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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 1,027 records · Page 57
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Damage-free X-ray spectroscopy characterization of oxide thin films

Thin polymer or oxide films are ubiquitous components in many devices, including membranes for filtration or electrodes in electrochemical energy storage. High energy electron or x-ray probes for microscopy and spectroscopy are useful to characterize and understand these materials. However, irreversible damage by the probe radiation remains a challenge. Here, we show that graphene serves as an x-ray and electron transparent substrate that substantially reduces radiation damage of an oxide thin film. We demonstrate this using highly focused x-ray beams, which show that compared to oxide thin films supported on a substrate, graphene-supported regions show minimal changes in the x-ray spectra as a function of x-ray dose. Further, these results pave the way for the development of experimental setups that allow for long exposure time measurements with limited sample damage and substrate-directed radiation patterning.

36 MATERIALS SCIENCE↗
DOE OSTI2023

A novel method for quantifying irradiation damage in nuclear graphite using Raman spectroscopy

Raman spectroscopy has long been used in studying irradiation damage in carbon/graphite materials. It is however unclear if the measurements from different types of materials are directly comparable. Further, decoupling the contribution from irradiation temperature and fluence to the total damage in nuclear graphite possessing irradiation damage gradient is currently not readily feasible as it requires a complete set of test reactor irradiation experiments over the relevant temperature and fluence range. A novel methodology has therefore been proposed and developed to quantify total irradiation damage evolution at crystal level based on graphite Raman G-band position shift. Specifically, G-band positions derived from a large number of spectra collected from the fractured surface of microfine-grained POCO ZXF-5Q graphite possessing proton irradiation damage gradient were plotted with open literature Raman data on HOPG, BEPO (AXGP graphite), PCEA and IG-110 graphite as a function of dpa. The total damage level within 2σ beam radius in this POCO graphite was estimated to be equivalent to ~2–5 dpa at ~350–370 °C. Derived G-band positions were then mapped to the three-stage amorphization trajectory model indicating beam centre area has entered the second stage, i.e., transitioning from nanocrystalline graphite into amorphous carbon. G-band position relative shift (ΔG) curve with a ‘turn-around’ peak as a function of total damage can be used for in-service lifetime prediction. Importantly, the developed methodology has the potential to ‘unify’ total damage levels across different grades of nuclear graphite caused by ion, neutron and proton irradiation at different temperatures.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Tracking the prelude of the electroreduction of carbon monoxide via its interaction with Cu(100): Studies by operando scanning tunneling microscopy and infrared spectroscopy

The first isolable intermediate in the electrochemical reduction of carbon dioxide is carbon monoxide. This species, or its hydrated form, formic acid, is also the primary end product from all but a handful of metallic electrodes; with the latter, hydrogen gas is generated, but it emanates from the reduction of water and not from CO 2 . Only one electrode material, zerovalent copper, can spawn, in greater-than-trace quantities, a variety of species that are more highly reduced than CO. Hence, if the aim is to pursue a reaction trail of the reduction of CO 2 to products other than CO, it would be both logical and expedient to track the electrocatalytic reaction of CO itself. Heterogeneous electrocatalysis is a surface phenomenon; it transpires only when the reactant, CO in this case, chemisorbs on, or chemically interacts with, the Cu electrode surface. There is no electrocatalytic reaction if there is no CO adsorption. In ultrahigh vacuum, no CO resides on the Cu(100) surface at temperatures higher than 200 K. However, under electrochemical conditions, CO is chemisorbed on Cu at ambient temperatures at a given potential. Here, we thus paired, in seriatim fashion, scanning tunneling microscopy (STM) and polarization-modulation IR reflection-absorption spectroscopy (PMIRS) to document the influence of applied potential on the coverage, the molecular orientation, and the adlattice structure of CO adsorbed on Cu(100) in alkaline solutions; the results are described in this paper.

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

Mechanisms of Zn removal from water by amorphous geopolymer: Molecular-level insights from X-ray absorption spectroscopy, isotope fractionation, and surface complexation modeling

Porous geopolymers have attracted widespread attention as promising heavy metal adsorbents that can be synthesized from aluminosilicate solid wastes. However, the precise microstructural evidence for adsorbed heavy metals on geopolymers remains unclear due to the insensitivity of conventional characterization techniques on minerals with amorphous structure and surface disorder. Batch adsorption and column experiments coupled with X-ray absorption spectroscopy (XAS), Zn stable isotope, and surface complexation model (SCM) were employed to reveal the Zn removal mechanisms with coal fly ash porous geopolymer (CFAPG) at a molecular scale. The macroscopic kinetic and isothermal adsorption of Zn on CFAPG were well described by the pseudo-second-order model and Bi_Langmuir equation, respectively, indicating the presence of abundant heterogeneous active sites on the CFAPG surface. Further, two types of active sites on the CFAPG surface were identified by XAS coupled with Zn isotopes in batch experiments at pH <= 6.0: one is pH-dependent and associated with tetrahedral zinc coordi-nation, and the other is pH-insensitive and associated with octahedral zinc coordination; these sites were confirmed by the bidentate SCM as the variable charge site (surface complexation, >S-OH) and the permanent negative charge site (cation exchange, >X - ), respectively. Furthermore, the important contribution of surface co -precipitation besides surface complexation and cation exchange to the Zn adsorption on CFAPG was identified by XAS coupled with SCM in a flow-through column experiment at pH >6.0. These investigations provide a systemic understanding of the Zn adsorption mechanisms on CFAPG and an SCM reference for the application and prediction of geopolymers in heavy metal-contaminated water remediations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Evaluation of microstructural changes in fresh cement paste using AC impedance spectroscopy vs. oscillation rheology and 1H NMR relaxometry

AC impedance spectroscopy (ACIS) is a promising technique for monitoring the microstructure evolution of fresh cement paste in real-time. This paper compared the change of bulk electric resistivity (ρ{sub bulk}) obtained from ACIS with the developments of storage modulus (G′) and the mean transverse relaxation times (T{sub 2}) of fresh Portland cement pastes within 5 h. It was found that the three different phases (Phase I, II, and III) on the microstructural build-up process of fresh paste can be accurately distinguished by analyzing ρ{sub bulk}, as well as G′ and T{sub 2}. The use of ρ{sub bulk} fails to characterize the microstructural changes in Phase I due to the great sensitivity on the electrical conductivity of the interstitial solution. However, it can successfully reflect the developing features of microstructure in Phases II and III, and reliably evaluate the impacts of water to cement ratio, superplasticizer, and supplementary cementitious materials on the microstructural development.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evaluation of adsorption and mechanical strength of 13X zeolite mixtures with phyllosilicate binders using molecular dynamics simulation and positron annihilation spectroscopy

There is growing interest in developing zeolites with novel internal structures that have optimal adsorptive capacity and high mechanical strength, while offering advantages, such as being light weight. We integrate computational and experimental methods to explore the effect of binder/zeolite types, and weight percentages on the mechanical strength of 13X zeolite and adsorption capacities of N 2 , H 2 O, and CO 2 for additive manufacturing (AM) applications with the goal of maximizing both adsorption and strength. Zeolite 13X mixtures and phyllosilicate binders (either bentonite or kaolin) are combined using molecular dynamics (MD) simulations to create structures with various binder/zeolite weight percentages. Further, adsorption capabilities and mechanical strength are assessed using the grand canonical Monte Carlo (GCMC) and ReaxFF modules, respectively. Our modeling shows that an optimized zeolite/binder ratio for N 2 adsorption is around 15 wt% for kaolin and roughly 10 wt% for bentonite. The resulting parameters can be applied to facilitate macro-scale computational fluid dynamics (CFD) and finite element method (FEM) simulations of an AM zeolite structure. We also performed Positron Annihilation Lifetime Spectroscopy (PALS) measurements on zeolite samples to explore the effect of changes in the internal volume. The results show an inverse relationship between the free volume and the solid loading and adding a binder changes the morphology of the zeolite-binder compound and decreases open-volume area significantly.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Quantification of the REE 3+ aqua ions and chloride species in aqueous fluids by in situ Raman spectroscopy using perturbations of the water band

Acidic NaCl-rich aqueous fluids play a crucial role in forming hydrothermal rare earth elements (REE) mineral deposits. Aqueous REE mobility is mostly controlled by the stabilities of REE 3+ and REE chloride species. Our current knowledge of REE speciation is based on solubility data, thermodynamic models and in situ spectroscopic measurements, sometimes coupled with molecular simulations. Here, in this study, we investigate Nd and Yb speciation in pH2 Cl-bearing solutions at 25 °C and 0.1 MPa with variable Cl/REE ratios using Raman Spectroscopy in solutions with 0.1 to 0.6 mol/kg NdCl 3 or YbCl 3 and 0.2 to 3.2 mol/kg NaCl. Due to the challenges in resolving the REE-Cl band, we developed a new method using the water vibrational mode and multivariate curve resolution (MCR) analysis. The Raman spectra for the vibrational band of water (2700 to 3900 cm –1 ) were collected at 25 °C and fitted by three Gaussian sub-peaks, then quantified using MCR analysis to de-convolute the water band into bulk H 2 O and the perturbations caused by of Cl – , REE 3+ , and REE chloride species. REE speciation based on the perturbations of the water band indicates that REE 3+ aqua ions dominate acidic solutions at 25 °C, but up to ~20 mol% YbCl 2+ forms at high YbCl 3 concentrations. The new method is promising for quantifying in situ speciation of the REE 3+ aqua ions and REE chloride species in aqueous fluids while providing information on the hydration of ions. This method improves our molecular level understanding of REE aqueous species stability and their role in REE mobilization during fluid-rock interaction.

58 GEOSCIENCES↗
DOE OSTI2025

Probing air-water interfaces of dibutyl phosphoric acid (HDBP) aqueous solutions using vibrational sum frequency generation (vSFG) spectroscopy

Liquid-liquid extraction is a separation technique implemented in a wide variety of areas, achieving particular success in both the nuclear and biomedical fields. In this work, vibrational sum frequency generation spectroscopy (VSFG) and surface tension measurements were used to investigate the adsorption of dibutyl phosphate (DBP) at air-aqueous interfaces to simulate liquid-liquid systems relevant to the Plutonium Uranium Redox Extraction (PUREX) Process. The objective of this work is to establish qualitative relationships between changes in the bulk aqueous phase concentrations of DBP and its concentration and structure at air-liquid interface as probed with VSFG. Nitric acid concentration and solution ionic strength were varied to examine their effect on the interfacial DBP.. Introduction of DBP into neat water resulted in reduction of the VSFG spectral intensity in the dangling O-H region (3680 – 3800 cm -1 ) but large increase in the H-bonded O-H stretch frequency region (3000 – 3500 cm-1) and the appearance of the CH 3 symmetric stretch and CH 3 Fermi resonance peaks at ~ 2880 and 2945 cm -1 , respectively, indicating DBP at the air-water interface. The intensity of the C-H strecth peaks increased as DBP concentration increased from 0.24 to 32 mM, accompanied by a decreasing surface tension values. At fixed DBP concentration, the addition of either or both of HNO 3 and NaNO 3 to an ionic strength of 1 M or 3 M led to significant reduction of the O-H VSFG peaks and enhancement of the C-H peaks. The origins of these experimental observations are attributed to both the increased HDBP molecules partitioning and adsorption to the interface and the protonation of the interfacial DBP- molecules.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

The deep-DRT: A deep neural network approach to deconvolve the distribution of relaxation times from multidimensional electrochemical impedance spectroscopy data

Electrochemical impedance spectroscopy (EIS) is an experimental technique ubiquitously used to study electrochemical systems. However, conventional EIS data interpretation through physical and equivalent circuit models is challenging because physical models are problem-specific, and equivalent circuits are often just lumped-element analogs lacking physical meaning. The distribution of relaxation times (DRT) has emerged as a complementary approach to resolve these issues. One drawback of conventional DRT deconvolution is that the EIS data is understood to be (only) a function of frequency (i.e. 1D data) and deconvolved accordingly. This work proposes a novel deconvolution method based on deep neural networks (DNNs), allowing the analysis of multidimensional EIS spectra to bridge data dependency on both frequencies and experimental conditions. Two particularly appealing traits of the deep-DRT method developed in this article are that neither regularization nor specific spacing on the state variables defining the experiment are required. Finally, leveraging DNN to examine complex EIS spectra and their dependence on experimental conditions, this work opens a new research direction in the area of EIS analysis and DRT deconvolution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

A comprehensive review of diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) techniques in protonic ceramic cells (PCCs): Current status and future perspective

Protonic ceramic cells (PCCs) have emerged as a promising technology for power generation, energy storage, and value-added chemical synthesis, offering benefits such as fuel flexibility, low emissions, and efficient operation at intermediate temperatures (300–600 ​°C). Recently, significant breakthroughs in materials and manufacturing methods have markedly enhanced the performance of PCCs. However, establishing a fundamental understanding of their electrocatalytic reactions has gained less attention. As a fast and cost-effective method for physicochemical fingerprinting, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) has proven to be a surface-sensitive analytical tool for structural and functional studies. This review critically examines the most up-to-date applications of DRIFTS for characterizing key components of PCCs, including oxygen electrodes, protonic electrolytes, and hydrogen electrodes for different applications, with a focus on revealing hydration properties and catalytic reactions, and guiding rational material design. The challenges for advancing DRIFTS, including quantitative capabilities and operando applications for PCC investigations, are highlighted and strategies to tackle these challenges are discussed. Ultimately, this review underscores the critical role of DRIFTS in accelerating the development of high-performance and durable PCCs for next-generation energy solutions, offering methodologies and insights broadly applicable to a wide range of electrochemical energy conversion and storage technologies.

Diffuse Reflectance Infrared Fourier Transform Spe↗
DOE OSTI2020

Dual frequency comb spectroscopy of solid fuel pyrolysis and combustion: Quantifying the influence of moisture content in Douglas fir

As the fire research community develops multi-scale models to predict the spread of wildland fires, there is a need for well-controlled, small-scale experiments which provide benchmark data and fundamental understanding of the effects of key parameters on the combustion of wildland fuels. Here, we implement a unique suite of non-intrusive, quantitative diagnostics that simultaneously measure mass loss, surface temperature, in situ gas temperature and water vapor concentration, including the first implementation of dual frequency comb spectroscopy for the study of solid fuels. As a demonstration, we examine the effect of fuel moisture content on the burning of Douglas fir wood samples that are ignited under constant radiative heat flux from a cone calorimeter to provide benchmark data for multi-scale models. Peak flame temperatures 3 mm above the sample surface measured with the dual frequency comb laser spectrometer are in excess of 1200 K. The flame temperature decreases by over 150 K as fuel moisture content increases from 0.7% to 40%. This work demonstrates a platform for simultaneous, quantitative measurements of well-controlled small-scale experiments which provide benchmark data for the development of advanced modeling and simulations capable of capturing the complex physics present in wildland fire systems.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Synthetic aromatic kerosene property prediction improvements with isomer specific characterization via GCxGC and vacuum ultraviolet spectroscopy

This research explores an advanced method of fuel composition determination and builds upon typical hydrocarbon group type analyses performed with two-dimensional gas chromatography (GCxGC). In this study, structural information of individual species within Virent’s Synthetic Aromatic Kerosene (SAK) is identified by vacuum ultraviolet (VUV) spectroscopy. By mass, 71.3% of the components elute within six peaks of the chromatogram, from which 12 unique species are identified through a novel deconvolution method. Overall, the identification of 93.6%m across 26 structural isomers is made by the methods described in this work. With 93.6%m ascribed to specific isomers, the precision of fuel property predictions improves dramatically. For example, the absolute error of the viscosity prediction is reduced by 90% because of this advancement in diagnostic capability, and its 95-percentile confidence interval (precision only) is reduced by 93%. Additionally, the properties of SAK, blended with hydro processed esters fatty acids (HEFA), are demonstrated to have blended properties consistent with conventional jet fuel.

10 SYNTHETIC FUELS↗
DOE OSTI2023

Application of machine learning for optical emission spectroscopy data in NAGDIS-II

In this study, we applied machine learning to optical emission spectroscopy (OES) data and device parameters from the linear plasma device NAGDIS-II to explore the potential application of machine learning for predicting electron density, $n$ e , and temperature, $T$ e . The covered ranges of $n$ e and $T$ e , which were measured by an electrostatic probe, are 3.6 × 10 17 –2.4 × 10 19 m -3 and 0.3–7.1 eV, respectively. A three hidden layer neural network (NN) is introduced to model the relationship between $n$ e /$T$ e and the combination of line intensities, radial position, and device parameters. It is shown that the errors in $n$ e and $T$ e become 18.0 and 18.8%, respectively, which were almost the same level for the electrostatic probe, using all available data. Lasso regression and greedy algorithm are used to select the necessary line emissions. In conclusion, it is shown that four- or five-line intensities are sufficient to obtain almost the same quality as the one with all the other lines.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2023

Electrochemical Li intercalation in b-As y P 1–y alloys: In-situ Raman spectroscopy study

Structural evolution of b-As y P 1-y alloys with varying As concentration, y was studied during Li-intercalation using in-situ Raman spectroscopy. A monotonic redshift of all the vibrational modes corresponding to P-P bonds (A 1 g , A 2 g , B 2g ), As-As bonds (A 1 g , A 2 g , B 2g ), and As-P bonds of all the samples was observed during the initial stages of the intercalation process due to the softening of each mode caused by the intercalation driven donor-type charge-transfer from Li to b-As y P 1-y . The emergence of a new peak identified as the E g mode of gray As, above an intercalation threshold, is indicative of the presence of an intercalation-driven structural phase segregation process. Further, the A 1g mode of gray As emerging after this intercalation threshold lies in close proximity of the A 2 g Raman mode of b-As y P 1-y . All the peaks beyond the intercalation threshold show an upshift due to the co-existence of gray As with b-As y P 1-y alloys causing strain and thus hardening of the phonon modes. In the sample with the highest As concentration phase segregation takes place during the synthesis process. Computational modeling reveals the co-existence of gray As in the b-As y P 1-y alloys with high As concentrations. It also confirms the existence of a local structural segregation taking place at a critical Li concentration during the intercalation process. Furthermore, this work shows the significance of intercalation on structural changes in the search for new phases of b-As y P 1-y alloys.

2D Materials↗
DOE OSTI2025

Probing the Self-Assembly dynamics of cellulose nanocrystals by X-ray photon correlation spectroscopy

Charge-stabilized colloidal cellulose nanocrystals (CNCs) can self-assemble into higher-ordered chiral nematic structures by varying the volume fraction. The assembly process exhibits distinct dynamics during the isotropic to liquid crystal phase transition, which can be elucidated using X-ray photon correlation spectroscopy (XPCS). Anionic CNCs were dispersed in propylene glycol (PG) and water spanning a range of volume fractions, encompassing several phase transitions. Coupled with traditional characterization techniques, XPCS was conducted to monitor the dynamic evolution of the different phases. Additionally, simulated XPCS results were obtained using colloidal rods and compared with the experimental data, offering additional insights into the dynamic behavior of the system. The results indicate that the particle dynamics of CNCs undergo a stepped decay in three stages during the self-assembly process in PG, coinciding with the observed phases. The phase transitions are associated with a total drop of Brownian diffusion rates by four orders of magnitude, a decrease of more than a thousand times slower than expected in an ideal system of repulsive Brownian rods. Given the similarity in the phase behaviors in CNCs dispersed in PG and in water, we hypothesize that these dynamic behaviors can be extrapolated to other polar solvent environments. Importantly, these findings represent the direct measurement of CNC dynamics using XPCS, underscoring the feasibility of directly assessing the dynamic behavior of other rod-like colloidal suspensions.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Reprint of "Selective conversion of CO into ethanol on Cu(511) surface reconstructed from Cu(pc): Operando studies by electrochemical scanning tunneling microscopy, mass spectrometry, quartz crystal nanobalance, and infrared spectroscopy"

A polycrystalline copper, surface-terminated by a well-defined (511)-oriented facet, was electrochemically generated by a series of step-wise surface reconstruction and iterations of mild oxidative-reductive processes in 0.1 M KOH. The electrochemical reduction of CO on the resultant stepped surface was investigated by four surface-sensitive operando methodologies: electrochemical scanning tunneling microscopy (STM), electrochemical quartz crystal nanobalance (EQCN), differential electrochemical mass spectrometry (DEMS), and polarization-modulation infrared spectroscopy (PMIRS). The stepped surface catalyzed the facile conversion of CO into ethanol, the exclusive alcohol product at a low overpotential of -1.06 V (SHE) or - 0.3 V (RHE). Additionally, the chemisorption of CO was found to be a necessary prelude to ethanol production; i.e. the surface coverages, rather than solution concentrations, of CO and its surface-bound intermediates primarily dictate the reaction rates (current densities). Contrary to the expected predominance of undercoordinated step-site reactivity over the coordination chemistry of vicinal surfaces, vibrational spectroscopic evidence reveals the involvement of terrace-bound CO adsorbates during the multi-atomic transformations associated with the production of ethanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Cell design for laser-induced breakdown spectroscopy measurements on reactive gas samples

Uranium hexafluoride (UF 6 ) is the primary material used for the enrichment of uranium in the production of light water nuclear reactor fuels worldwide. Accurate, rapid quantification of uranium isotopic composition in nuclear materials is required for safeguards programs and nonproliferation purposes. One potential technique for isotopic measurements in uranium species in the field is laser induced breakdown spectroscopy (LIBS). Safe and effective application of LIBS to UF 6 for enrichment measurements is uniquely challenging due to the chemical and physical properties of UF 6 , which necessitate specific handling procedures. The objective of this work is to design a cell for isotopic analysis of UF 6 that is (1) compatible with chemical and physical properties of UF 6 , (2) compatible with LIBS laser, and (3) portable-sized for nuclear safeguards applications. Along with cell design, initial testing of the cell for basic performance and chemical compatibility is performed. As designed and constructed, the portable gas cell was gas-tight, chemically compatible with UF 6 , and withstood long-duration laser exposure. In this work, the cell has proven capability for handling reactive gasses, such as UF 6 , with specification application to isotopic analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

In-situ investigation of the vibrational properties of H 2 O CO 2 -bearing and dry K-rich basaltic glasses at high pressure by mid infrared spectroscopy

Here, the vibrational properties of CO 2 –H 2 O-bearing and dry synthetic K-rich basaltic glasses were investigated at room temperature and pressures between 0.0001–5.5 GPa using the diamond anvil cell combined with in situ reflectance and transmittance Fourier Transform infrared micro-spectroscopy. The absorption coefficient a(v) calculated from the Kramers-Kronig relation shows that glasses are dominated by the Q 2 aluminosilicate unit followed by Q 1 , Q 3 . The variation in Q n concentration upon compression suggests that glasses undergo polymerization from ambient pressure to 2 GPa followed by less marked structural changes up to 4 GPa, above which the structure is further polymerized. Once decompressed, glasses retained a polymerized structure. Our results show that 1.03 wt% CO 2 -1.42 wt% H 2 O in a glass with 3.10 wt% K 2 O and 46.77 wt% SiO 2 prevent the formation of fully polymerized connections when cold-compressed. Our results can be used to explain the effect of volatiles and alkali on the rheology of natural basaltic magmas.

36 MATERIALS SCIENCE↗