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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 415 records · Page 23
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Enhanced flexibility and thermal conductivity of HfC decorated carbon nanofiber mats

Future-generation spacecraft components allude discovery of novel materials that can withstand extreme environments (>2000 °C). The combined effect of ultra-high temperature ceramics (UHTCs) and carbon fibers (C f ) can satisfy the demanding requirements of aerospace applications. A novel, hybrid, and flexible hafnium carbide (HfC)-decorated carbon nanofiber (C nf ) mat was fabricated via electrospinning. Enhanced thermal stability of the flexible HfC decorated C nf over C nf can be elucidated from the 20-fold increment in thermal conductivity and the onset of degradation at higher temperatures (840 °C). Successful integration of multi-layered sandwich lattice using in-housed fabricated HfC decorated C nf showed retention of the fibrous structure even after extreme spark plasma sintering (SPS) process at 1850 °C. Fabricating a similar multi-layered structure using procured C f was unsuccessful due to bundled agglomeration and micron-sized fibers. High-load indentation suggests that HfC decorated C nf interlayer is stronger (~2.3 times) than the parent UHTC with no cracking at the interface. Compared with the HfC matrix, the indentation-damaged area at the interface reduced up to ~56% due to toughening mechanisms such as C nf , fiber pull-out and bridging. The synthesized HfC decorated Cnf mat is proposed as an ultra-thin filler material for joining similar or dissimilar UHTCs while maintaining similar chemistry and better mechanical integrity at the interface. Furthermore, the findings insinuate a new paradigm in designing hybrid and flexible ceramic-containing materials for thermal protection systems (TPS) of future-generation spacecraft components that can mitigate failure in extreme environments (>2000 °C).

36 MATERIALS SCIENCE↗
DOE OSTI2021

Synthesis and behavior of bulk iron nitride soft magnets via high-pressure spark plasma sintering

Abstract In this study, dense bulk iron nitrides (Fe x N) were synthesized for the first time ever using spark plasma sintering (SPS) of Fe x N powders. The Fe 4 N phase of iron nitride in particular has significant potential to serve as a new soft magnetic material in both transformer and inductor cores and electrical machines. The density of SPSed Fe x N increased with SPS temperature and pressure. The microstructure of the consolidated bulk Fe x N was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. XRD revealed a primary phase of Fe 4 N with secondary phases of Fe 3 N and metallic iron. Finite element analysis (FEA) was also applied to investigate and explain localized heating and temperature distribution during SPS. The effects of processing on interface bonding formation and phase evolution were investigated and discussed in detail to provide insight into fundamental phenomena and microstructural evolution in SPSed Fe x N. Graphic abstract

36 MATERIALS SCIENCE↗
DOE OSTI2024

The evolution of model Rh/Fe 3 O 4 (001) catalysts in hydrogen environments

Single metal atoms dispersed on oxides are a new emerging class of catalysts owing to their unique electronic and chemical properties. Here, in this study, we have prepared a series of model single-atom catalysts possessing well-characterized Rh sites that include Rh adatoms (Rh ad ), mixed surface layers with octahedrally-coordinated Rh (Rh oct ), as well as metallic Rh clusters and nanoparticles (Rh met ) on Fe 3 O 4 (001). Using X-ray photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM), we investigated the activity of such model systems towards H2 and their stability in reducing environments. Our results show that the atomically dispersed Rhad and Rhoct species do not activate H 2 , which would result in the formation of surface hydroxyls on Fe 3 O 4 (001). In contrast, the presence of Rh met in H 2 results in the formation of hydroxyls and subsequent etching of the Fe 3 O 4 (001) at higher temperatures (≥ 500 K) due to water formation via the Mars-van Krevelen mechanism. Additionally, such surface etching leads to the release of the Rh oct from the surface lattice and their sintering to Rh met . To bridge the material gap between the surface science models and high surface area catalysts, we perform parallel studies on powder Rh/Fe 3 O 4 catalysts. The XPS characterization shows remarkable similarities between these systems. Further, our surface science studies provide an atomistic picture of the behavior of high surface area catalysts in the H 2 atmosphere.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Investigation of Cu Species in Dealuminated Beta Zeolite Studied by Operando Closed-Cell Gas Reaction STEM

Direct conversion of ethanol to C3+ olefins is an attractive pathway to produce sustainable aviation fuels [1]. We recently reported a copper-containing catalyst supported on dealuminated (DeAl) beta zeolite that is capable of catalyzing cascade ethanol to olefins reactions with high olefins selectivity (88% C3+ olefin selectivity at 100% ethanol conversion). However, one of the deactivation mechanisms of the catalyst is copper sintering [2]. It was found that copper agglomerates can be redispersed through a simple oxidative treatment. To better understand the kinetics and process conditions conducive to redispersion, we studied the atmosphere and temperature dependent Cu species in Cu/DeAl-Beta catalyst under conditions matching those of the working catalyst.

beta zeolite↗
DOE OSTI2026

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗
DOE OSTI2020

Role of phosphate source in improving the proton conductivity of tin pyrophosphate and its composite electrolytes

Metal pyrophosphates (MPPs) in general, and tin pyrophosphate (TPP) in particular, have received significant interest in the last decade due to their potential as proton conductors for electrolyte application in intermediate temperature (IT)-fuel cells. However, for MPP based electrolytes, despite high reported proton conductivities, achieving good fuel cell performance and high open circuit voltage (OCV) remains a challenge with synthesis methods playing a crucial role in determining the final proton conductivity. Here we report the role of phosphate precursor in determining the TPP proton conductivity by examining five different precursors: (1) phosphoric acid (TPP-PA), (2) ammonium hydroxide + phosphoric acid (TPP-NH 4 OH), (3) diammonium phosphate (TPP-DAP), (4) tetramethylammonium sulphate + phosphoric acid (TPP-TMAP), and (5) tetrabutylammonium phosphate (TPP-TBAP), where a maximum conductivity of 88 mS cm -1 at 200 °C was obtained for TPP prepared from the TBAP precursor. TPP prepared from all of the different precursors formed the crystalline cubic Pa-3 with combining macron] phase after sintering at 650 °C for 2.5 hours. Furthermore, TPP-TBAP/Nafion® composite membranes prepared with a 90 : 10 ratio exhibited an OCV of 0.98 V and produced a maximum peak power density (PPD) of 630 mW cm -2 at an operating temperature of 220 °C. Our results demonstrate the significant impact of the TPP precursor on proton conductivity and fuel cell performance.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Neural Learning Based Blind Source Separation for Detection of Material Defects in Pulsed Thermography Images

In this paper, we introduce a neural learning-based approach to blind source separation for detection of material flaws in pulsed thermography (PT) images. This approach can be used to detect internal defects (pores) in metallic Additively Manufactured (AM) materials. Such defects occur in high-strength alloys produced with direct laser sintering AM method for nuclear energy applications. Pulsed thermal imaging system utilizes a high intensity flash lamp to rapidly heat surface of sample, a high sensitivity infrared camera to capture data of surface temperature variations. The data cube obtained with PT (stack of surface temperature images at different times) can be analyzed with image processing algorithms to detect material defects. Compared with conventional nondestructive evaluation (NDE) methods, such as digital radiography and ultrasonic testing, the PT pulsed infrared thermal detection technique has advantages of one-sided non-contact measurements, fast processing of large sample areas captured in one image. Detection of small material defects requires finding features in thermal images, which have signal contrast levels approaching sensitivity limit of IR camera. In this study, an optimized Neural Learning based Blind Source Separation (NLBSS) algorithm, including Principal Component Analysis (PCA), and Independent Component Analysis (ICA) is demonstrated to automatically extract principal temporal and spatial features of thermography frames to enhance flaw detection. By using the NLBSS algorithm, material internal defects can be automatically detected. Furthermore, this processing approach compensates for experimental thermal imaging artifacts, such as noise and uneven heating. By merging artificial intelligence with the photothermic, the NDE system detects internal calibrated defects of various sizes and depths in AM nuclear-grade metallic alloys.

Zhang, Xin↗
DOE OSTI2023

Reactive flash sintering of TiZrN and TiAlN ternary metal nitrides

Here, this study demonstrated the reactive flash sintering (RFS) for two powder mixtures: TiN-ZrN (both conducting) and AlN-TiN (TiN conducting but AlN insulating), targeting ternary metal nitrides (TMN) of Ti 0.5 Zr 0.5 N and Ti 0.5 Al 0.5 N, respectively. A constant volage and pressure (e.g., 8 V DC, ∼15 MPa) at room temperature triggered the flash (current density up to 27 A/mm 2 ) without pre-heating, and the entire RFS process finished in a few minutes. For TiZrN, the flash was instantaneous whereas for TiAlN, there was a long incubation before the flash followed by a quick and dramatic flash. Both conventional ex situ XRD and in situ synchrotron study had been carried out. They showed a uniform Ti 0.57 Zr 0.43 N solution formed in RFS and persisted upon cooling, while (Ti, Al) N solid solution formed at high temperature was not stable and likely went through a very quick phase separation in the cooling process. The final products from RFS had been characterized using SEM/EDS for microstructure. Both TiZrN and TiAlN were dense. Distribution of Ti, Zr, and N was uniform for TiZrN; for TiAlN, Ti and N distribution was uniform, while association of Al with oxygen was observed. TGA-DSC revealed the onset oxidation temperature for TiZrN was comparable to TiN and ZrN, while it was higher by ∼200 °C for TiAlN, likely due to the formation of Al 2 O 3 . In terms of mechanical properties such as hardness or fracture toughness, forming a single-phase solid solution (like TiZrN) does not offer obvious benefits. while large grain size from RFS seemed to be unfavorable. Future optimization of RFS condition and in-depth study by both experiments and simulation are needed to fully understand the composition-processing-structure-property relationships for such TMN from the reactive flash sintering process.

Flash Sintering↗
DOE OSTI2020

In situ characterization of ceramic cold sintering by small-angle scattering

The first in situ characterization of the pore morphology evolution during the cold sintering process (CSP) is presented using small-angle X-ray scattering methods. For practical reasons, measurements have been made on a model system, KH 2 PO 4 (KDP). The scattering signal revealed a striking behavior that could be modeled with nanoscale structural features associated with the dissolution and reprecipitation of KDP close to the grain/pore interface during CSP. The prospects for future more quantitative experiments under a range of temperature and pressure conditions, as well as for studies of more technologically important materials such as ZnO are considered.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Thermal-Mechanical Analysis of an Additive Manufacturing Ceramic Heat Exchanger for High-Temperature Recuperator in a sCO2 Power System

Supercritical CO2 (sCO2) Brayton power cycle can be configured in a closed-loop power system and has a potentially high cycle efficiency. Compactness and high efficiency of a sCO2 power block make the sCO2 Brayton cycle a versatile power cycle in broad applications. While many heat sources are of sufficient intensity to produce high temperature working fluids to achieve high cycle efficiency, the thermal-mechanical stability of traditional materials (e.g., steels and nickel-based superalloys) used in construction of heat exchangers and turbine components limits the operating conditions and thus thermodynamic efficiency of the system. This effort seeks to establish the viability of ceramic heat exchanger technologies for the most extreme operating conditions envisioned for power generation and other high temperature processes. Heat exchangers constructed from ultra-high temperature ceramics, a class of extreme environment materials featuring melting points (Tmp.) above 3000 degrees C, is particularly appealing for sCO2 Brayton cycles given their ultra-low creep rates and very high retained strength at low homologous temperatures (i.e., T < 0.5 Tmp., or at least 1500 degrees C). To translate these materials properties to ultra-high temperature heat exchangers, innovations are required in ceramic manufacturing techniques to realize the complex architectures featured in compact heat exchangers with high power density. With appropriate processing, ZrB2-SiC based compositions can be sintered to near full density and shaped into complex topologies via ceramic additive manufacturing methods. This paper analyzes heat exchanger designs and explores thermal-mechanical implications of the operating environment. Thermal flow, heat transfer, and conjugate mechanical analyses provide insights into benefits and risks associated with the design approach.

additive manufacturing↗
DOE OSTI2020

Novel High Temperature Carbide and Boride Ceramics for Direct Power Extraction Electrode Applications. Final report

The current project aims to develop new carbide and boride ceramic materials that incorporate different metal elements (e.g., (Hf 1-x Zr x )B 2 , also called ceramic solid solutions) and understand the fundamental composition-processing-structure-property relationships for such materials. Specifically, nano powders and related nano-composites for selected mixed metal carbide and boride materials are synthesized from nano-scale mixed precursors obtained from solution-based processing via heat treatment in inert atmosphere. The obtained fine powders were then consolidated into dense ceramics via a novel flash sintering process. The mechanical properties and thermal oxidation resistance for the obtained materials were evaluated for these materials. It was found that different synthesis routes produced powders with somewhat different characteristics in terms of composition and microstructure, which then led to different properties for the final ceramics. The synthesis and processing methods demonstrated in this study might be adopted for developing other similar high temperature ceramics, while the mixed metal or solid solution ceramic materials obtained from this study might be used as hot electrodes for direction power extraction and other energy-related applications.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2024

Quantification of Swelling in Hematite Pellets Reduced Using Hydrogen–Nitrogen Gas Mixture

Iron ore pellets are reduced in a 50%H 2 –50%N 2 1 atm gas mixture at 750, 800, 850, 900, and 950 °C while simultaneously documenting swelling (change in pellet radius) and weight change. Swelling increases with increasing temperature, with catastrophic swelling (>20% of reduction swelling index) observed at 850, 900, and 950 °C. As the pellet is reduced, the pellet radius increases until 40–50% reduction is achieved, followed by a decrease in diameter beyond 40–50% reduction at 750 and 850 °C. At 950 °C, the pellet radius continues to increase with additional pellet reduction without any subsequent decrease in diameter. Scanning electron microscopy (SEM) analysis shows that the neighboring grains inside the pellet sinter together at 750 and 850 °C, whereas the individual grains sinter internally at 950 °C. SEM analysis and observations suggest that the reduction process at 750 and 850 °C can be approximated as a topochemical reaction process, while the reduction process at 950 °C can no longer be approximated as a topochemical reaction process. In conclusion, an empirical equation for the radius of the pellet is derived with fitting parameters dependent on temperature and the degree of reduction of the pellet undergoing reduction based on the experimental data.

08 HYDROGEN↗
DOE OSTI2020

Cr-doped U 3 Si 2 composite fuels under steam corrosion

Dense Cr-doped U 3 Si 2 composite fuels were manufactured by spark plasma sintering, and the effects of Cr addition on mechanical properties and oxidation resistance were investigated. Furthermore, dynamic oxidation testing by thermogravimetric analysis revealed significantly improved oxidation resistance of U 3 Si 2 with minimal doping of 3 wt% Cr. The onset oxidation temperature increased to above 550 °C in air and ~520 °C in steam conditions for the 5 wt% and 10 wt% Cr-doped composites. Steam corrosion testing under 360 °C for 24 hours indicated well-maintained pellet integrity without pulverization for the 10 wt% Cr-doped U 3 Si 2 pellet which only showed minor surface oxidation. The first promising results open up the possibility of designing and manufacturing metal additive-doped U 3 Si 2 composite fuels with significantly-improved corrosion resistance as a potential candidate for accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Constructing high-performance radiation-resistant ternary YSZ-MgO-CNT nanocomposites via tailored nanostructures

Developing long-lifetime bulk-form ceramic-based materials with high irradiation resistance is crucial for advanced nuclear systems. Here, we incorporated carbon nanotubes (CNTs) into yttria-stabilized zirconia (YSZ) and magnesia (MgO) nanocrystals to fabricate bulk YSZ-MgO-CNT nanocomposites with abundant ternary nanostructures by spark plasma sintering. To understand the role of tailored ternary nanostructure on irradiation, we investigated the microstructure and mechanical properties evolutions of the YSZ-MgO-CNT nanocomposites irradiated by multi-energy He + ions at high temperature to different fluences. Compared with the single-phase YSZ and ultrafine-grained YSZ-MgO composites, the YSZ-MgO-CNT nanocomposites possessed higher ability to manage irradiation-induced He bubbles/defects via the defect-interface interactions of proposed “loading-unloading” and “loading-transporting-unloading” mechanisms for controlling the dynamical behaviors of He atoms/defects in the CNT-doped ternary nanostructures, thereby presenting more stable microstructure and better performance in resisting irradiation hardening. In conclusion, this work provides insight into the design of advanced inert matrix nuclear fuel and new nuclear waste management materials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

High density UO 2 and high thermal conductivity UO 2 composites by spark plasma sintering (SPS)

Embodiments of the invention are directed to a method for production of a nuclear fuel pellet by spark plasma sintering (SPS), wherein a fuel pellet with more than 80% TD or more than 90% TD is formed. The SPS can be performed with the imposition of a controlled uniaxial pressure applied at the maximum temperature of the processing to achieve a very high density, in excess of 95% TD, at temperatures of 850 to 1600° C. The formation of a fuel pellet can be carried out in one hour or less. In an embodiment of the invention, a nuclear fuel pellet comprises UO 2 and a highly thermally conductive material, such as SiC or diamond.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

High density UO2 and high thermal conductivity UO2 composites by spark plasma sintering (SPS)

Embodiments of the invention are directed to a method for production of a nuclear fuel pellet by spark plasma sintering (SPS), wherein a fuel pellet with more than 80% TD or more than 90% TD is formed. The SPS can be performed with the imposition of a controlled uniaxial pressure applied at the maximum temperature of the processing to achieve a very high density, in excess of 95% TD, at temperatures of 850 to 1600° C. The formation of a fuel pellet can be carried out in one hour or less. In an embodiment of the invention, a nuclear fuel pellet comprises UO 2 and a highly thermally conductive material, such as SiC or diamond.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Ultra-high temperature carbide foams and methods of fabricating the same

Ultra-high temperature carbide (UHTC) foams and methods of fabricating and using the same are provided. The UHTC foams are produced in a three-step process, including UHTC slurry preparation, freeze-drying, and spark plasma sintering (SPS). The fabrication methods allow for the production of any kind of single- or multi-component UHTC foam, while also providing flexibility in the shape and size of the UHTC foams to produce near-net-shape components.

Agarwal, Arvind↗
DOE OSTI2023

Ultra-high temperature carbide foams and methods of fabricating the same

Ultra-high temperature carbide (UHTC) foams and methods of fabricating and using the same are provided. The UHTC foams are produced in a three-step process, including UHTC slurry preparation, freeze-drying, and spark plasma sintering (SPS). The fabrication methods allow for the production of any kind of single- or multi-component UHTC foam, while also providing flexibility in the shape and size of the UHTC foams to produce near-net-shape components.

Agarwal, Arvind↗