introduce many new challenges for next-generation targetry systems, primarily due to the increased levels of beam-induced radiation damage combined with thermal shock effects during a beam pulse. Novel material classes, such as high-entropy alloys and electro-spun nanofibers are currently being investigated as materials that will be more tolerant of these effects in high beam power applications. Low-energy ion irradiation will be used for pre-screening and down selecting candidate novel materials prior to prototypic high-energy irradiation studies. Specific nano and micro-scale characterization techniques will be used to evaluate the radiation damage and thermal shock resistance of the new materials. Irradiation induced lattice spacing alteration and defect concentrations, as well as mechanical and thermal properties of the novel materials will be measured and compared to those of conventional targetry materials. This poster will detail plans for initial low-energy ion irradiation tests, and the post-irradiation examination techniques that will be used to develop and screen these novel target materials.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NASA NTRS1992

Biodeterioration of materials in water reclamation systems

The chemicals produced by the microbial processes involved in the 'biofilms' which form on the surfaces of manned spacecraft water reclamation systems encompass both metals and organic poisons; both are potential hazards to astronaut health and the growth of the plants envisioned for closed-cycle life support systems. Image analysis is here shown to be a very useful technique for the study of biofilm formation on candidate water-processor materials for Space Station Freedom. The biodeterioration of materials exposed to biofilms can be swiftly evaluated by means of electrochemical impedance spectroscopy.

Ford, Tim↗

DOE OSTI2020

STRUCTURE AND PROPERTIES STUDY ON ENERGY MATERIALS: THERMOELECTRIC MATERIAL TETRAHEDRITE AND LITHIUM ION CONDUCTOR LiPON

Development of efficient energy materials is critical in order to ease the energy demand and reduce our dependence of fossil fuel. Thermoelectric materials are promising due to their capability of generating electrical power by recovering waste heat. The performance of thermoelectric materials is quantified by a dimensionless figure of merit zT, which depends on their properties such as electrical conductivity, Seebeck coefficient and thermal conductivity. Tetrahedrites, a copper antimony sulfosalt mineral, typified by Cu12-xMxSb4S13, where M is a transition metal element such as Ni, Zn, Fe or Mn, have great potential for thermoelectric application due to their relatively high zT (close to 1 at 700 K), earth-abundance, environmental friendliness, favorable electrical properties, and most importantly intrinsic low lattice thermal conductivity (less than 1 W m-1 K-1) in wide temperature. In addition to energy recovery, reliable energy storage devices are also emerging to relieve the energy demand and improve the efficiency of consuming energy resources. Lithium-ion batteries are known to be reliable and successful electrochemical energy storage devices and appliable in various aspects, including laptops, smartphones and electrical vehicles. Lithium phosphorous oxynitride (LiPON) are widely used as thin-film solid-state electrolytes in Li-ion battery, which is the only demonstrated solid-state electrolyte that is quite stable in direct contact with Li metal at potentials from 0-5 V. However, the structure of LiPON, the effects of N doping, and the origin of its good electrochemical stability remains inconclusive.In this thesis, reliable modeling techniques accompanied with experimental tools, are applied to study the thermoelectric material tetrahedrite and the ionic conductor LiPON, in order to study their structural and dynamical properties. Accurate and efficient density-functional theory (DFT) and density-functional tight-binding (DFTB) methods, combined with molecular dynamics (MD) simulations are utilized in order to investigate the structures and properties of these energy materials. The incoherent and coherent atomic dynamics study of tetrahedrite Cu10.5NiZn0.5Sb4S13 provides the origin of softening upon cooling by investigate the motion of Cu12e at different temperatures. The dynamic structure factors in the longitudinal and transverse direction will also be discussed. The Cu movement of Cu-rich tetrahedrite Cu14Sb4S13 is revealed by Cu self-diffusivity, nuclear density map and "nudged elastic band" (NEB). Moreover, we investigate the effect of simulation cell size and basis sets on the DFT-based MD simulation results using tetrahedrite Cu10Zn2Sb4S13 thermoelectric as a model material, showing the advantage of larger cell by accessing smaller Q range. In addition, the low-temperature structural properties of Cu12Sb4S13 is measured by neutron diffraction, which indicates that no cubic to tetragonal transition occurs at metal-semiconductor transition (MST) temperature. Thermoelectric properties such as Seebeck coefficient, electrical resistivity and electrical thermal conductivity will also be investigated. DFTB method is implemented to study the structure and transport properties of Li3PO4 and LiPON, while the exploration of N doping effect is included. Lastly, the LiPON/Li interphase will be revealed in order to study the origin of electrochemical stability

25 ENERGY STORAGE↗

DOE OSTI2020

STRUCTURE AND PROPERTIES STUDY ON ENERGY MATERIALS: THERMOELECTRIC MATERIAL TETRAHEDRITE AND LITHIUM ION CONDUCTOR

Development of efficient energy materials is critical in order to ease the energy demand and reduce our dependence of fossil fuel. Thermoelectric materials are promising due to their capability of generating electrical power by recovering waste heat. The performance of thermoelectric materials is quantified by a dimensionless figure of merit zT, which depends on their properties such as electrical conductivity, Seebeck coefficient and thermal conductivity. Tetrahedrites, a copper antimony sulfosalt mineral, typified by Cu 12-x MxSb 4 S 13 , where M is a transition metal element such as Ni, Zn, Fe or Mn, have great potential for thermoelectric application due to their relatively high zT (close to 1 at 700 K), earth-abundance, environmental friendliness, favorable electrical properties, and most importantly intrinsic low lattice thermal conductivity (less than 1 W m -1 K -1 ) in wide temperature. In addition to energy recovery, reliable energy storage devices are also emerging to relieve the energy demand and improve the efficiency of consuming energy resources. Lithium-ion batteries are known to be reliable and successful electrochemical energy storage devices and appliable in various aspects, including laptops, smartphones and electrical vehicles. Lithium phosphorous oxynitride (LiPON) are widely used as thin-film solid-state electrolytes in Li-ion battery, which is the only demonstrated solid-state electrolyte that is quite stable in direct contact with Li metal at potentials from 0-5 V. However, the structure of LiPON, the effects of N doping, and the origin of its good electrochemical stability remains inconclusive. In this thesis, reliable modeling techniques accompanied with experimental tools, are applied to study the thermoelectric material tetrahedrite and the ionic conductor LiPON, in order to study their structural and dynamical properties. Accurate and efficient density-functional theory (DFT) and density-functional tight-binding (DFTB) methods, combined with molecular dynamics (MD) simulations are utilized in order to investigate the structures and properties of these energy materials. The incoherent and coherent atomic dynamics study of tetrahedrite Cu 10.5 NiZn 0.5 Sb 4 S 13 provides the origin of softening upon cooling by investigate the motion of Cu12e at different temperatures. The dynamic structure factors in the longitudinal and transverse direction will also be discussed. The Cu movement of Cu-rich tetrahedrite Cu 14 Sb 4 S 13 is revealed by Cu self-diffusivity, nuclear density map and “nudged elastic band” (NEB). Moreover, we investigate the effect of simulation cell size and basis sets on the DFT-based MD simulation results using tetrahedrite Cu1 0 Zn 2 Sb 4 S 13 thermoelectric as a model material, showing the advantage of larger cell by accessing smaller Q range. In addition, the low-temperature structural properties of Cu 12 Sb 4 S 13 is measured by neutron diffraction, which indicates that no cubic to tetragonal transition occurs at metal-semiconductor transition (MST) temperature. Thermoelectric properties such as Seebeck coefficient, electrical resistivity and electrical thermal conductivity will also be investigated. DFTB method is implemented to study the structure and transport properties of Li 3 PO 4 and LiPON, while the exploration of N doping effect is included. Lastly, the LiPON/Li interphase will be revealed in order to study the origin of electrochemical stability.

Li, Junchao↗

NASA NTRS1995

Material Measurements Using Groundplane Apertures

A technique for material parameter determination using an aperture in a groundplane is studied. The material parameters are found by relating the measured reflected field in the aperture to a numerical model. Two apertures are studied which can have a variety of different material configurations covering the aperture. The aperture cross-sections studied are rectangular and coaxial. The material configurations involved combinations of single layer and dual layers with or without a resistive exterior resistive sheet. The resistivity of the resistive sheet can be specified to simulate a perfect electric conductor (PEC) backing (0 Ohms/square) to a free space backing (infinity Ohms/square). Numerical parameter studies and measurements were performed to assess the feasibility of the technique.

Komisarek, K.↗

NASA NTRS1995

Laboratory Studies of DIB Carriers

Spectroscopic studies of the following potential diffuse interstellar band (DIB) carriers are reviewed: unspecified organics, carbon chains, polycyclic aromatic hydrocarbons (PAHs), fullerenes and derivatives, as well as porphyrins and related material. An assessment of each is given, along with suggestions for further experimental studies needed to fully test each candidate. Of the experimental techniques in common use matrix isolation spectroscopy with neon matrices is the most appropriate for the DIBs. The low vapor pressure and high reactivity of these materials preclude gas phase studies on many of these species. At this point, given the type and quality of published data available, carbon chains and PARs are the most promising candidates for a number of the DIBs.

Allamandola, L. J.↗

NASA NTRS2006

Manned Spacecraft Requirements for Materials and Processes

A major cause of project failure can be attributed to an emphasized focus on end products and inadequate attention to resolving development risks during the initial phases of a project. The initial phases of a project, which we will call the "study period", are critical to determining project scope and costs, and can make or break most projects. If the requirements are not defined adequately, how can the scope be adequately determined, also how can the costs of the entire project be effectively estimated, and how can the risk of project success be accurately assessed? Using the proper material specifications and standards and incorporating these specifications and standards in the design process should be considered inherently crucial to the technical success of a project as just as importantly, crucial to the cost and schedule success. This paper will intertwine several important aspects or considerations for project success: 1) Characteristics of a "Good Material Requirement"; 2) Linking material requirements to the implementation of "Design for Manufacturing"; techniques and 3) The importance of decomposing materials requirements during the study phase/development phase to mitigate project risk for the maturation of technologies before the building of hardware.

Vaughn, Timothy P.↗

DOE OSTI2020

Dynamics of reconfigurable artificial spin ice: Toward magnonic functional materials

Over the past few years, the study of magnetization dynamics in artificial spin ices has become a vibrant field of study. Artificial spin ices are ensembles of geometrically arranged, interacting magnetic nanoislands, which display frustration by design. These were initially created to mimic the behavior in rare earth pyrochlore materials and to study emergent behavior and frustration using two-dimensional magnetic measurement techniques. Recently, it has become clear that it is possible to create artificial spin ices, which can potentially be used as functional materials. In this perspective, we review the resonant behavior of spin ices in the GHz frequency range, focusing on their potential application as magnonic crystals. In magnonic crystals, spin waves are functionalized for logic applications by means of band structure engineering. While it has been established that artificial spin ices can possess rich mode spectra, the applicability of spin ices to create magnonic crystals hinges upon their reconfigurability. Consequently, we describe recent work aiming to develop techniques and create geometries allowing full reconfigurability of the spin ice magnetic state. We also discuss experimental, theoretical, and numerical methods for determining the spectral response of artificial spin ices and give an outlook on new directions for reconfigurable spin ices.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Electron tomography of unirradiated and irradiated nuclear graphite

Graphite is the moderator material of several Generation IV nuclear reactor concepts, as well as the British Advanced Gas-cooled Reactors (AGR). Porosity can heavily influence the material properties, mechanical irradiation response, and neutron induced shrinkage or swelling of nuclear-grade graphite. Due to the sub-micron size of several types of pores found in graphite, only a high-resolution imaging technique such as electron tomography are capable of visualizing these features in three dimensions. In this research, we used electron tomography to characterize as-received and neutron irradiated samples of IG-110 nuclear-grade graphite to show for the first time the 3D structure of both native and irradiation-induced nano-cracks. This technique also reveals unique characteristics of graphite such as the structure that surrounds pores and could be used to inform molecular dynamic simulations of irradiated graphite and experimental techniques such as gas-absorption. This work also shows the utility of this technique for the study of other nuclear porous carbon-based materials.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Smaller and faster: a review of conventional and nanocalorimetry techniques for determining thermophysical properties of nuclear materials

Thermal analysis of nuclear materials is critical for the advancement of nuclear technology. The heat effects associated with heat capacity, phase transformation, and radiation damage can be measured with conventional calorimeters. However, conventional calorimetric techniques are often restricted in terms of heating rate and sample mass, especially when studying the limited amounts of materials subject to extreme conditions. In this review, we summarize conventional calorimetric studies of critical thermophysical and thermochemical properties of pure actinide metals (U, Np, Am, Pu), fast reactor metallic fuel alloy systems (U–Zr, U–Pu–Zr, Pu–U, Pu–Zr), and actinide oxides that are primary constituents or transmutation products in light water reactor fuel rods (U–O, Np–O, Am–O, Pu–O, Pu–U–O). Adiabatic and drop calorimetry have been the primary techniques used for these studies, however the development of fast scanning calorimetry using micro-electro-mechanical-based systems allows determination of thermodynamic properties from smaller sample masses. We report recent investigations that leverage the fast heating rates of nanocalorimetry by itself or combined with other characterization techniques. Furthermore, we then discuss opportunities for nanocalorimetry to provide solutions to some of the technical challenges inherent in thermal analysis of nuclear materials, namely a reduction in sample activity, emulating heating transients, investigation of phase evolution in irradiated samples, and characterization of radiation damage evolution. Nanocalorimetry has the potential to significantly advance the understanding of thermophysical properties in nuclear materials and thus accelerate the development of nuclear technology.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Biobased chemical recycling: aminolysis of PET using renewable reagents and monomers to synthesize new semi-aromatic polyamides

Chemical recycling of PET is a method of depolymerizing polymer chains to monomeric components enabling the synthesis of second-generation materials with virgin-like quality. Commercial chemical recycling techniques rely upon high pressure methanolysis to create precursors capable of synthesizing a second-generation PET resin. However, despite the circular approach of methanolysis, a product with a very short lifespan and similar value is created. The approach of the current study is to utilize aminolysis as an ambient pressure technique to create precursors for higher value materials with longer lifespans to address the current crisis in plastic waste. Semi-aromatic polyamides (SAP) are desired in this circumstance because of their high melting point and heat resistance combined with good melt-processability similar to aliphatic polyamides. In this study SAPs were synthesized using precursors recovered from the aminolysis of PET employing biobased diamines and dicarboxylic acids. While aminolysis has been explored in previous studies, this work investigated the use of biobased components from castor oil: decamethylene diamine during recycling and sebacic acid during polymerization. Polymer synthesis resulted in the formation of SAPs similar to polyphthalamides (PPA) with novel structures given the aromatic portion from terephthalic acid (TPA) and aliphatic portion from the diamines and diacids. The synthesized materials exhibited excellent thermal stability with high glass transition temperatures. Novel polymers were created with varying aliphatic chain length to understand fundamental parameters needed to produce a valuable polymer from post-consumer waste.

High performance Applications↗

DOE OSTI2022

ICTAC Kinetics Committee recommendations for analysis of thermal decomposition kinetics

Here in this review article, the Kinetics Committee of the International Confederation for Thermal Analysis and Calorimetry (ICTAC) delivers a collection of recommendations for the kinetic analysis of thermal decomposition processes. These recommendations specifically focus on the thermal decomposition processes in inorganic, organic, and polymeric materials, as well as biomass and solid fuels. A general introduction to the kinetic analysis of thermal decompositions studied by thermal analysis techniques is followed by individual sections that discuss thermal decomposition of specific classes of materials and respective kinetic approaches. In each section, various kinetic analysis procedures are introduced with regard to specific features of the reactions and explained progressively from simple to complex reactions with examples of practical kinetic analysis. These recommendations are expected to provide a guidance for performing reliable and meaningful kinetic analysis in terms of practical usefulness and physico-chemical significance of the results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1977

Crystal growth in a low gravity environment

Crystal growth in microgravity possesses several distinct technological advantages over earth-bound processes; containerless handling and reduction of density gradient driven as well as sedimentation flows. Experiments performed in space to date have been basically reproductions of processes currently used on earth and the results have clarified our understanding of crystal growth dynamics. In addition, both unresolved problems and areas requiring further study on earth have been identified. Future work in space processing of materials must address these areas of study as soon as possible if the full potential of a space environment to develop new techniques and materials is to be realized.

Carruthers, J. R.↗

NASA NTRS1998

Experiments on Nucleation in Different Flow Regimes

The vast majority of metallic engineering materials are solidified from the liquid phase. Understanding the solidification process is essential to control microstructure, which in turn, determines the properties of materials. The genesis of solidification is nucleation, where the first stable solid forms from the liquid phase. Nucleation kinetics determine the degree of undercooling and phase selection. As such, it is important to understand nucleation phenomena in order to control solidification or glass formation in metals and alloys. Early experiments in nucleation kinetics were accomplished by droplet dispersion methods. Dilitometry was used by Turnbull and others, and more recently differential thermal analysis and differential scanning calorimetry have been used for kinetic studies. These techniques have enjoyed success; however, there are difficulties with these experiments. Since materials are dispersed in a medium, the character of the emulsion/metal interface affects the nucleation behavior. Statistics are derived from the large number of particles observed in a single experiment, but dispersions have a finite size distribution which adds to the uncertainty of the kinetic determinations. Even though temperature can be controlled quite well before the onset of nucleation, the release of the latent heat of fusion during nucleation of particles complicates the assumption of isothermality during these experiments. Containerless processing has enabled another approach to the study of nucleation kinetics. With levitation techniques it is possible to undercool one sample to nucleation repeatedly in a controlled manner, such that the statistics of the nucleation process can be derived from multiple experiments on a single sample. The authors have fully developed the analysis of nucleation experiments on single samples following the suggestions of Skripov. The advantage of these experiments is that the samples are directly observable. The nucleation temperature can be measured by noncontact optical pyrometry, the mass of the sample is known, and post-processing analysis can be conducted on the sample. The disadvantages are that temperature measurement must have exceptionally high precision, and it is not possible to isolate specific heterogeneous sites as in droplet dispersions. Levitation processing of refractory materials in ultra high vacuum provides an avenue to conduct these kinetic studies on single samples. Two experimental methods have been identified where ultra high vacuum experiments are possible; electrostatic levitation in ground-based experiments and electromagnetic processing in low earth orbit on TEMPUS. Such experiments, reported here, were conducted on zirconium. Liquid zirconium is an excellent solvent and has a high solubility for contaminants contained in the bulk material as well as those contaminants found in the vacuum environment. Oxides, nitrides, and carbides do not exist in the melt, and do not form on the surface of molten zirconium, for the materials and vacuum levels used in this study. Ground-based experiments with electrostatic levitation have shown that the statistical nucleation kinetic experiments are viable and yield results which are consistent with classical nucleation theory. The advantage of low earth orbit experiments is the ability to vary the flow conditions in the liquid prior to nucleation. The put-pose of nucleation experiments in TEMPUS was to examine.

Bayuzick, R. J.↗

DOE OSTI2021

Computing inelastic neutron scattering spectra from molecular dynamics trajectories

Abstract Inelastic neutron scattering (INS) provides a weighted density of phonon modes. Currently, INS spectra can only be interpreted for perfectly crystalline materials because of high computational cost for electronic simulations. INS has the potential to provide detailed morphological information if sufficiently large volumes and appropriate structural variety are simulated. Here, we propose a method that allows direct comparison between INS data with molecular dynamics simulations, a simulation method that is frequently used to simulate semicrystalline/amorphous materials. We illustrate the technique by analyzing spectra of a well-studied conjugated polymer, poly(3-hexylthiophene-2,5-diyl) (P3HT) and conclude that our technique provides improved volume and structural variety, but that the classical force field requires improvement before the morphology can be accurately interpreted.

36 MATERIALS SCIENCE↗

NASA NTRS1977

Minimum-mass design of filamentary composite panels under combined loads: Design procedure based on a rigorous buckling analysis

A procedure is presented for designing uniaxially stiffened panels made of composite material and subjected to combined inplane loads. The procedure uses a rigorous buckling analysis and nonlinear mathematical programing techniques. Design studies carried out with the procedure consider hat-stiffened and corrugated panels made of graphite-epoxy material. Combined longitudinal compression and shear and combined longitudinal and transverse compression are the loadings used in the studies. The capability to tailor the buckling response of a panel is also explored. Finally, the adequacy of another, simpler, analysis-design procedure is examined.

Stroud, W. J.↗

DOE OSTI2020

Characterizing material transitions in large-scale Additive Manufacturing

Integrating Multiple Materials (MM) into large-scale Additive Manufacturing (AM) is a key for various industrial applications wishing to incorporate site-specific properties into geometrically complex designs that are difficult to manufacture with traditional techniques. Printing with multiple materials is typically accomplished by using layers as natural material boundaries, but having the capability to switch between materials within a single layer without pausing would further expand MM possibilities. This study used Cincinnati Incorporated’s Big Area Additive Manufacturing (BAAM) system to explore material transitions with a novel dual-hopper that enables in-situ material blending of a pelletized feedstock. Constructing MM and functionally graded material (FGM) structures requires depositing a specific material composition at a specific geometric location to achieve a desired performance. Furthermore, accurately implementing this with the BAAM’s blended extrusion system requires a thorough understanding of the transition between distinct material compositions. This study characterizes a step-change transition between neat acrylonitrile butadiene styrene (ABS) and carbon fiber-reinforced ABS. Three distinct techniques were compared for analyzing the fiber content, and the transition zone between materials was characterized as a function of transition direction. The transition process was consistent to within 0.7 wt% carbon fiber variation between different layers and prints. The transition between materials was found to be directionally dependent, with ABS to CF/ABS having a transition length of 3.5 m compared to 3.2 m for CF/ABS to ABS. Furthermore, the transition from Material A to Material B was found to be repeatable with a possible variance in transition length of 0.3 m.

36 MATERIALS SCIENCE↗