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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 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Rapid synthesis of barium titanate microcubes using composite-hydroxides-mediated avenue

Highlights: • Barium titanate oxides microcubes can be synthesized within 1 min. • Composite-hydroxides-mediated strategy provided a possible large scale production. • BST obtained in the strategy showed fairly good crystallinity and tetragonality. - Abstract: This paper reports the rapid synthesis of barium titanate (BaTiO{sub 3}, BTO) microcubes via composite-hydroxides-mediated reaction within 1 min. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectrum (EDS) results confirmed both cubic and tetragonal lattices in the sample and the uniform microcubes with an average size of 1 μm. Ultraviolet–visible (UV–vis) spectrum indicated that the band gap of the BTO powder was 3.05 eV. Ferroelectric polarization vs. electric field (P–E) tests showed that the ferroelectric domains had formed in the as-synthesized BTO microcubes and sintered ceramics. BTO ceramics sintered at 1100 °C for 3 h showed fairly good tetragonality and possessed a maximum polarization of 0.21 μC/cm{sup 2}, indicating that the sintering temperature for the BTO powders prepared via this method was relatively low. The process and equipment reported herein provided a potential method for the rapid synthesis of titanate based perovskites.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Origin of giant permittivity and high-temperature dielectric anomaly behavior in Na{sub 0.5}Y{sub 0.5}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics

Na{sub 0.5}Y{sub 0.5}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics prepared by the conventional solid-state reaction method under various sintering conditions were found to exhibit a giant dielectric constant over 10 000 around room temperature. Two electrical responses were observed in the combined modulus and impedance plots, indicating the presence of Maxwell-Wagner relaxation. The contributions of semiconducting grains and insulating grain boundaries (corresponding to high-frequency and low-frequency electrical response, respectively) played important roles in the dielectric properties of Na{sub 0.5}Y{sub 0.5}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics. The correlations between grain boundaries resistance and low frequency dielectric loss, grains resistance and the position of dielectric loss peak were addressed. Mixed-valent structures of Cu{sup 2+}/Cu{sup 3+} and Ti{sup 3+}/Ti{sup 4+} had been determined using X-ray photoelectron spectroscopy. Electron hopping between Cu{sup 2+} and Cu{sup 3+} and electron transport in Ti{sup 3+}-O-Ti{sup 4+} paths were proposed as the origin of the semiconducting nature of Na{sub 0.5}Y{sub 0.5}Cu{sub 3}Ti{sub 4}O{sub 12} ceramics. In particular, high-temperature dielectric anomaly behavior was investigated in detail. A dielectric peak exhibiting relaxor-like behavior was observed around 200 Degree-Sign C, which was linked with the formation of oxygen vacancies. Based on the electric modulus results, this behavior was explored in the light of the defect formation and explained in terms of a competition process depending on the combinational contribution to polarization between n- and p-type carriers rather than a relaxation process.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Novel refractory high-entropy metal-ceramic composites with superior mechanical properties

A new concept of refractory high-entropy metal-ceramic composites (HEMCC) has been proposed that combines the outstanding physical properties of both high-entropy alloy (HEA) and high-entropy ceramic (HEC). As the first HEMCC system, to the best of our knowledge, TiTaNbZr-(TiTaNbZr)C, has been developed by a powder metallurgy process. The HEA and HEC phases exhibit body-centered cubic (BCC) and rock-salt B1 crystal structures, respectively, and both phases have non-equimolar chemical compositions. Further, with the increase of the HEC phase in HEMCC, the hardness is enhanced while the density and fracture toughness are decreased. HEA50C sintered from 50vol% HEA and 50vol% HEC precursor powders shows a favorable combination of flexural strength (541±48MPa) and fracture toughness (6.93±0.27 MPa·m 1/2 ) at room temperature and a high compressive strength at 1300ºC (275MPa). The optimized mechanical performance of HEMCC might be attributed to the combination of the ductile HEA and strong HEC phases, smaller grain size, and crack arrest at HEC/HEA interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

In situ synchrotron pair distribution function analysis to monitor synthetic pathways under electromagnetic excitation

Electromagnetic (EM) fields, specifically microwave radiation (MWR), can significantly influence the synthesis of ceramic oxide materials and promote rapid, low-temperature growth. However, the mechanisms by which EM fields affect the phase formation process are not well understood. A major limitation to increasing this understanding has been the lack of information regarding dynamic changes in local atomic structure during MWR exposure compared to conventional hydrothermal synthesis routes. Here, we utilize in situ synchrotron X-ray pair distribution function (PDF) analysis to monitor MWR-assisted SnO 2 nanoparticle synthesis. A clear impact of the EM field is demonstrated, with MWR inducing changes in nearest neighbor distances and peaks in oxygen atomic displacement that do not occur during synthesis without MWR exposure. The observed local structural disorder serves as a precursor to rapid rutile SnO 2 nanoparticle crystallization, suggesting that EM field-assisted growth is mediated by changes to the oxygen sublattice. These findings further our understanding of the mechanisms underlying MWR-assisted synthesis and represent a step towards utilizing EM fields to engineer tailored atomic structures for a broad range of applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Python-EPICS RF Conditioning Automatic Control System at the Spallation Neutron Source

The RF Test Facility (RFTF) at the Spallation Neutron Source (SNS) is used for the conditioning of RF compo-nents such as ceramic vacuum windows and power cou-plers prior to their installation in the H- ion linear accel-erator. This process exposes components to high-power RF fields and thermal cycling to improve performance and remove surface impurities. To automate and optimize this process, a Python-based EPICS control system was developed alongside targeted hardware upgrades. The system enables real-time monitoring and control of RF power levels, temperature, and vacuum pressure. A user-friendly graphical interface was implemented using CS-Studio (Phoebus), allowing operators to adjust parameters and collect data efficiently. The system integrates a High-Power Protection Module (HPM) for interlocks based on vacuum and arc detection, ensuring safe operation. These upgrades have significantly improved the efficiency, accuracy, and safety of RF conditioning at the SNS RFTF. This paper describes the updated RF conditioning sys-tem, highlighting the software and hardware develop-ments and their application in support of the Proton Pow-er Upgrade (PPU) project.

Lee, Sung-Woo [ORNL] (ORCID:000000030915835X)↗
DOE OSTI2024

Abrasive Waterjet Machining

The abrasive waterjet machining process was introduced in the 1980s as a new cutting tool; the process has the ability to cut almost any material. Currently, the AWJ process is used in many world-class factories, producing parts for use in daily life. A description of this process and its influencing parameters are first presented in this paper, along with process models for the AWJ tool itself and also for the jet–material interaction. The AWJ material removal process occurs through the high-velocity impact of abrasive particles, whose tips micromachine the material at the microscopic scale, with no thermal or mechanical adverse effects. The macro-characteristics of the cut surface, such as its taper, trailback, and waviness, are discussed, along with methods of improving the geometrical accuracy of the cut parts using these attributes. For example, dynamic angular compensation is used to correct for the taper and undercut in shape cutting. The surface finish is controlled by the cutting speed, hydraulic, and abrasive parameters using software and process models built into the controllers of CNC machines. In addition to shape cutting, edge trimming is presented, with a focus on the carbon fiber composites used in aircraft and automotive structures, where special AWJ tools and manipulators are used. Examples of the precision cutting of microelectronic and solar cell parts are discussed to describe the special techniques that are used, such as machine vision and vacuum-assist, which have been found to be essential to the integrity and accuracy of cut parts. The use of the AWJ machining process was extended to other applications, such as drilling, boring, milling, turning, and surface modification, which are presented in this paper as actual industrial applications. To demonstrate the versatility of the AWJ machining process, the data in this paper were selected to cover a wide range of materials, such as metal, glass, composites, and ceramics, and also a wide range of thicknesses, from 1 mm to 600 mm. The trends of Industry 4.0 and 5.0, AI, and IoT are also presented.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Ceramic oxygen transport membrane array reactor and reforming method

The invention relates to a commercially viable modular ceramic oxygen transport membrane system for utilizing heat generated in reactively-driven oxygen transport membrane tubes to generate steam, heat process fluid and/or provide energy to carry out endothermic chemical reactions. The system provides for improved thermal coupling of oxygen transport membrane tubes to steam generation tubes or process heater tubes or reactor tubes for efficient and effective radiant heat transfer.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

High-Energy All-Solid-State Organic–Lithium Batteries Based on Ceramic Electrolytes

Recent studies have identified unique properties of organic battery electrode materials such as moderate redox potentials and mechanical softness which are uniquely beneficial for all-solid-state batteries based on ceramic electrolytes. Here, we further explore the promise of organic materials and demonstrate a sulfide electrolyte- based organic-lithium battery with a specific energy of 828 Wh kg –1 , rivaling the state-of- the-art of all-solid-state batteries. Two innovation steps are responsible for the accomplishment. First, the combination of lithium anode and the high-capacity cathode material pyrene-4,5,9,10-tetraone ensures a high theoretical specific energy. Second, the microstructure of the organic cathode is optimized with the introduction of cryomilling, a technique common to processing soft materials but not familiar to electrode fabrication. The cathode material utilization increases to 99.5% as a result, up from the 55–89% previously reported for ceramic electrolyte-based solid-state organic batteries. In conclusion, the improvement highlights the special requirements of solid-state organic electrodes for microstructural engineering while preserving the chemical integrity of components.

25 ENERGY STORAGE↗
DOE OSTI2017

Thermodynamic and Microstructural Mechanisms in the Corrosion of Advanced Ceramic Tc-bearing Waste Forms and Thermophysical Properties

Technetium-99 (Tc, t 1/2 = 2.13x10 5 years) is a challenge from a nuclear waste perspective and is one of the most abundant, long-lived radioisotopes found in used nuclear fuel (UNF). Within the Hanford Tank Waste Treatment and Immobilization Plant, technetium volatilizes at typical glass melting temperature, is captured in the off-gas treatment system and recycled back into the feed to eventually increase Tc-loadings of the glass. The aim of this NEUP project was to provide an alternative strategy to immobilize fission technetium as durable ceramic waste form and also to avoid the accumulation of volatile technetium within the off gas melter system in the course of vitrifying radioactive effluents in a ceramic melter. During this project our major attention was turned to the fabrication of chemical durable mineral phases where technetium is structurally bond entirely as tetravalent cation. These mineral phases will act as the primary waste form with optimal waste loading and superior resistance against leaching and corrosion. We have been very successful in fabricating phase-pure micro-gram amounts of lanthanide-technetium pyrochlores by dry-chemical synthesis. However, upscaling to a gram-size synthesis route using either dry- or wet-chemical processing was not always successful, but progress can be reported on a variety of aspects. During the course of this 5-year NEUP project (including a 2-year no-cost extension) we have significantly enhanced the existing knowledge on the fabrication and properties of ceramic technetium waste forms.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Relationship between ferroelectric properties and local structure of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} ceramic materials studied by X-ray absorption and Raman spectroscopies

This paper reports on the structural characterization of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} (PBZT) ferroelectric ceramic compositions prepared by the conventional solid state reaction method. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used in the probing of the local structure of PBZT samples that exhibit a normal or relaxor ferroelectric behavior. They showed a considerable local disorder around Zr and Pb atoms in the samples of tetragonal or cubic long-range order symmetry. The intensity of the E(TO{sub 3}) mode in the Raman spectra of PBZT relaxor samples remains constant at temperatures lower than T{sub m}, which has proven the stabilization of the correlation process between nanodomains. - Graphical abstract: X-ray absorption measurements showed considerable local disorder around Zr and Pb atoms in the samples of tetragonal or cubic long-range order symmetry. The intensity of the E(TO{sub 3}) mode in the Raman spectra of PBZT relaxor samples remains constant at temperatures lower than T{sub m}, which has proven the stabilization of the correlation process between nanodomains. Display Omitted - Highlights: • Structural characterization of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} (PBZT) ferroelectric ceramic. • X-ray absorption and Raman spectroscopies were used to probe the structure of PBZT. • Dissymmetry of Zr and Pb sites was observed in samples long-range cubic symmetry. • Local disorder in all PBZT samples through the observation of Raman active modes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Dielectric silicone elastomers with mixed ceramic nanoparticles

Highlights: • Composite ceramics nanoparticles (MCN) with zirconium dioxide and lead zirconate. • Dielectric elastomer films wDith PDMS matrix and MCN as dielectric filler. • Hydrophobic character—water resistant and good flexibility specific to siloxanes. • Increased value of dielectric constant with the content of MCN in dielectric films. • Increased energy output from uniaxial deformation of the dielectric elastomer films. - Abstract: A ceramic material consisting in a zirconium dioxide-lead zirconate mixture has been obtained by precipitation method, its composition being proved by wide angle X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The average diameter of the ceramic particles ranged between 50 and 100 nm, as revealed by transmission electron microscopy images. These were surface treated and used as filler for a high molecular mass polydimethylsiloxane-α,ω-diol (Mn = 450,000) prepared in laboratory, the resulted composites being further processed as films and crosslinked. A condensation procedure, unusual for polydimethylsiloxane having such high molecular mass, with a trifunctional silane was approached for the crosslinking. The effect of filler content on electrical and mechanical properties of the resulted materials was studied and it was found that the dielectric permittivity of nanocomposites increased in line with the concentration of ceramic nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Fracture toughness measurement of ceramics with fuel pellet geometry

The crack initiation of nuclear fuel pellets, driven by extreme temperature gradients, is a critical factor impacting reactor performance. Although this fact is widely acknowledged, there is limited fracture toughness data for specimens with representative geometry and fabricated using relevant processing methods. Here, to address this, a new chevron-notched short-rod specimen configuration with diameter and length both equal to 10 mm, representative of a conventional fuel pellet and tested in tension, was developed in an attempt to validly measure Mode I fracture toughness, K Ic . Test calibration was carried out by testing polycrystalline ZrO 2 , SiC, and Si 3 N 4 ceramics fabricated with conventional fuel pellet geometry and known fracture toughnesses. The results suggest that the method described in this paper produces valid K Ic measurements using conventional ceramic fuel pellets.

Ceramics↗
DOE OSTI2016

The influence of A-site strontium ion in controlling the microstructure and electrical properties of P{sub 1−x}S{sub x}ZNZT ceramics

A Pb{sub 1−x}Sr{sub x}(Zn{sub 1/3}Nb{sub 2/3}){sub 0.2}(Zr{sub 0.5}Ti{sub 0.5}){sub 0.8}O{sub 3} (P{sub 1−x}S{sub x}ZNZT, 0.00 ≤ x ≤ 0.10) system was prepared through a conventional solid oxide process. Increasing addition of Sr{sup 2+} was found to induce a continuous decrease in grain size from 2.46 μm to 1.14 μm, accompanied by a phase transformation from coexisting rhombohedral and tetragonal phases to tetragonal phase only. The underlying mechanism of the evolution of dielectric and ferroelectric behavior in the P{sub 1−x}S{sub x}ZNZT ferroelectric ceramics was ascribed to the synergy between the grain size effect and the dilution of Pb-O covalency. Additionally, the grain size effect on domain wall displacement was found to be the main origin of the superior permittivity and piezoelectricity of the ceramics at intermediate grain size. The optimal electrical properties achieved for the P{sub 0.95}S{sub 0.05}ZNZT specimen at a grain size of about 1.79 μm, d{sub 33} = 465 pC/N, d{sub 33} × g{sub 33} = 11 047 × 10{sup −15} m{sup 2}/N make this material promising for multilayer energy harvesting device applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Poster - 01: LabPET II Pixelated APD-Based PET Scanner for High-Resolution Preclinical Imaging

Purpose: LabPET II is a new generation APD-based PET scanner designed to achieve sub-mm spatial resolution using truly pixelated detectors and highly integrated parallel front-end processing electronics. Methods: The basic element uses a 4×8 array of 1.12×1.12 mm{sup 2} Lu{sub 1.9}Y{sub 0.1}SiO{sub 5}:Ce (LYSO) scintillator pixels with one-to-one coupling to a 4×8 pixelated monolithic APD array mounted on a ceramic carrier. Four detector arrays are mounted on a daughter board carrying two flip-chip, 64-channel, mixed-signal, application-specific integrated circuits (ASIC) on the backside interfacing to two detector arrays each. Fully parallel signal processing was implemented in silico by encoding time and energy information using a dual-threshold Time-over-Threshold (ToT) scheme. The self-contained 128-channel detector module was designed as a generic component for ultra-high resolution PET imaging of small to medium-size animals. Results: Energy and timing performance were optimized by carefully setting ToT thresholds to minimize the noise/slope ratio. ToT spectra clearly show resolved 511 keV photopeak and Compton edge with ToT resolution well below 10%. After correction for nonlinear ToT response, energy resolution is typically 24±2% FWHM. Coincidence time resolution between opposing 128-channel modules is below 4 ns FWHM. Initial imaging results demonstrate that 0.8 mm hot spots of a Derenzo phantom can be resolved. Conclusion: A new generation PET scanner featuring truly pixelated detectors was developed and shown to achieve a spatial resolution approaching the physical limit of PET. Future plans are to integrate a small-bore dedicated mouse version of the scanner within a PET/CT platform.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

A Self-Healing, Flowable, Yet Solid Electrolyte Suppresses Li-Metal Morphological Instabilities

In this article, lithium metal (Li 0 ) solid-state batteries encounter implementation challenges due to dendrite formation, side reactions, and movement of the electrode–electrolyte interface in cycling. Notably, voids and cracks formed during battery fabrication/operation are hot spots for failure. Here, a self-healing, flowable yet solid electrolyte composed of mobile ceramic crystals embedded in a reconfigurable polymer network is reported. This electrolyte can auto-repair voids and cracks through a two-step self-healing process that occurs at a fast rate of 5.6 µm h -1 . A dynamical phase diagram is generated, showing the material can switch between liquid and solid forms in response to external strain rates. The flowability of the electrolyte allows it to accommodate the electrode volume change during Li 0 stripping. Simultaneously, the electrolyte maintains a solid form with high tensile strength (0.28 MPa), facilitating the regulation of mossy Li 0 deposition. The chemistries and kinetics are studied by operando synchrotron X-ray and in situ transmission electron microscopy (TEM). Solid-state NMR reveals a dual-phase ion conduction pathway and rapid Li + diffusion through the stable polymer-ceramic interphase. This designed electrolyte exhibits extended cycling life in Li 0 –Li 0 cells, reaching 12 000 h at 0.2 mA cm -2 and 5000 h at 0.5 mA cm -2 . Furthermore, owing to its high critical current density of 9 mA cm -2 , the Li 0 –LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) full cell demonstrates stable cycling at 5 mA cm -2 for 1100 cycles, retaining 88% of its capacity, even under near-zero stack pressure conditions.

25 ENERGY STORAGE↗
DOE OSTI2020

The effect of submicron grain size on thermal stability and mechanical properties of high-entropy carbide ceramics

(Hf 0.2 Zr 0.2 Ta 0.2 Nb 0.2 Ti 0.2 )C high-entropy ceramics (HEC) with a submicron grain size of 400 to 600 nm were fabricated by spark plasma sintering using a two-step sintering process. Both X-ray and neutron diffractions confirmed the formation of single-phase with rock salt structure in the as-fabricated (Hf 0.2 Zr 0.2 Ta 0.2 Nb 0.2 Ti 0.2 )C samples. The effect of submicron grain size on the thermal stability and mechanical properties of HEC was investigated. The grain growth kinetics in the fine-grained HEC was small at 1300 and 1600°C, suggesting high thermal stability that was possibly related to the compositional complexity and sluggish diffusion in HEC. Compared to the coarse-grain HEC with a grain size of 16.5 µm, the bending strength and fracture toughness of fine-grained HEC were 25% and 20% higher respectively. The improvement of mechanical properties in fine-grained HEC may be attributed to micromechanistic mechanisms such as crack deflection.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Synthesis and Flash Sintering of (Hf1-xZrx)B2 Solid Solution Fine Powders

Fine powders of (Hf1-xZrx)B2 solid solution were synthesized by two methods. In the first one, solution-based processing of HfCl4, ZrCl4, sucrose and H3BO3 was carried out followed by heat treatment (e.g., at 1500 °C for 1 h) in Argon to achieve the carbothermal reduction (CTR) reaction to form the boride solid solution. In the second one, called boron hydride reduction (BHR) method, HfCl4, ZrCl4 and NaBH4 were directly mixed in a glove box followed by heat treatment in Argon at elevated temperatures from 700 to 1500 °C. In addition, the powders synthesized via both methods were flash sintered without sample preheating in a homemade setup. The synthesized powders as well as the flash sintered bulk ceramics were characterized using different techniques including XRD, SEM, EDS, TEM, TGA-DSC, and Vickers hardness test to reveal the inter-relationships between starting materials composition, processing conditions, and the resulting materials microstructure and physical/chemical properties.

Belisario, Jose↗
DOE OSTI2018

Coalescence growth mechanism of inserted tin dioxide belts in polycrystalline SnO2-based ceramics

Highlights: • Grain growth in SnO{sub 2}-based varistors was studied. • The growth of 1D SnO{sub 2} belts in the SnO{sub 2}-CoO-Cr{sub 2}O{sub 3}-Nb{sub 2}O{sub 5} system occurs by coalescence process. • Cross-Section and Tomography images showed tridimensional and pore free “giant grains”. • TEM was used to prove the alignment of the grains towards the SnO{sub 2} belt. • The coalescence growth just occurs with 1D structure and grains having the same crystal structure. - Abstract: SnO{sub 2}-based varistors have been considered promising technological devices. However their practical application is usually stated as limited to high voltage circuits based on the high breakdown electric field exhibited by these ceramics. Recently, authors have shown that the insertion of one-dimensional (1D) SnO{sub 2} belts allows overcoming this limitation. In this work, we present a detailed study of the growth mechanism of the belts inside varistors using electron microscopy techniques. We were able to show that mass transport has an intrinsic dependence on the sintering time and requires similar crystalline structure between the belts and the matrix. Dual beam and high-resolution transmission electron microscopy techniques permitted determining that 3D growth of belts occurs by coalescence.

36 MATERIALS SCIENCE↗