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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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Role of Surface Hydroxyls and Lattice Oxygen in Governing Selectivity and Restructuring During Acetic Acid Conversion on Fe 3 O 4 (001)

Understanding the reactivity of carboxylic acids on metal oxide surfaces is critical for elucidating ketonization mechanisms relevant to biomass upgrading. Here, we investigate the adsorption and thermal decomposition of acetic acid (CH 3 COOH) on Fe 3 O 4 (001) using scanning tunneling microscopy (STM), temperature-programmed reaction spectroscopy (TPRS), and X-ray photoelectron spectroscopy (XPS). At room temperature, acetic acid adsorbs dissociatively to form ordered bidentate acetate (CH 3 COO) overlayer that lifts the (√2 × √2)R 45° surface reconstruction. TPRS reveals ketene (CH 2 CO) as the dominant product, along with CO, CO 2 , and H 2 O, the latter evolving via a Mars–van Krevelen (MvK) mechanism. Isotopic labeling shows preferential CO 2 formation from the carboxyl carbon and a more balanced CO/CO 2 ratio from the methyl carbon, suggesting distinct oxidation pathways. STM imaging reveals embedded acetate intermediates filling surface oxygen vacancies created in MvK steps. Upon product formation completion (~700 K), extensive surface etching is observed, with pits elongated along the octahedral Fe rows. Approximately 20% of the surface oxygen is removed, consistent with vacancy formation stoichiometry inferred from product distributions. These findings demonstrate that carboxylate-induced restructuring of Fe 3 O 4 (001) involves both surface healing and reduction processes, offering mechanistic insights relevant to ketonization and broader carboxylic acid chemistry on metal oxides.

acetic acid↗
DOE OSTI2020

Nanometer-Scale Imaging of Inhomogeneous Active Charge Carriers in Arsenic-Doped CdTe Thin Films

We report nanometer-scale imaging of active carrier distribution of As-doped CdTe films by scanning capacitance microscopy (SCM). We developed SCM sample preparation for CdTe by ion-milling followed by thermal processing. The nanometer-resolution carrier delineation for CdTe was validated by imaging on a CdTe cross-section sample made by a molecular beam epitaxy layer stack with As-doping concentrations of 10^15 ~10^18 /cm 3 . We found that the carrier distribution in As-doped films was significantly nonuniform, with inhomogeneity ranging from sub-um to a few um and concentration variation of one order of magnitude (low 10^16 to low 10^17 /cm 3 ). This nonuniformity is distributed randomly, independent of grain structure and grain boundary (GB). We used Kelvin probe force microscopy (KPFM) and cathodoluminescence (CL) to further map the surface potential and radiative illumination on the same area as the SCM image. Higher potential and lower CL intensity were found on GBs but not on SCM contrast, illustrating positive GB charging and GB recombination but not GB-distinguished doping. The overall KPFM potential image is in rough agreement with the SCM carrier distribution, in terms of Fermi-level position relative to the bandgap edge - thus resulting in the band-edge potential fluctuation. Nonuniform carrier concentration, potential fluctuation, and defect recombination can all together cause the Voc deficit of the As-doped CdTe device.

14 SOLAR ENERGY↗
NASA NTRS2001

Controlling Growth Orientation of Phthalocyanine Films by Electrical Fields

Organic Phthalocyanine films have many applications ranging from data storage to various non-linear optical devices whose quality is affected by the growth orientation of Phthalocyanine films. Due to the structural and electrical properties of Phthalocyanine molecules, the film growth orientation depends strongly on the substrate surface states. In this presentation, an electrical field up to 4000 V/cm is introduced during film growth. The Phthalocyanine films are synthesized on quartz substrates using thermal evaporation. An intermediate layer is deposited on some substrates for introducing the electrical field. Scanning electron microscopy, x-ray diffraction, and Fourier transform infrared spectroscopy are used for measuring surface morphology, film structure, and optical properties, respectively. The comparison of Phthalocyanine films grown with and without the electrical field reveals different morphology, film density, and growth orientation, which eventually change optical properties of these films. These results suggest that the growth method in the electrical field can be used to synthesized Phthalocyanine films with a preferred crystal orientation as well as propose an interaction mechanism between the substrate surface and the depositing molecules. The details of growth conditions and of the growth model of how the Phthalocyanine molecules grow in the electrical field will be discussed.

Zhu, S.↗
DOE OSTI2026

A Comparative Study of Thermal Oxidization Resistance of a High-Entropy Metal Boride and a High-Entropy Metal Carbide

We present a systematic study of thermal oxidation resistance of transition metal borides and carbides up to 1300 °C in a dry air environment. A High-Entropy Metal Boride (HEMB), of composition (Hf 0.2 , Mo 0.2 , Nb 0.2 , Ta 0.2 , Zr 0.2 )B 2 , and a similar High-Entropy Metal Carbide (HEMC) (Hf, Mo, Nb, Ta, Zr)C 5 were synthesized from precursor mixtures, under 30 MPa of pressure at a temperature of 1800 °C using a Spark Plasma Sintering Device. The synthesized phases were confirmed via X-ray Diffraction analysis, which showed a pure hexagonal AlB 2 -type structure for HEMB and a face-centered cubic (FCC) structure for HEMC, with lattice parameters, a = 3.10 Å and c = 3.37 Å for HEMB and a = 4.524 Å for HEMC. Oxidation resistance was evaluated using a simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA/DSC) stage in which HEMB and HEMC were heated up to 1300 °C at a rate of 2 °C/min in a dry air environment. Scanning electron microscopy (SEM) was used to analyze the resulting oxidized material. Our study demonstrates that HEMB shows better thermal oxidation resistance as compared to a similar metal composition HEMC at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Scanning ultrafast electron microscopy reveals photovoltage dynamics at a deeply buried $p^- \mathrm{Si/SiO_2}$ interface

The understanding and control of charge carrier interactions with defects at buried insulator/semiconductor interfaces is essential for achieving optimum performance in modern electronics. In this work, we report on the use of scanning ultrafast electron microscopy (SUEM) to remotely probe the dynamics of excited carriers at a Si surface buried below a thick thermal oxide. Our measurements illustrate a previously unidentified SUEM contrast mechanism, whereby optical modulation of the space-charge field in the semiconductor modulates the electric field in the thick oxide, thus affecting its secondary electron yield. By analyzing the SUEM contrast as a function of time and laser fluence we demonstrate the diffusion mediated capture of excited carriers by interfacial traps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Thermal cycling-driven microstructural changes of eutectic Al–Si phase change materials in SS304 containers revealed by multi-modal imaging

Aluminum-based Al–Si alloys are widely used as phase change materials (PCMs) in thermal energy storage (TES) systems owing to their high volumetric latent heat and superior thermal conductivity. However, their long-term reliability is limited by degradation processes that remain insufficiently understood. In this work, we employ a multimodal, correlative characterization framework to systematically resolve the degradation behavior of eutectic Al–Si PCMs in contact with SS304 containers under repeated thermal cycling. By integrating high-resolution electron microscopy, three-dimensional X-ray fluorescence (3D XRF) imaging, and differential scanning calorimetry (DSC), we directly link spatially resolved compositional and microstructural evolution to changes in thermophysical properties. The correlative analysis reveals that elemental leaching of Fe, Cr, and Ni from the stainless-steel container into the PCM drives the formation of intermetallic compounds (IMCs) both at the interface and within the bulk PCM, leading to pronounced compositional heterogeneity. These interfacial reactions and diffusion-induced transformations progressively destabilize the Al–Si eutectic, reducing the effective phase-transforming fraction. Consistent with these observations, DSC measurements show a decrease in melting temperature and latent heat of fusion with thermal cycling. These results underscore the critical influence of interfacial reactions and material compatibility on the stability, durability, and overall performance of Al–Si-based TES systems.

25 ENERGY STORAGE↗
DOE OSTI2020

U 3 Si 2 and UO 2 composites densified by spark plasma sintering for accident-tolerant fuels

This work reports the synthesis and characterization of the U 3 Si 2 and UO 2 composites sintered by spark plasma sintering (SPS) with controlled microstructures for accident-tolerant fuel application. The U 3 Si 2 and UO 2 composites with different silicide and oxide ratios were synthesized by SPS at temperatures from 1000 to 1300 °C for 5 minutes. The microstructure and phase composition of the SPS densified composite fuels were characterized with scanning electron microscopy, X-ray diffraction (XRD), and energy dispersed spectroscopy (EDS). A systematic study of the thermal and mechanical properties was conducted using microhardness testing and laser flash apparatus, along with oxidation resistance measurements using thermogravimetric analysis (TGA). The results show that the synthesis of composite fuels can be achieved with a 90% theoretical density (TD) at 1000 °C and over 95% TD when sintered at 1300 °C. XRD and EDS results confirmed that the dominant phases in the composites are U 3 Si 2 and UO 2 . Improved physical density generally leads to improved hardness, fracture toughness, thermal diffusivity, and onset temperature during the oxidation process. U 3 Si 2 was found to play a dominant role in determining the mechanical and oxidation properties of the composite fuels, whereas UO 2 had a more important impact on controlling the thermal diffusivity of the composites. The composite with 50 wt% UO 2 sintered at 1300 °C displayed the onset oxidation temperature of 500 °C by dynamic oxidation testing using TGA at a ramp degree of 10 °C/min. The composite also achieved a high fracture toughness of ~3.5 MPa m ½ . Finally, these results highlight the potential of composite fuel forms densified by SPS with simultaneously enhanced fissile element density, fracture toughness, thermal transport properties, and oxidation resistance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1988

Synthesis and characterization of high-T(sub c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, x-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c)(onset) approx 96 K, T(sub c)(zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗
NASA NTRS1988

Synthesis and characterization of high-T(c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, X-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c) (onset) approx 96 KK, T(sub c) (zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗
NASA NTRS1992

Results of examination of silvered Teflon from the Long Duration Exposure Facility

A significant effort to determine the effects of low earth orbit (LEO) exposure on silver backed fluorinated ethylene-propylene (FEP) blankets from the Long Duration Exposure Facility (LDEF) was performed, and the results of this investigation are described. Extensive measurements of surface, optical, chemical, and mechanical properties were conducted. Effects of contamination and erosion rates of the FEP layer were determined. Specific results are reported on solar absorptance, thermal emittance, diffuse reflectance, cross sectional microphotography, secondary ion mass spectroscopy, electron scattering for chemical analysis, scanning electron microscopy, percent elongation, and tensile strength. These measurements show the effects of two distinctly different exposure environments, solar exposure, and simultaneous atomic oxygen (AO) and solar exposure.

Rousslang, Ken↗
NASA NTRS1993

Microstructural analysis of the 2195 aluminum-lithium alloy welds

The principal objective of this research was to explain a tendency of 2195 Al-Li alloy to crack at elevated temperature during welding. Therefore, a study was made on the effect of welding and thermal treatment on the microstructure of Al-Li Alloy 2195. The critical roles of precipitates, boundaries, phases, and other features of the microstructure were inferred from the crack propagation paths and the morphology of fracture surface of the alloy with different microstructures. Particular emphasis was placed on the microstructures generated by the welding process and the mechanisms of crack propagation in such structures. Variation of the welding parameters and thermal treatments were used to alter the micro/macro structures, and they were characterized by optical and scanning electron microscopy. A theoretical model is proposed to explain changes in the microstructure of welded material. This model proposes a chemical reaction in which gases from the air (i.e., nitrogen) release hydrogen inside the alloy. Such a reaction could generate large internal stresses capable to induce porosity and crack-like delamination in the material.

Talia, George E.↗
DOE OSTI2024

Characterization of Two Fast-Turnaround Dry Dilution Refrigerators for Scanning Probe Microscopy

Low-temperature scanning probe microscopes (SPMs) are critical for the study of quantum materials and quantum information science. Due to the rising costs of helium, cryogen-free cryostats have become increasingly desirable. However, they typically suffer from comparatively worse vibrations than cryogen-based systems, necessitating the understanding and mitigation of vibrations for SPM applications. Here, in this work, we demonstrate the construction of two cryogen-free dilution refrigerator SPMs with minimal modifications to the factory default and we systematically characterize their vibrational performance. We measure the absolute vibrations at the microscope stage with geophones and use both microwave impedance microscopy and a scanning single-electron transistor to independently measure tip-sample vibrations. Additionally, we implement customized filtering and thermal anchoring schemes and characterize the cooling power at the scanning stage and the tip electron temperature. This work serves as a reference to researchers interested in cryogen-free SPMs, as such characterization is not standardized in the literature or available from manufacturers.

36 MATERIALS SCIENCE↗
NASA NTRS1994

(abstract) Optical Scattering and Surface Microroughness of Ion Beam Deposited Au and Pt Thin Films

Thin films of gold and platinum have been deposited onto superpolished fused silica substrates using thermal evaporation, ion assisted deposition (IAD), and ion assisted sputtering. The influence of ion beam flux, thin film material, and deposition rate on the films microroughness have been investigated. Short range surface microroughness of the films has been examined using scanning tunneling microscopy (STM) and atomic force microscopy (AFM). Long range surface microroughness has been characterized using an angle resolved optical scatterometer. Results indicate that ion beam deposited coatings have improved microstructure over thermally evaporated films.

assisted sputtering fused silica ion beam microrou↗
DOE OSTI2023

Direct Visualization of Localized Vibrations at Complex Grain Boundaries

Abstract Grain boundaries (GBs) are a prolific microstructural feature that dominates the functionality of a wide class of materials. The functionality at a GB results from the unique atomic arrangements, different from those in the grain, that have driven extensive experimental and theoretical studies correlating atomic‐scale GB structures to macroscopic electronic, infrared optical, and thermal properties. In this work, a SrTiO 3 GB is examined using atomic‐resolution aberration‐corrected scanning transmission electron microscopy and ultrahigh‐energy‐resolution monochromated electron energy‐loss spectroscopy, in conjunction with density functional theory. This combination enables the correlation of the GB structure, nonstoichiometry, and chemical bonding with a redistribution of vibrational states within the GB dislocation cores. The new experimental access to localized GB vibrations provides a direct route to quantifying the impact of individual boundaries on macroscopic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Recycled polyethylene and crumb rubber composites modified asphalt with improved aging resistance and thermal stability

Crumb rubbers (CR) and recycled Polyethylene (PE) are commonly used as modifiers to improve the asphalt properties. However, the addition of these modifiers individually may result in phase separation of PE and inadequate degradation of CR, which may not simultaneously satisfy the rheological and aging resistance of the binder blends. In this study, a type of CR/PE composites manufactured through melt extrusion procedures was adopted for the improvement of the modified binder blends. The modified binder blends after short-term (RTFO) and long-term (PAV) aging were collected for dynamic shear rheometer and bending beam rheometer tests. FTIR tests were also used to quantify the aging resistance, while differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were applied to evaluate the thermal behaviors of the binder blends. Optical microscopy tests were used to explore the modification mechanism and visualize the microstructures of original and PAV aged binder blends. Test results showed that CR/PE composites could significantly improve the aging resistance of the binder blends. The dispersed PE particles still interacted with each other and meanwhile worked with the diffused rubbery phase, which could form a similar TPEs network. The oxidation and high-temperature aging of such binder blends would strengthen the network that resisted the aging severity of the binder blends. Furthermore, it was also revealed that CR/PE modified asphalt could sustain more heat before a rapid degradation and the well-dispersed PE particles could interact with the diffused CR particles to form a network to resist aging.

02 PETROLEUM↗
DOE OSTI2025

In situ high-temperature Raman spectroscopy for online EAF slag analysis

Real-time monitoring of slag chemistry is critical for optimizing Electric Arc Furnace (EAF) steelmaking operations, where dynamic variations in slag composition directly influence slag foaming, refractory degradation, and thermal efficiency. Conventional techniques such as X-ray fluorescence (XRF), Fourier-transform infrared (FTIR), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) are commonly used to analyze slag composition, but their offline nature and equipment constraints limit their applicability for online monitoring in harsh industrial environments. To address this challenge, we present an in situ, high-temperature analytical approach that integrates Raman spectroscopy with a custom designed fiber-optic probe for real-time slag characterization at 1550 °C. The system enables non destructive spectral acquisition from molten slags, providing molecular-level insights into silicate polymerization and iron oxidation states. Eight synthetic slag samples were evaluated, and key Raman features—such as Q n silicate units and FeO₄/FeO₆ coordination environments—were identified and quantitatively correlated with slag basicity and Fe₂O₃ content. The results demonstrate agreement between Raman spectral ratios and bulk slag chemistry, validating the method’s capability to track compositional and structural changes under molten temperature. This work establishes the feasibility of deploying fiber-optic Raman probe for online EAF slag monitoring and highlights their potential to support closed-loop control strategies, thereby enhancing process stability, refractory protection, and steel quality in industrial steelmaking applications.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Possible impacts of Mo chemical banding and second phase impurities on the irradiation behavior of monolithic U-10Mo fuels

This study investigated the microstructural behavior of both full-size and mini-size monolithic U-10Mo fuel plates irradiated to high burnup with a focus on the evolution of the second phase impurities in monolithic U-Mo using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and wavelength dispersive spectroscopy (WDS). Key indicators of possible mechanical and thermal compromise include cracks, large fission gas porosity, and interconnection of fission gas pores. For the fission densities evaluated in this work (3.5 × 10 21 fissions/cm 3 -5.1 × 10 21 fissions/cm 3 ), fine porosity can develop along the UC phase boundary; however, the size of the fission gas pores is no more than those observed in the U-Mo fuel phase. Further, other inclusions such as Si-rich second-phase impurities found in the as-fabricated microstructure were difficult to resolve post-irradiation because they can become overshadowed by porosity development in the fuel phase. Additionally, the presence of a Fe-rich sublayer formed in the Zr diffusion layer during fabrication remained enriched in the Zr layer in the irradiated U-10Mo microstructures near the U-Mo/Zr interface; however, based on the burnup assessed in this study the identified impurities did not appear to contribute to notable microstructural degradation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

3D Printing of Polyelectrolyte Complex-Integrated Photocurable Hydrogel Resins

In this study, we developed a photocurable hydrogel resin incorporating a polyelectrolyte complex (PEC) for 3D printing. Acrylamide-based monomers were formulated with varying PEC contents (0–15 wt %) in an aqueous KBr medium to fabricate patterned porous hydrogel structures. The morphology of printed hydrogels was characterized by field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. Notably, the PEC5 and PEC10 formulations exhibited optimal thermal stability and compressive properties, attributed to the homogeneous distribution of PEC domains within the hydrogel matrix. Furthermore, dye adsorption experiments demonstrated excellent removal efficiency, highlighting the potential of PEC-containing hydrogels for environmental remediation applications, particularly in the treatment of dye-contaminated wastewater.

Yang, Jinchul [University of Tennesse Knoxville]↗