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Results for “AM Powder Characterization”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

A Crystalline Polyimide Porous Organic Framework for Selective Adsorption of Acetylene over Ethylene

The separation of acetylene from ethylene is a crucial process in the petrochemical industry, as even small acetylene impurities can lead to premature termination of ethylene polymerization. Herein, we present the synthesis of a robust, crystalline naphthalene diimide porous aromatic framework via imidization of linear naphthalene-1,4,5,8-tetracarboxylic dianhydride and triangular tris(4-aminophenyl)amine. The resulting material, PAF-110, exhibits impressive thermal and long-term structural stability, as indicated by thermogravimetric analysis and powder X-ray diffraction characterization. Gas adsorption characterization reveals that PAF-110 has a capacity for acetylene that is more than twice its ethylene capacity at 273 K and 1 bar, and it exhibits a moderate acetylene selectivity of 3.9 at 298 K and 1 bar. Complementary computational investigation of each guest binding in PAF-110 suggests that this affinity and selectivity for acetylene arises from its stronger electrostatic interaction with the carbonyl oxygen atoms of the framework. As a result, to the best of our knowledge, PAF-110 is the first crystalline porous organic material to exhibit selective adsorption of acetylene over ethylene, and its properties may provide insight into the further optimized design of porous organic materials for this key gas separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

The grain-size effect on thermal conductivity of uranium dioxide

We have investigated the grain-boundary scattering effect on the thermal transport behavior of uranium dioxide (UO 2 ). The polycrystalline samples having different grain-sizes (0.125, 1.8, and 7:2 µm) have been prepared by a spark plasma sintering technique and characterized by x-ray powder diffraction, scanning electron microscope, and Raman spectroscopy. The thermal transport properties (the thermal conductivity and thermoelectric power) have been measured in the temperature range of 2–300 K, and the results were analyzed in terms of various physical parameters contributing to thermal conductivity in these materials in relation to grain-size. We show that thermal conductivity decreases systematically with lowering grain-size in the temperatures below 30 K, where the boundary scattering dominates the thermal transport. At higher temperatures, more scattering processes are involved in the heat transport in these materials, making the analysis difficult. We determined the grain-boundary Kapitza resistance that would result in the observed increase in thermal conductivity with grain-size and compared the value with Kapitza resistances calculated for UO 2 using molecular dynamics from the literature.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of cobalt substitution on the magnetism of NiBr 2

Co-substituted Ni 1-x Co x Br 2 (0≤x≤1) single crystals were synthesized using vapor transport. As a result, the physical properties of the crystals were characterized by x-ray powder diffraction, magnetization, and specific-heat measurements. Room-temperature x-ray powder diffraction data indicate that a change from the CdCl 2 structure type to the CdI 2 structure type occurs within 0.56 2 has a commensurate antiferromagnetic phase below T N ≈ 46 K and an incommensurate magnetic ground state below T IC ≈ 20 K. Both magnetic transitions are affected by cobalt substitution, and the incommensurate phase transition is present up to at least x=0.56. Here, the evolution of magnetism has been studied as a function of cobalt content and is summarized in the temperature-composition phase diagram.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The T 2 structure of polycrystalline cubic human insulin

The polymorphism of human insulin upon pH variation was characterized via X-ray powder diffraction, employing a crystallization protocol previously established for co-crystallization with phenolic derivatives. Two distinct rhombohedral ( R 3) polymorphs and one cubic ( I 2 1 3) polymorph were identified with increasing pH, corresponding to the T 6 , T 3 R 3 f and T 2 conformations of insulin, respectively. The structure of the cubic T 2 polymorph was determined via multi-profile stereochemically restrained Rietveld refinement at 2.7 Å resolution. This constitutes the first cubic insulin structure to be determined from crystals grown in the presence of zinc ions, although no zinc binding was observed. The differences of the polycrystalline variant from other cubic insulin structures, as well as the nature of the pH-driven phase transitions, are discussed in detail.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

Characterization Report on Fuels for NEAMS Model Variation

We have investigated the grain boundary scattering effect on the thermal transport behavior of uranium dioxide (UO 2 ). The polycrystalline samples having different grain sizes (0.125, 1.8, and 7.2 μm) have been prepared by spark plasma sintering technique and characterized by x-ray powder diffraction (XRD), scanning electron microscope (SEM), and Raman spectroscopy. The thermal transport properties (the thermal conductivity and thermoelectric power) have been measured in the temperature range 2-300 K and the results were analyzed in terms of various physical parameters contributing to the thermal conductivity in these materials in relation to grain-size. We show that thermal conductivity decreases systematically with lowering grain-size in the temperatures below 30 K, where the boundary scattering dominates the thermal transport. At higher temperatures more scattering processes are involved in the heat transport in these materials. We analyzed the results obtained using molecular dynamics (MD) calculations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Understanding Microstructural Effects on Dynamic Performance Towards the Development of Shock Metamaterials

With the recent advances in additive manufacturing (AM), long-range periodic lattice assemblies are being developed for vibration and shock mitigation components in aerospace and military applications with unique geometric and topological structures. There has been extensive work in understanding the static properties associated with varying topology of these lattice architectures, but there is almost no understanding of microstructural affects in such structures under high-strain rate dynamic loading conditions. Here we report the shock behavior of lattices with varying intrinsic grain structures achieved by post process annealing. High resolution 316L stainless steel lattices were 3D printed by a laser-powder bed fusion machine and characterized by computed tomography. Subsequent annealing resulted in stress-relieved and recrystallized lattices. Overall the lattices had strong cubic texture aligning with the x-, y- and z-directions of the build with a preference outside the build direction (z). The recrystallized sample had more equiaxed polygonal grains and a layer of BCC ferrite at the surface of the structure approximately 1 grain thick. Upon dynamic compression the as-deposited lattice showed steady compaction behavior while the heat-treated lattices exhibit negative velocity behavior indicative of failure. We attribute this to the stiffer BCC ferrite in the annealed lattices becoming damaged and fragmenting during compression.

36 MATERIALS SCIENCE↗
DOE OSTI2022

New NDA Methods for Thorium Fuel Cycle Safeguards (Mid-Project Report)

This project is developing new Non-Destructive Assay (NDA) safeguards techniques for emergent thorium fuel cycles based on Neutron Resonance Transmission Analysis (NRTA), which can assay 233 U and 235 U when they are present together in a sample with potentially high gamma-ray backgrounds from fission products and 232 U. Existing passive techniques face large challenges for this task so new active interrogation methods are needed. This effort is also exploring how gamma-ray signatures can complement NRTA for enhanced assayed performance. This project leverages an NRTA system being developed at PNNL in collaboration with MIT, which uses a commercially available deuterium-tritium neutron generator at short standoff (~2 m). We aim to assess the feasibility and performance of these new NDA techniques for the range of relevant samples in thorium fuel cycles. Key advancements described in this mid-project report include NRTA system design for thorium safeguards measurements, characterization of 233 U oxide powder at PNNL, a survey of detector technologies suitable for NRTA in high gamma background environments, successful preliminary demonstration of a quantitative isotopic estimation algorithm, and first NRTA measurements of a thorium sample.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

A&L Annual Report: GRM-MAPS

Exploding Bridge Wire (EBW) is an important design for initiating detonators relevant to several LLNL systems. In such designs, a metal bridge wire is in direct contact with a porous secondary high explosive (HE), typically pressed to around 50% of its crystalline density. Initiation is believed to occur through shock waves generated when the bridge wire is made to explode via the rapid passing of a strong current pulse. Permeametry is an important characterization tool for the porous powdered HE (PETN, HMX, etc.) component in such devices. Such powders are well known to coarsen with age, with an accompanying deterioration in performance, which includes increased function time and sensitivity. Among various material characteristics, one that has been shown to correlate the most with such performance parameters is the flow-permeable surface area (FSSA), measured using air-permeametry. Commercially available permeametry apparatuses, such as that from Fisher Scientific or a more modern version from Micromeritics suffer from a few drawbacks, most notably as related to monitoring age-related changes in FSSA. This is because it requires re-compaction of the aged powder into the permeametry tube, which in most cases leads to an unwanted increase in FSSA. To address this and a few other shortcomings, we have been developing a modern version of the permeameter, Gee-Reinstein-Maiti Modern Air-Permeametry System (GRM-MAPS). In this report, we summarize progress made in FY25 toward perfecting and calibrating the instrument, which we aim at deploying within surveillance in FY26.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fractal nature structure reconstruction method in designing microstructure properties

Highlights: • Structure and material’s properties, within the material’s consolidation triad: Synthesis – Structure – Properties. • The grain prediction methods is based on the measurements of the solid Euclidean geometric fractal characteristics. • The intergranular contacts inside the BaTiO3 -ceramic are responsible for intergranular capacities. • The inner complex geometry of intergrain contacts imposes fractal correction factor for permeability. - Abstract: In the process of predicting materials properties, it is necessary to predict microstructures. This is important for ceramic materials, for the purpose of miniaturization and for a higher level of integration. Although the method of material structure reconstruction is for the first time used on BaTiO{sub 3}-ceramics by these authors, it can also be used for silicate, refractory and other ceramics, and, for any powder-based material. The reconstruction is based on the grain perimeter fractal analysis and the Richardson method. The main contribution of this paper is establishing the relationship between the electronic properties of BaTiO{sub 3}-ceramics and its microstructural fractal nature. Similar relations can be used for any ceramics or even any materials. The samples consolidation includes both powder pressing (cold sintering phase) and sintering in a furnace (hot sintering phase). The fractal nature characterization has a very important role from the powder phase up to the final microstructure, through which structures it directly impacts electro-physical and other ceramics properties. Thereby, the new possibilities in the microstructure characterization applications are directly introduced to an engineering system, providing the new solutions related to computer aided support. This creates new industrial production and application possibilities, especially in the process of ceramics material consolidation, now based on microstructural properties, which is providing a basis for “fractal electronics’’ development.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Comparison of Electron Beam and Laser Beam Powder Bed Fusion Additive Manufacturing Process for High Temperature Turbine Component Materials, Phase II. CRADA Final Report

The evolving additive manufacturing (AM) technology is now at the point where some metallic turbine components are being fabricated for both development and production purposes. The goal of this phase II project is to continue the evaluation of AM Nickel Alloy X fabricated by electron beam (EB) or laser beam (LB) powder bed fusion (PBF) process for gas turbine applications. Microstructure, mechanical and oxidation properties characterization was conducted on test specimens produced with powders of different chemistries within the typical material specification range. Powders with high Silicon (Si) content for the LB-PBF and low Si content for the EB-PBF displayed significant cracking levels in the AM Nickel Alloy X material. Accordingly, optimum fatigue performance would require careful control of powder chemistry, optimization of the fabrication parameters for a given powder and use of hot isostatic pressing (HIP) post treatment. Oxidation testing conducted at 1472°F (800ºC) in air showed that the roughness of the EB-PBF specimens led to an increase in specimen mass change, but overall the AM specimens exhibited oxidation behavior at 1472°F (800ºC) that is appropriate for applications in gas turbine engines. Assessment of the geometric capability of the LB-PBF and EBPBF systems using artifacts representative of turbine component geometries revealed that the LB-PBF process is well-suited for the fabrication of intricate geometries needed for turbine engine fuel injector components, but further process development is required to improve the EB-PBF system feature resolution.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanostructured Powders Made from Flame Spray Pyrolysis for Li-Ion Cathode

Flame processes are the most economic ones to produce fine powders and have been used to produce pigment titanium oxide and fused silica in large volumes. In this work a flame spray pyrolysis (FSP) process is used to make positive electrode materials for Li-ion battery, which is made of complex metal oxide powders, such as Li(Ni1/3Mn1/3Co1/3)O2. In particular, the work was focused on making the NMC materials with stoichiometric compositions and desired morphologies. During the pyrolysis process different morphologies can be formed, involving often powders with primary nanoparticles. Such nanostructures were found to have affected the battery performance. Detailed results of the synthesis, characterization, and battery testing of the NMC powder materials will be presented.

25 ENERGY STORAGE↗
DOE OSTI2018

Microstructure and nanoindentation analysis of Mg-SiC nanocomposite powders synthesized by mechanical milling

Highlights: • Mechanical milling as an effective solution to reach a homogeneous distribution of SiC nanoparticles up to 10 vol% in Mg matrix • No deformation twinning in the nanostructured Mg matrix even after the severe plastic deformation and hard SiC nanoparticles up to 10 vol%. • Significant enhancement of nanohardness and reduced elastic modulus in the milled nanocomposite powders - Abstract: Mixtures of magnesium powder and SiC nanoparticles at various volume fractions were mechanically milled to produce nanocrystalline Mg-SiC nanocomposites. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were utilized to characterize the microstructure of the milled powders. The microstructural evidences revealed that mechanical milling is a proper method to achieve a uniform distribution of the SiC nanoparticles, even up to 10% in the Mg matrix. Based on the results, higher volume fraction of the SiC nanoparticles raise the value of measured microstrain and reduce the crystallite size of the Mg matrix. The TEM results pointed to the fact that no deformation twinning takes place in the nanostructured Mg matrix even after severe plastic deformation through mechanical milling and the presence of hard SiC nanoparticles up to 10 vol%. The effects of nanoparticle volume fraction on mechanical properties of the milled Mg-SiC nanocomposites were evaluated using nanoindentation tests. The results clearly showed a significant enhancement of nanohardness and reduced elastic modulus in the milled powders compared to that of the reference material namely as-received pure magnesium. It was found that the SiC nanoparticles (even up to 10 vol%), well distributed in the magnesium matrix, remarkably improve the reduced elastic modulus and nanohardness of the nanocomposite powders.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Lithography-based Ceramics Manufacturing Technologies

In this work, surrogate powders were prepared with lithography-based ceramic printing. Lanthanum oxide, a powder from Oak Ridge National Laboratory (ORNL), was prepared by milling, characterizing, and printing of coupon samples. The printing resulted in net-shaped green parts. Alumina, a more developed powder, was also printed and characterized at ORNL, and these parts were surrogate geometries larger than coupons that were sintered to net shape within 0.3% of the desired geometry.

36 MATERIALS SCIENCE↗
DOE OSTI2026

A solid-state extrusion pathway extensible to upcycling aluminum scrap and end-of-life permanent magnets into ductile Al-6061/SmCo 5 structural magnetic composites

Permanent magnets offer strong potential for multifunctional structural components, but their inherent brittleness limits direct integration. Here, SolidStir® Extrusion (SSE) is used to embed SmCo5 powder into AA6061 in the solid state, and the resulting microstructure, interfacial chemistry, mechanical properties, and magnetic response are systematically characterized. SSE fragments the initial SmCo 5 powder into predominantly fine particles dispersed within an ultrafine Al matrix, with a volume fraction of ∼ 4–6 % in this proof-of-concept study. Interfacial reactions form a continuous Al–Co reaction layer, with local atomic-resolution indexing consistent with Al 13 Co 4 , together with Sm–Si-rich reaction products, while the matrix contains Sm–Co–Si-rich precipitates and Mg 2 Si, producing features from nanometers to micrometers. Compared with an Al extrudate, this architecture increases yield strength by ∼ 42 % and tensile strength by ∼ 31 %, while preserving uniform elongation, and it sustains work hardening in compression from 150 to 400 °C. The composite retained hard-magnetic behavior, with axial magnetization of 12.7 A·m 2 kg −1 at 6 T and intrinsic coercivity of 9.6 kOe. These findings demonstrate that SSE can produce Al-based load-bearing magnetic composites while preserving useful SmCo5 functionality.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Polycapillary x-ray lenses for single-shot, laser-driven powder diffraction

X-ray diffraction measurements to characterize phase transitions of dynamically compressed, high-Z matter at Mbar pressures require both sufficient photon energy and fluence to create data with high fidelity in a single shot. Large-scale laser systems can be used to generate x-ray sources above 10 keV utilizing line radiation of mid-Z elements. However, the laser-to-x-ray energy conversion efficiency at these energies is low, and thermal x-rays or hot electrons result in unwanted background. We employ polycapillary x-ray lenses in powder x-ray diffraction measurements using solid target x-ray emission from either the Z-Beamlet (ZBL) long-pulse or the Z-Petawatt (ZPW) short-pulse laser systems at Sandia National Laboratories. Polycapillary lenses allow for a 100-fold fluence increase compared to a conventional pinhole aperture while simultaneously reducing the background significantly. This enables diffraction measurements up to 16 keV at the few-photon signal level as well as diffraction experiments with ZPW at full intensity.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

The evolution history of superalloy powders during hot consolidation and plastic deformation

Highlights: • Element segregations in a powder metallurgy superalloy at different states are identified. • The surface energy drives precipitation of oxides, carbides, and γ' particles on powder surface during hot consolidation. • Prior particle boundary structure is distorted and more uniformly refined grains are obtained after hot extrusion. - Abstract: Powder metallurgy superalloys are widely used to produce critical rotating parts in turbine engines. However, the issues like what is the driving force of precipitation on prior particle boundary (PPB) during consolidation and how the PPB structure evolves during plastic deformation still remain to be resolved. In this study, with the characterization of the microstructure evolution from powder, consolidation, to plastic deformation, the segregation of alloying elements on the particle boundaries at elevated temperature was analyzed by equilibrium thermodynamic calculations, and the distortion of PPB structure under large plastic deformation was quantitively simulated by finite element (FE) methods. The results indicated that surface energy serves as the main driving force of PPB precipitation and hot extrusion could distort the PPB structure and yield more uniformly refined grains.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Supply Chain Improvement & Process Modification Printing in Tantalum

Refractory metals and alloys are distinguished by their exceptional thermophysical properties, including high melting and recrystallization temperatures, remarkable strength, and superior corrosion resistance, all of which surpass those of conventional alloys. These unique characteristics position these materials as ideal candidates for applications in extreme environments. However, their potential has historically been underexploited due to limitations in processing capabilities. Recent advancements in melt-based additive manufacturing (AM) processes present opportunities to overcome these limitations. Previous Sandia studies have successfully characterized pure tantalum produced through laser powder bed fusion (LPBF) externally at Castheon, revealing that LPBF-fabricated tantalum exhibits properties exceeding those of wrought materials. This promising outcome sparked increased interest in the internal additive manufacturing of tantalum. This project aimed to establish the new SLM 280 machine at SNL-CA to successfully produce the first tantalum prints and characterize the material. Additionally, efforts were made to enhance the machine by incorporating Inert equipment to minimize oxygen content within the print volume. The results demonstrated that internally manufactured LPBF tantalum not only met but exceeded the standards of wrought materials, even prior to the integration of the additional equipment. The inert equipment is almost successfully integrated and ready for use. Future research should focus on understanding how this equipment influences the process-structure-property relationships, as well as further optimizing the printing parameters for tantalum.

36 MATERIALS SCIENCE↗