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DOE OSTI2023

Chapter 14: Surface plasmon resonance enhanced artificial photosynthesis of chemical fuels for energy storage

Nanostructured noble metals such as Au, Ag, and Cu have interesting optical properties because of the oscillation motions of their surface electrons upon strong coupling with light under resonance conditions. This resonant oscillation motion of conduction electrons refers to surface plasmon resonance (SPR) and localized SPR (LSPR) when localized near the surface of a nanoparticle. The extinction spectrum of a solution of plasmonic nanoparticles has tunable wavelength responses from UV to NIR due to strong light scattering and absorption which are highly sensitive to the permittivity of the nanoparticles, their sizes and shapes, and chemical environment. Strong light scattering due to the LSPR of plasmonic nanoparticles creates a strong localized and far-field intensity capable of enhancing light absorption characteristics of a chromophore near a plasmonic surface. Engineering the chromophores’ radiative decay dynamics can be done by 1) increasing its radiative decay rate to increase its photoluminescence intensity and 2) increasing its nonradiative decay rates associated to direct charge transfer to the metal surface. Such interesting photophysical properties of a chromophore can be extended to other light-absorbing materials such as semiconductor thin films and nanostructures. This plasmonic effect on the photophysics of a light-absorbing material can be theoretically and experimentally validated. The phenomenon has also been applied to advanced optoelectronic devices such as organic light-emitting diodes (OLED)1 and organic photovoltaics (OPV).2-4 The local field created by the SPR can provide an intense EM field to enhance photoluminescence emission of an organic chromophore5-8 and Raman scattering of an organic molecule, and single-molecule Raman9-10 can be detected on specially designed LSPR substrate. (Figure 1 on SPR for energy) Recent studies suggest that LSPR can be incorporated in light-harvesting and conversion systems to increase energy conversion in a solar cell and photoelectrochemical cell and chemical transformations of CO2 to chemical fuels.11-12 Plasmonic active metals naturally exhibit catalytic activities for electrochemical fuel conversion that can be enhanced by engineering their structures to form unique catalytic structures such as symmetry-broken Au-Cu Janus nanocrystals.13 These studies are critical to addressing the global challenges of energy14-15 and CO2 emission from nonrenewable sources such as coal, petroleum, and natural gas.16-17 Electrochemical systems comprised of unique photonic structures and functions that enable efficient and affordable energy harvesting/conversion/storage are highly desired for providing safe and environment-friendly energy sources. This chapter reviews our recent work of LSPR enabled photoelectrochemical water splitting and recent advances in LSPR-enabled CO2 reduction and photochemical reactions reported in the literature. Scientific and technical challenges of applying LSPR to enhance these energy conversion and storage systems are discussed at the conclusion of this chapter.

Pan, Shanlin↗

DOE OSTI2021

Ionizing photon interactions modulate the optical properties of crystals with femtosecond scale temporal resolution

In this work, we continue our study of a new method for the detection of ionizing radiation with the potential for a dramatic improvement in coincidence time resolution (CTR) for time-of-flight positron emission tomography (ToF-PET) using the modulation of a material's optical properties instead of the scintillation mechanism. Our previous work has shown that for non-scintillation materials such as bismuth silicon oxide (BSO) and cadmium telluride (CdTe), their refractive index can be modulated by annihilation photon interactions. Additionally, the ultrafast nature of this process however remains unexplored. The ionizing radiation-induced charge carriers alter the local band structure in these materials, thus changing the complex refractive index. This mechanism is routinely used at the linac coherent light source (LCLS) facility of the SLAC National Accelerator Laboratory to measure x-ray pulse arrival times with femtosecond scale resolution for photon energies between 0.5 and 10 keV. The method described here follows that example by using a frequency chirped visible continuum pulse to provide a monotonic wavelength-to-time mapping by which one can measure the time-dependent refractive index modulation. In addition, we describe an interference-based measurement setup that allows for significantly improved sensitivity while preserving a timing precision of approximately 10 fs (σ) when measuring the arrival time of below 10 keV x-ray pulses with yttrium aluminum garnet (YAG) crystal. The method is presented in the context of ToF-PET application with further discussions on the potential CTR achievable if a similar detection concept is adopted for detecting 511 keV photons. Semi-empirical analysis indicates that the predicted CTR achievable is on the order of 1 ps (FWHM).

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2007

Differential Radiometers Using Fabry-Perot Interferometric Technique for Remote Sensing of Greenhouse Gases

A new type of remote sensing radiometer based upon the Fabry-Perot interferometric technique has been developed at NASA's Goddard Space Flight Center and tested from both ground and aircraft platform. The sensor uses direct or reflected sunlight and has channels for measuring column concentration of carbon dioxide at 1570 nm, oxygen lines sensitive to pressure and temperature at 762 and 768 nm, and water vapor (940 nm). A solid Fabry-Perot etalon is used as a tunable narrow bandpass filter to restrict the measurement to the gas of interest's absorption bands. By adjusting the temperature of the etalon, which changes the index of refraction of its material, the transmission fringes can be brought into nearly exact correspondence with absorption lines of the particular species. With this alignment between absorption lines and fringes, changes in the amount of a species in the atmosphere strongly affect the amount of light transmitted by the etalon and can be related to gas concentration. The technique is applicable to different chemical species. We have performed simulations and instrument design studies for CH4, "Cot isotope, and CO detection. Index Terms- Absorbing media, Atmospheric measurements, Fabry-Perot interferometers, Optical interferometry, Remote sensing.

Georgieva, Elena M.↗

DOE OSTI2020

Ptychographic atomic electron tomography: Towards three-dimensional imaging of individual light atoms in materials

Through numerical simulations, we demonstrate the combination of ptychography and atomic electron tomography as an effective method for low dose imaging of individual low-Z atoms in three dimensions. After generating noisy diffraction patterns with multislice simulations of an aberration-corrected scanning transmission electron microscope through a 5-nm zinc-oxide nanoparticle, we have achieved three-dimensional (3D) imaging of individual zinc and oxygen atoms and their defects by performing tomography on ptychographic projections. The methodology has also been simulated in 2D materials, resolving individual sulfur atoms in vertical WS 2 /WSe 2 van der Waals heterostructure with a low total electron dose where annular-dark-field images fail to resolve. Overall, we envision that the development of this method could be instrumental in studying the precise 3D atomic structures of radiation sensitive systems and low-Z atomic structures such as 2D heterostructures, catalysts, functional oxides, and glasses.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

ORNL Second Target Station Project: Biological & Environmental Science Workshop

Recent advances in neutron sources and instrumentation have opened up many new opportunities for the application of neutron scattering techniques in the biological and environmental sciences. Neutrons enable studies of the structure and dynamics of biological and environmental samples with a particular sensitivity to light elements, such as hydrogen, which is a key component of biological and environmental samples. Studies using neutrons are complementary to X-rays and have the unique advantage of being non-destructive and highly-penetrating. Oak Ridge National Laboratory’s upcoming Spallation Neutron Source (SNS) Second Target Station (STS) will provide high brightness cold neutron sources that significantly advance the scientific capabilities of neutron scattering instruments. The STS will advance our understanding of biological and environmental processes across spatial and temporal scales. The capabilities will enhance our ability to discover, design, and develop new materials essential for advanced sustainable technologies to address society’s most pressing needs. This report summarizes the discussions and recommendations from a joint workshop held by the STS Project and the Biological and Environmental Systems Science Directorate (BESSD) in June 2022. The purpose of the workshop was to explore science opportunities and capabilities related to biological and environmental systems that could be incorporated into both current and future STS instrument designs, as well as additional instruments at the SNS First Target Station (FTS) and High Flux Isotope Reactor (HFIR). With six breakout sessions, each with two invited plenary speakers from other institutions, the participants discussed a wide range of topics relevant to biological and environmental research. Based on the input from participants, a number of recommendations on instrumentation, sample environments, complementary multi-modal methods, data processing and analysis and sample deuteration are provided in the report. The participants also identified science opportunities that are emerging from the planned instrument capabilities at STS. Selected recommendations and science opportunities are listed in the Executive Summary.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2003

Instrument for Measuring Temperature of Water

A pseudo-Brewster-angle infrared radiometer has been proposed for use in noncontact measurement of the surface temperature of a large body of water (e.g., a lake or ocean). This radiometer could be situated on a waterborne, airborne, or spaceborne platform. The design of the pseudo-Brewster-angle radiometer would exploit the spectral-emissivity and polarization characteristics of water to minimize errors attributable to the emissivity of water and to the reflection of downwelling (e.g., Solar and cloud-reflected) infrared radiation. The relevant emissivity and polarization characteristics are the following: . The Brewster angle is the angle at which light polarized parallel to the plane of incidence on a purely dielectric material is not reflected. The pseudo-Brewster angle, defined for a lossy dielectric (somewhat electrically conductive) material, is the angle for which the reflectivity for parallel-polarized light is minimized. For pure water, the reflectivity for parallel-polarized light is only 2.2 x 10(exp -4) at its pseudo- Brewster angle of 51deg. The reflectivity remains near zero, several degrees off from the 51deg optimum, allowing this angle of incidence requirement to be easily achieved. . The wavelength range of interest for measuring water temperatures is 8 to 12 microns. The emissivity of water for parallel- polarized light at the pseudo-Brewster angle is greater than 0.999 in this wavelength range. The radiometer would be sensitive in the wavelength range of 8 to 12 microns, would be equipped with a polarizer to discriminate against infrared light polarized perpendicular to the plane of incidence, and would be aimed toward a body of water at the pseudo- Brewster angle (see figure). Because the infrared radiation entering the radiometer would be polarized parallel to the plane of incidence and because very little downwelling parallel-polarized radiation would be reflected into the radiometer on account of the pseudo-Brewster arrangement, the radiation received by the radiometer would consist almost entirely of thermal emission from the surface of the water. Because the emissivity of the water would be very close to 1, the water could be regarded as a close approximation of a blackbody for the purpose of computing its surface temperature from the radiometer measurements by use of the Planck radiation law.

Ryan, Robert↗

DOE OSTI2022

Metallic support films reduce optical heating in cryogenic correlative light and electron tomography

Super-resolved cryogenic correlative light and electron tomography is an emerging method that provides both the single-molecule sensitivity and specificity of fluorescence imaging, and the molecular scale resolution and detailed cellular context of tomography, all in vitrified cells preserved in their native hydrated state. Technical hurdles that limit these correlative experiments need to be overcome for the full potential of this approach to be realized. Chief among these is sample heating due to optical excitation which leads to devitrification, a phase transition from amorphous to crystalline ice. Here, in this work, we show that much of this heating is due to the material properties of the support film of the electron microscopy grid, specifically the absorptivity and thermal conductivity. We demonstrate through experiment and simulation that the properties of the standard holey carbon electron microscopy grid lead to substantial heating under optical excitation. In order to avoid devitrification, optical excitation intensities must be kept orders of magnitude lower than the intensities commonly employed in room temperature super-resolution experiments. We further show that the use of metallic films, either holey gold grids, or custom made holey silver grids, alleviate much of this heating. For example, the holey silver grids permit 20× the optical intensities used on the standard holey carbon grids. Super-resolution correlative experiments conducted on holey silver grids under these increased optical excitation intensities have a corresponding increase in the rate of single-molecule fluorescence localizations. This results in an increased density of localizations and improved correlative imaging without deleterious effects from sample heating.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Bulk and Nanocrystalline Cesium Lead-Halide Perovskites as Seen by Halide Magnetic Resonance

Lead-halide perovskites increasingly mesmerize researchers because they exhibit a high degree of structural defects and dynamics yet nonetheless offer an outstanding (opto)electronic performance on par with the best examples of structurally stable and defect-free semiconductors. This highly unusual feature necessitates the adoption of an experimental and theoretical mindset and the reexamination of techniques that may be uniquely suited to understand these materials. Surprisingly, the suite of methods for the structural characterization of these materials does not commonly include nuclear magnetic resonance (NMR) spectroscopy. The present study showcases both the utility and versatility of halide NMR and NQR (nuclear quadrupole resonance) for probing the structure and structural dynamics of CsPbX 3 (X = Cl, Br, I), in both bulk and nanocrystalline forms. The strong quadrupole couplings, which originate from the interaction between the large quadrupole moments of, e.g., the 35 Cl, 79 Br, and 127 I nuclei, and the local electric-field gradients, are highly sensitive to subtle structural variations, both static and dynamic. The quadrupole interaction can resolve structural changes with accuracies commensurate with synchrotron X-ray diffraction and scattering. It is shown that space-averaged site-disorder is greatly enhanced in the nanocrystals compared to the bulk, while the dynamics of nuclear spin relaxation indicates enhanced structural dynamics in the nanocrystals. The findings from NMR and NQR were corroborated by ab initio molecular dynamics, which point to the role of the surface in causing the radial strain distribution and disorder. These findings showcase a great synergy between solid-state NMR or NQR and molecular dynamics simulations in shedding light on the structure of soft lead-halide semiconductors.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Feasibility of using Low-Cost COTS Sensors for Particulate Monitoring in Space Missions

Real-time measurement of particles suspended in the spacecraft cabin is of great importance to verify that maximum allowable dust concentrations are not exceeded. This is primarily to protect astronaut health, but also has implications for dust-sensitive equipment. Recently, there is growing interest in low-cost commercial off-the-shelf (COTS) particle sensors by air quality researchers for their ability to map concentrations of airborne particulate matter in various terrestrial settings. In addition to low cost (< $2,000), the compact size and minimal weight of these sensors make them a potential choice for space missions. The detection mechanism for these aerosol sensors is typically measurement of light scattered by particles as they flow through a sensing volume. The amount of scattered light for detection depends on the particle size, shape, density, and refractive index of the particle material. Ideally, particle instruments should be calibrated with reference instruments for each different type of aerosol measurement. In this study we review multiple parameters that may impact the performance of state-of-the-art low-cost aerosol sensors. Environmental factors such as temperature, relative humidity, low ambient pressure, radiation and charge environment, partial-gravity and microgravity can affect the accuracy of particle measurements. Characteristics of the dust aerosols including particle size distribution, aerosol composition, refractive index, morphology and concentration levels also affect the measurement accuracy. Finally, we look at these parameters and issues with respect to an example COTS low-cost aerosol sensor. Instrument performance specifications are evaluated, and experiments are performed to measure real-time concentrations of Arizona Road Dust (a terrestrial reference test dust) and lunar dust simulant in a laboratory chamber. Overall, this study provides insight for evaluating spacecraft particulate monitoring technologies and raises questions to be answered before incorporating low-cost COTS sensors in future space missions to dusty destinations.

lunar dust↗

DOE OSTI2020

Reflectivity and PDE of VUV4 Hamamatsu SiPMs in liquid xenon

Considering reflective properties of materials and photodetection efficiency (PDE) of photodetectors is important for optimizing energy resolution and sensitivity of the next generation neutrinoless double beta decay, direct detection dark matter, and neutrino oscillation experiments that will use noble liquid gases, such as nEXO, DARWIN, DarkSide-20k, and DUNE . Little information is currently available about reflectivity and PDE in liquid noble gases, because such measurements are difficult to conduct in a cryogenic environment and at short enough wavelengths. Here we report a measurement of specular reflectivity and relative PDE of Hamamatsu VUV4 silicon photomultipliers (SiPMs) with 50 μ m micro-cells conducted with xenon scintillation light ( ~ 175 nm) in liquid xenon. The specular reflectivity at 15 o incidence of three samples of VUV4 SiPMs is found to be 30.4 ± 1.4%, 28.6 ± 1.3%, and 28.0 ± 1.3%, respectively. The PDE at normal incidence differs by ± 8% (standard deviation) among the three devices. The angular dependence of the reflectivity and PDE was further measured for one of the SiPMs. Both the reflectivity and PDE decrease as the angle of incidence increases. This is the first measurement of an angular dependence of PDE and reflectivity of a SiPM in liquid xenon.

47 OTHER INSTRUMENTATION↗

NASA NTRS2004

Space Application Requirements for Organic Avionics

The NASA Marshall Space Flight Center is currently evaluating polymer based components for application in launch vehicle and propulsion system avionics systems. Organic polymers offer great advantages over inorganic corollaries. Unlike inorganics with crystalline structures defining their sensing characteristics, organic polymers can be engineered to provide varying degrees of sensitivity for various parameters including electro-optic response, second harmonic generation, and piezoelectric response. While great advantages in performance can be achieved with organic polymers, survivability in the operational environment is a key aspect for their practical application. The space environment in particular offers challenges that must be considered in the application of polymer based devices. These challenges include: long term thermal stability for long duration missions, extreme thermal cycling, space radiation tolerance, vacuum operation, low power operation, high operational reliability. Requirements for application of polymer based devices in space avionics systems will be presented and discussed in light of current polymer materials.

Watson, Michael D.↗

DOE OSTI2023

3D printable polyvinyltoluene-based plastic scintillators with pulse shape discrimination

A feasibility of preparing bulk photopolymerized plastics scintillators that contain vinyltoluene with multifunctional monomers, pentaerythritol tetraacrylate is shown. This formulation offers a simple and fast way to prepare polyvinyltoluene-based plastics with efficient fast neutron/gamma pulse shape discrimination (PSD) within minutes. 30 wt% of 2,5-diphenyloxazole (PPO) was added in the mixtures of vinyltoluene and pentaerythritol tetraacrylate with different secondary dyes to understand the effect of dyes on the scintillation. Prepared resins were photopolymerized under different conditions, and the scintillation performance was compared to a commercially available standard, EJ-276. Additional functionality for thermal neutron sensitivity was introduced by the incorporation of 6 Li and 6 B nuclei. With optimized conditions, prepared plastics showed light output up to 90% relative to the same size of EJ-276. Here, the best plastic scintillators had PSD figures of merit (FoMs) up to 2.77 compared to 3.25 of EJ-276. The 3D-printability of the tested formulations was demonstrated.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Phase Transition Dynamics in a Complex Oxide Heterostructure

Understanding the behavior of defects in the complex oxides is key to controlling myriad ionic and electronic properties in these multifunctional materials. The observation of defect dynamics, however, requires a unique probe-one sensitive to the configuration of defects as well as its time evolution. Here, we present measurements of oxygen vacancy ordering in epitaxial thin films of SrCoO x and the brownmillerite-perovskite phase transition employing x-ray photon correlation spectroscopy. These and associated synchrotron measurements and theory calculations reveal the close interaction between the kinetics and the dynamics of the phase transition, showing how spatial and temporal fluctuations of heterointerface evolve during the transformation process. The energetics of the transition are correlated with the behavior of oxygen vacancies, and the dimensionality of the transformation is shown to depend strongly on whether the phase is undergoing oxidation or reduction. Finally, the experimental and theoretical methods described here are broadly applicable to in situ measurements of dynamic phase behavior and demonstrate how coherence may be employed for novel studies of the complex oxides as enabled by the arrival of fourth-generation hard x-ray coherent light sources.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Colloids in Microgravity

Colloidal particles are important in a broad range of applications in technology and materials processing. Due to high sensitivity to thermal fluctuations, a suspension of colloidal particles is considered as an assembly of super-atoms in condensed matter physics. This feature provides an excellent experimental model in statistical mechanics for fundamental studies of microstructural evolution and phase transformation at the individual particle level. However, using colloids to probe three-dimensional phase transitions on Earth remains a challenge as they can be influenced by the gravity force causing the particles to sediment and the solvent to flow. To suppress the undesirable gravity effects, experiments on concentrated colloids were carried out in the International Space Station (ISS) Light Microscopy Module. We will present results of these experiments.

Colloids↗

DOE OSTI2023

Through thick and thin: how optical cavities control spin

When light interacts with matter by means of scattering and absorption, we observe the resulting color. Light also probes the symmetry of matter and the result is encoded in its polarization. In the special case of circularly-polarized light, which is especially relevant in nonlinear optics, quantum photonics, and physical chemistry, a critical dimension of symmetry is along the longitudinal direction. We examine recent advances in controlling circularly-polarized light and reveal that the commonality in these advances is in judicious control of longitudinal symmetry. In particular, in the use of high quality-factor modes in dielectric metasurfaces, the finite thickness can be used to tune the modal profile. These symmetry considerations can be applied in multiplexed optical communication schemes, deterministic control of quantum emitters, and sensitive detection of the asymmetry of small molecules.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Resistivity and thickness effects in dendritic web silicon solar cells

The decrease of minority carrier lifetime as resistivity decreases in dendritic-web silicon solar cells is addressed. This variation is shown to be consistent with the presence of defect levels in the bandgap which arise from extended defects in the web material. The extended defects are oxide precipitates (SiOx) and the dislocation cores they decorate. Sensitivity to this background distribution of defect levels increases with doping because the Fermi level moves closer to the majority carrier band edge. For high-resistivity dendritic-web silicon, which has a low concentration of these extended defects, cell efficiencies as high as 16.6 percent (4 sq cm, 40 ohm-cm boron-doped base, AM1.5 global, 100 mW/sq cm, 25 C JPL LAPSS1 measurement) and a corresponding electron lifetime of 38 microsec have been obtained. Thickness effects occur in bifacial cell designs and in designs which use light trapping. In some cases, the dislocation/precipitate defect can be passivated through the full thickness of web cells by hydrogen ion implantation.

Meier, D. L.↗

NASA NTRS2009

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Panda, Binayak↗

NASA NTRS2011

Structural Efficiency of Composite Struts for Aerospace Applications

The structural efficiency of carbon-epoxy tapered struts is considered through trade studies, detailed analysis, manufacturing and experimentation. Since some of the lunar lander struts are more highly loaded than struts used in applications such as satellites and telescopes, the primary focus of the effort is on these highly loaded struts. Lunar lander requirements include that the strut has to be tapered on both ends, complicating the design and limiting the manufacturing process. Optimal stacking sequences, geometries, and materials are determined and the sensitivity of the strut weight to each parameter is evaluated. The trade study results indicate that the most efficient carbon-epoxy struts are 30 percent lighter than the most efficient aluminum-lithium struts. Structurally efficient, highly loaded struts were fabricated and loaded in tension and compression to determine if they met the design requirements and to verify the accuracy of the analyses. Experimental evaluation of some of these struts demonstrated that they could meet the greatest Altair loading requirements in both tension and compression. These results could be applied to other vehicles requiring struts with high loading and light weight.

Jegley, Dawn C.↗