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At least 1,315 records · Page 73
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

From Pollutant Removal to Renewable Energy: MoS2-Enhanced P25-Graphene Photocatalysts for Malathion Degradation and H2 Evolution

The widespread presence of pesticides—especially malathion—in aquatic environments presents a major obstacle to conventional remediation strategies, while the ongoing global energy crisis underscores the urgency of developing renewable energy sources such as hydrogen. In this context, photocatalytic water splitting emerges as a promising approach, though its practical application remains limited by poor charge carrier dynamics and insufficient visible-light utilization. Herein, we report the design and evaluation of a series of TiO2-based ternary nanocomposites comprising commercial P25 TiO2, reduced graphene oxide (rGO), and molybdenum disulfide (MoS2), with MoS2 loadings ranging from 1% to 10% by weight. The photocatalysts were fabricated via a two-step method: hydrothermal integration of rGO into P25 followed by solution-phase self-assembly of exfoliated MoS2 nanosheets. The composites were systematically characterized using X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and photoluminescence (PL) spectroscopy. Photocatalytic activity was assessed through two key applications: the degradation of malathion (20 mg/L) under simulated solar irradiation and hydrogen evolution from water in the presence of sacrificial agents. Quantification was performed using UV-Vis spectroscopy, gas chromatography–mass spectrometry (GC-MS), and thermal conductivity detection (GC-TCD). Results showed that the integration of rGO significantly enhanced surface area and charge mobility, while MoS2 served as an effective co-catalyst, promoting interfacial charge separation and acting as an active site for hydrogen evolution. Nearly complete malathion degradation (~100%) was achieved within two hours, and hydrogen production reached up to 6000 µmol g−1 h−1 under optimal MoS2 loading. Notably, photocatalytic performance declined with higher MoS2 content due to recombination effects. Overall, this work demonstrates the synergistic enhancement provided by rGO and MoS2 in a stable P25-based system and underscores the viability of such ternary nanocomposites for addressing both environmental remediation and sustainable energy conversion challenges.

Chemistry↗
DOE OSTI2022

Variable Temperature Behaviour of the Hybrid Double Perovskite MA 2 KBiCl 6

Perovskite-related materials show very promising properties in many fields. Pb-free perovskites are particularly interesting, because of the toxicity of Pb. In this study, hybrid double perovskite MA 2 KBiCl 6 (MA = methylammonium cation) was found to have interesting variable temperature behaviours. Both variable temperature single crystal X-ray diffraction, synchrotron powder diffraction, and Raman spectroscopy were conducted to reveal a rhombohedral to cubic phase transition at around 330 K and an order to disorder transition for inorganic cage below 210 K.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Partial Least Squares, Experimental Design, and Near-Infrared Spectrophotometry for the Remote Quantification of Nitric Acid Concentration and Temperature

Near-infrared spectrophotometry and partial least squares regression (PLSR) were evaluated to create a pleasantly simple yet effective approach for measuring HNO3 concentration with varying temperature levels. A training set, which covered HNO3 concentrations (0.1–8 M) and temperature (10–40 °C), was selected using a D-optimal design to minimize the number of samples required in the calibration set for PLSR analysis. The top D-optimal-selected PLSR models had root mean squared error of prediction values of 1.4% for HNO 3 and 4.0% for temperature. The PLSR models built from spectra collected on static samples were validated against flow tests including HNO 3 concentration and temperature gradients to test abnormal conditions (e.g., bubbles) and the model performance between sample points in the factor space. Based on cross-validation and prediction modeling statistics, the designed near-infrared absorption approach can provide remote, quantitative analysis of HNO 3 concentration and temperature for production-oriented applications in facilities where laser safety challenges would inhibit the implementation of other optical techniques (e.g., Raman spectroscopy) and in which space, time, and/or resources are constrained. The experimental design approach effectively minimized the number of samples in the training set and maintained or improved PLSR model performance, which makes the described chemometric approach more amenable to nuclear field applications.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2023

Hybrid Mesoporous Carbon/Copper Ferrite Electrode for Asymmetric Supercapacitors

Asymmetric supercapacitors (ASCs) with two dissimilar electrodes are known to exhibit relatively moderate energy and power densities. If electrodes derived from earth-abundant materials or renewable resources such as lignocellulosic biomass (LCB) are used for fabrication, energy storage systems are expected to become less expensive and more sustainable. Hybrid electrode materials have advantages such as higher surface area, better chemical stability, and superior energy density. This study reports on the synthesis of a novel hybrid electrode material containing porous carbon (POC) and copper ferrite, which is designated as POC@Cu-ferrite, and its electrochemical performance in ASC configuration. Corn stover derived hydrochar is utilized for the sol–gel synthesis of POC@Cu-ferrite hybrid material using earth-abundant Cu and Fe-based precursors. This material is characterized using X-ray diffraction (XRD), Raman spectroscopy, Brunauer–Emmett–Teller (BET) surface area analyzer, and scanning and transmission electron microscopy (SEM/TEM). As-synthesized Cu-ferrite is found to contain 89.2% CuFe 2 O 4 and 10.8% Fe 2 O 3 , whereas other phases such as Fe 3 O 4 , CuFeO 2 , and CuO are observed for the POC@Cu-ferrite. BET-specific surface area (SSA) and pore volume of POC@Cu-ferrite are observed as 1068 m 2 /g and 0.72 cm 3 /g, respectively. POC@Cu-ferrite hybrid electrode is used with POC opposite electrode to fabricate ASC, which is tested using Gamry G-300 potentiostat/galvanostat/ZRA to obtain cyclic voltammetry (CV) profiles and galvanostatic charge–discharge (GCD) plots. ASC is also prepared using Cu-ferrite and POC materials and its specific capacitance and stability are compared with ASCs prepared with POC@Cu-ferrite and POC or graphene nanoplatelets (GNPs) electrodes. POC@Cu-ferrite hybrid electrode is found to be superior with a 2-fold higher capacitance and significant electrochemical stability over 100 GCD cycles as compared to the Cu-ferrite electrode.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Correlation of Fabrication Methods and Enhanced Wear Performance in Nanoporous Anodic Aluminum Oxide with Incorporated Molybdenum Disulfide (MoS 2 ) Nanomaterials

Wear performance is integral to component longevity, minimizing industrial waste and excess energy costs in a wide variety of applications. Anodized aluminum oxide (AAO) has many beneficial properties leading to its wide use across industries as a surface treatment for many aluminum components, but the wear properties of the coating could be improved significantly. Here, we used an electrochemical method to incorporate molybdenum disulfide (MoS 2 ), a nanomaterial used as a dry lubricant, to modify alloys of aluminum during AAO preparation. Using Raman spectroscopy and tribological scratch measurements, we thoroughly characterized the structure and wear behavior of the films. The MoS 2 deposition procedure was optimal on aluminum 5052 anodized in higher acid concentrations, with friction coefficients at around 0.05 (~10× better than unmodified AAO). Changing anodization conditions to produce harder films with smaller pores led to worsened wear properties, likely because of lower MoS 2 content. Studying a commercial MoS 2 /AAO film of a different Al alloy (7075) showed that a heat treatment step intended to fully convert all deposited MoS x species to MoS 2 can adversely affect wear in some alloys. While Al 6061 and 1100 produced films with worse wear performance compared to Al 5052 or 7075, our results show evidence that acid cleaning after initial anodization likely removes residual alloying elements, affecting MoS 2 incorporation. This study demonstrates a nanomaterial modified AAO film with superior wear characteristics to unmodified AAO and relates fabrication procedure, film structure, and practical performance.

36 MATERIALS SCIENCE↗
DOE OSTI2022

De Novo Synthesis of Bacteriochlorins Bearing Four Trideuteriomethyl Groups

Site-specific introduction of isotopes in tetrapyrrole macrocycles provides the foundation for probing physicochemical features germane to photosynthetic energy-transduction processes, but has chiefly been done with porphyrins rather than the more biologically relevant hydroporphyrin analogues of native photosynthetic pigments. A prior study incorporated pairwise 13C or 15N atoms in the skeleton of a bacteriochlorin containing a gem-dimethyl group in each pyrroline ring. Here, a complementary effort is reported that installs deuterium atoms in substituents at the perimeter of a bacteriochlorin. Thus, perdeuteriated 3-methyl-2,4-pentanedione was converted in an 8-step synthesis via the intermediacy of tert-butyl 5-formyl-3,4-bis(trideuteriomethyl)pyrrole-2-carboxylate to the 2,3,12,13-tetrakis(trideuteriomethyl)-8,8,18,18-tetramethylbacteriochlorin (BC-2). The fidelity of isotope substitution was maintained throughout the synthesis. Resonance Raman spectroscopy of the copper chelate (CuBC-2) revealed that addition of the four β-pyrrolic substituents alone is not sufficient to account for the vibronic complexity observed for the copper chelate of bacteriochlorophyll a (CuBChl a). The increased vibronic activity exhibited by the natural pigments and CuBChl a must arise from the increased structural complexity of the macrocycle.

Jing, Haoyu (ORCID:0000000178399582)↗
DOE OSTI2023

A Facile Aqueous Solution Route for the Growth of Chalcogenide Perovskite BaZrS 3 Films

The prototypical chalcogenide perovskite, BaZrS 3 (BZS), with its direct bandgap of 1.7–1.8 eV, high chemical stability, and strong light–matter interactions, has garnered significant interest over the past few years. So far, attempts to grow BaZrS 3 films have been limited mainly to physical vapor deposition techniques. Here, we report the fabrication of BZS thin films via a facile aqueous solution route of polymer-assisted deposition (PAD), where the polymer-chelated cation precursor films were sulfurized in a mixed CS 2 and Ar atmosphere. The formation of a single-phase polycrystalline BZS thin film at a processing temperature of 900 °C was confirmed by X-ray diffraction and Raman spectroscopy. The stoichiometry of the films was verified by Rutherford Backscattering spectrometry and energy-dispersive X-ray spectroscopy. The BZS films showed a photoluminescence peak at around 1.8 eV and exhibited a photogenerated current under light illumination at a wavelength of 530 nm. Temperature-dependent resistivity analysis revealed that the conduction of BaZrS 3 films under the dark condition could be described by the Efros–Shklovskii variable range hopping model in the temperature range of 60–300 K, with an activation energy of about 44 meV.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Exploring Mixed Ionic–Electronic-Conducting PVA/PEDOT:PSS Hydrogels as Channel Materials for Organic Electrochemical Transistors

Here, we report the preparation and evaluation of PVA/PEDOT:PSS-conducting hydrogels working as channel materials for OECT applications, focusing on the understanding of their charge transport and transfer properties. Our conducting hydrogels are based on crosslinked PVA with PEDOT:PSS interacting via hydrogen bonding and exhibit an excellent swelling ratio of ~180–200% w/w. Our electrochemical impedance studies indicate that the charge transport and transfer processes at the channel material based on conducting hydrogels are not trivial compared to conducting polymeric films. The most relevant feature is that the ionic transport through the swollen hydrogel is clearly different from the transport through the solution, and the charge transfer and diffusion processes govern the low-frequency regime. In addition, we have performed in operando Raman spectroscopy analyses in the OECT devices supported by first-principle computational simulations corroborating the doping/de-doping processes under different applied gate voltages. The maximum transconductance (gm~1.05 μS) and maximum volumetric capacitance (C*~2.3 F.cm -3 ) values indicate that these conducting hydrogels can be promising candidates as channel materials for OECT devices.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The Reactivity of Polyethylene Microplastics in Water under Low Oxygen Conditions Using Radiation Chemistry

Polyethylene (PE) is an intensely utilized polymer, which has consequently led to it becoming a common environmental contaminant. PE and other plastic waste are known to be highly persistent in surface waters; however, chemical and physical changes do take place over time, dependent mostly on highly variable natural conditions, such as oxygen (O2) availability. Gamma radiation was used to generate reactive oxygen species, namely hydroxyl radicals, in initially aerated aqueous solutions to simulate the natural weathering of microplastics in waters where there are fluctuations and often depletions in dissolved O2. The headspace of the irradiated PE-containing solutions was probed for the formation of degradation products using solid-phase microextraction (SPME) fibers in combination with gas chromatography mass spectrometry (GCMS). The major species detected were n-dodecane, with trace levels of tridecane, 2-dodecanone, and hexadecane, which were believed to be predominately adsorbed in the PE microplastics in excess of their aqueous solubility limits. Surface characterization by Raman spectroscopy and light and dark field microscopy indicated no change in the chemical composition of the irradiated PE microplastics under low O2 to anaerobic conditions. However, morphological changes were observed, indicating radical combination reactions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Exposure of Stainless Steel 316 to Subcritical, Transition, and Near-Supercritical Water

This work investigates the oxidation of austenitic stainless steel 316 at temperatures close to the critical point of water: subcritical water at 330°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water (SCW) at 380°C and 27 MPa. The surfaces of the samples were characterized using x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and x-ray photoelectron spectroscopy before and after exposure. Magnetite (Fe3O4) was found to be present on all surfaces of all samples. The samples exposed to subcritical water also showed the presence of a nickel-iron chromium mixed spinel Ni(Fe2-xCrx)O4. The oxide morphology was observed to vary based on exposure temperature; an increased nucleation and growth rate, and an increased generation of Fe2+ was observed on samples exposed to the transition region and SCW.

Materials Science↗
DOE OSTI2021

Oxidation of Alloy X in Subcritical, Transition, and Supercritical Water

This work investigates the oxidation of a nickel-based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 h. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using x-ray diffraction, Raman spectroscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

Materials Science↗
DOE OSTI2023

Chemical abrasion: the mechanics of zircon dissolution

Chemical abrasion is a technique that combines thermal annealing and partial dissolution in hydrofluoric acid (HF) to selectively remove radiation-damaged portions of zircon crystals prior to U–Pb isotopic analysis, and it is applied ubiquitously to zircon prior to U–Pb isotope dilution thermal ionization mass spectrometry (ID-TIMS). The mechanics of zircon dissolution in HF and the impact of different leaching conditions on the zircon structure, however, are poorly resolved. We present a microstructural investigation that integrates microscale X-ray computed tomography (µCT), scanning electron microscopy, and Raman spectroscopy to evaluate zircon dissolution in HF. We show that µCT is an effective tool for imaging metamictization and complex dissolution networks in three dimensions. Acid frequently reaches crystal interiors via fractures spatially associated with radiation damage zoning and inclusions to dissolve soluble high-U zones, some inclusions, and material around fractures, leaving behind a more crystalline zircon residue. Other acid paths to crystal cores include the dissolution of surface-reaching inclusions and the percolation of acid across zones with high defect densities. In highly crystalline samples dissolution is crystallographically controlled with dissolution proceeding almost exclusively along the c axis. Increasing the leaching temperature from 180 to 210 °C results in deeper etching textures, wider acid paths, more complex internal dissolution networks, and greater volume losses. How a grain dissolves strongly depends on its initial radiation damage content and defect distribution as well as the size and position of inclusions. As such, the effectiveness of any chemical abrasion protocol for ID-TIMS U–Pb geochronology is likely sample-dependent. We also briefly discuss the implications of our findings for deep-time (U-Th)/He thermochronology.

58 GEOSCIENCES↗
NASA NTRS1976

Planetary astronomy program

Visual photometric function data for Saturn's rings were analyzed in terms of elementary anisotropic scattering radiative transfer models which involve the Henyey-Greenstein function. Limits were placed on the combinations of single scattering albedo, and backscattering directivity, which are permitted by observation. Particles with lunar-like scattering properties were excluded by the analysis. Results are consistent with the ring particles being more-or-less pure, and spherical, conglomerates of H2O frost. Multicolor (5500 A-7600 A), narrow band (100 A), area scanning photometry was used to study the wavelength variation in the optical appearance of Uranus. Limb brightening was detected in two CH4 bands, i.e. 6190A and 7300A. Spectrophotometric observations and analysis of the asteroids and Raman spectroscopy of the atmosphere of Uranus are also briefly discussed.

Source record↗
NASA NTRS1977

Instrumentation techniques for studying heterogeneous combustion

Velocity measurements in flames and the simultaneous measurement of droplet size and velocity with the aid of laser anemometry are considered along with methods of particle size measurement and techniques based on laser Raman spectroscopy. Attention is given to high-speed photography and holography, computer compensated thermocouples, and the determination of turbulence characteristics. The employment of suction probes is also discussed, taking into account sampling methods, the effects of temperature change in sampling probes on particle formation, and the chemical analysis of samples.

Chigier, N. A.↗
NASA NTRS1981

A 100 microsec, reliable, 10 Hz pulsed supersonic molecular beam source

A 10-Hz repetition rate, 100-microsec duration, reliable pulsed supersonic molecular beam source is described. Mechanical and electrical design of the pulsed valve are given in detail. Characteristics of the supersonic expansion obtained using coherent anti-Stokes Raman spectroscopy in acetylene are presented. They include pulse shape, gas rotational and translational cooling as a function of distance from the nozzle, clustering effects, and shock heating at the leading edge of the pulse.

Byer, R. L.↗
NASA NTRS1983

CARS temperature measurements in the fuel preburner of the Space Shuttle main engine: A feasibility study

This report discusses the feasibility of making temperature profile measurements in the fuel preburner of the main engine of the space shuttle (SSME) using coherent anti-Stokes Raman spectroscopy (CARS). The principal thrust of the work is to identify problems associated with making CARS measurements in high temperature gas phase hydrogen at very high pressures (approx 400 atmospheres). To this end a theoretical study was made of the characteristics of the CAR spectra of H2 as a function of temperature and pressure and the accuracy with which temperatures can be extracted from this spectra. In addition the experimental problems associated with carrying out these measurements on a SSME at NSTL were identified. A conceptual design of a CARS system suitable for this work is included. Many of the results of the calculations made in this report are plotted as a function of temperature. In the course of presenting these results, it was necessary to decide whether the number of density or the pressure should be treated as a fixed parameter.

Beiting, E. J.↗
NASA NTRS1983

Comparison of CARS combustion temperatures with standard techniques

This paper describes a comparative study of temperatures measured with Coherent Anti-Stokes Raman Spectroscopy (CARS) and those using standard measurement techniques. CARS temperatures from nitrogen vibrational-rotational spectra have been obtained in a premixed hydrogen-air laboratory flame supported on a flat flame burner over a temperature range from about 1000 K to 2100 K. The techniques used for comparison were sodium line reversal, thin wire thermocouples and heat balance calculations. These studies show a good agreement over the entire temperature range studied.

Antcliff, R. R.↗
NASA NTRS1983

Coherent Anti-Stokes Raman scattering with reflective optics

Attention is given to the implementation of a novel reflective optics configuration in which the lens normally employed for focusing and crossing the input laser beams in Coherent Anti-Stokes Raman spectroscopy (CARS) is replaced by a spherical mirror, allowing large crossing angles to be obtained with a single focusing device and permitting the laser generation and collection equipment to be located on one side of the sample region. The experimental results obtained demonstrate the feasibility of mirror-based CARS in remote combustion diagnostics.

Antcliff, R. R.↗