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DOE OSTI2023

Tailoring Electrochemical CO 2 Reduction on Copper by Reactive Ionic Liquid and Native Hydrogen Bond Donors

Abstract Electrochemical CO 2 reduction (CO 2 RR) on copper (Cu) shows promise for higher‐value products beyond CO. However, challenges such as the limited CO 2 solubility, high overpotentials, and the competing hydrogen evolution reaction (HER) in aqueous electrolytes hinder the practical realization. We propose a functionalized ionic liquid (IL) which generates ion‐CO 2 adducts and a hydrogen bond donor (HBD) upon CO 2 absorption to modulate CO 2 RR on Cu in a non‐aqueous electrolyte. As revealed by transient voltammetry, electrochemical impedance spectroscopy (EIS), and in situ surface‐enhanced Raman spectroscopy (SERS) complemented with image charge augmented quantum‐mechanical/molecular mechanics (IC‐QM/MM) computations, a unique microenvironment is constructed. In this microenvironment, the catalytic activity is primarily governed by the IL and HBD concentrations; former controlling the double layer thickness and the latter modulating the local proton availability. This translates to ample CO 2 availability, reduced overpotential, and suppressed HER where C 4 products are obtained. This study deepens the understanding of electrolyte effects in CO 2 RR and the role of IL ions towards electrocatalytic microenvironment design.

Coskun, Oguz Kagan↗

DOE OSTI2023

Tailoring Electrochemical CO 2 Reduction on Copper by Reactive Ionic Liquid and Native Hydrogen Bond Donors

Electrochemical CO 2 reduction (CO 2 RR) on copper (Cu) shows promise for higher-value products beyond CO. However, challenges such as the limited CO 2 solubility, high overpotentials, and the competing hydrogen evolution reaction (HER) in aqueous electrolytes hinder the practical realization. We propose a functionalized ionic liquid (IL) which generates ion-CO 2 adducts and a hydrogen bond donor (HBD) upon CO 2 absorption to modulate CO 2 RR on Cu in a non-aqueous electrolyte. As revealed by transient voltammetry, electrochemical impedance spectroscopy (EIS), and in situ surface-enhanced Raman spectroscopy (SERS) complemented with image charge augmented quantum-mechanical/molecular mechanics (IC-QM/MM) computations, a unique microenvironment is constructed. In this microenvironment, the catalytic activity is primarily governed by the IL and HBD concentrations; former controlling the double layer thickness and the latter modulating the local proton availability. This translates to ample CO 2 availability, reduced overpotential, and suppressed HER where C 4 products are obtained. This study deepens the understanding of electrolyte effects in CO 2 RR and the role of IL ions towards electrocatalytic microenvironment design.

25 ENERGY STORAGE↗

DOE OSTI2023

The anisotropic nature of singlet fission in single crystalline organic semiconductors

The escalating global energy predicament implores for a revolutionary resolution—one that converts sunlight into electricity—holding the key to supreme conversion efficiency. This comprehensive review embarks on the exploration of the principle of generating multiple excitons per absorbed photon, a captivating concept that possesses the potential to redefine the fundamental confines of conversion efficiency, albeit its application remains limited in photovoltaic devices. At the nucleus of this phenomenon are two principal processes: multiple exciton generation (MEG) within quantum-confined environments, and singlet fission (SF) inside molecular crystals. The process of SF, characterized by the cleavage of a single photogenerated singlet exciton into two triplet excitons, holds promise to potentially amplify photon-to-electron conversion efficiency twofold, thereby laying the groundwork to challenge the detailed balance limit of solar cell efficiency. Our discourse primarily dissects the complex nature of SF in crystalline organic semiconductors, laying special emphasis on the anisotropic behavior of SF and the diffusion of the subsequent triplet excitons in single-crystalline polyacene organic semiconductors. We initiate this journey of discovery by elucidating the principles of MEG and SF, tracing their historical genesis, and scrutinizing the anisotropy of SF and the impact of quantum decoherence within the purview of functional mode electron transfer theory. We present an overview of prominent techniques deployed in investigating anisotropic SF in organic semiconductors, including femtosecond transient absorption microscopy and imaging as well as stimulated Raman scattering microscopies, and highlight recent breakthroughs linked with the anisotropic dimensions of Davydov splitting, Herzberg–Teller effects, SF, and triplet transport operations in single-crystalline polyacenes. Through this comprehensive analysis, our objective is to interweave the fundamental principles of anisotropic SF and triplet transport with the current frontiers of scientific discovery, providing inspiration and facilitating future ventures to harness the anisotropic attributes of organic semiconductor crystals in the design of pioneering photovoltaic and photonic devices.

Chemistry↗

NASA NTRS1968

Aerospace sensor systems.

Aerospace sensor systems, discussing adaptive multimode sensors and multispectral sensing, electronic recognition of image components, laser radar and Raman scattering technique

Mannella, G. G.↗

NASA NTRS1997

Qualitative Flow Visualization of a 110-N Hydrogen/Oxygen Laboratory Model Thruster

The flow field inside a 110 N gaseous hydrogen/oxygen thruster was investigated using an optically accessible, two-dimensional laboratory test model installed in a high altitude chamber. The injector for this study produced an oxidizer-rich core flow, which was designed to fully mix and react inside a fuel-film sleeve insert before emerging into the main chamber section, where a substantial fuel film cooling layer was added to protect the chamber wall. Techniques used to investigate the flow consisted of spontaneous Raman spectra measurements, visible emission imaging, ultraviolet hydroxyl spectroscopy, and high speed schlieren imaging. Experimental results indicate that the oxygen rich core flow continued to react while emerging from the fuel-film sleeve, suggesting incomplete mixing of the hydrogen in the oxygen rich core flow. Experiments also showed that the fuel film cooling protective layer retained its integrity throughout the straight section of the combustion chamber. In the converging portion of the chamber, however, a turbulent reaction zone near the wall destroyed the integrity of the film layer, a result which implies that a lower contraction angle may improve the fuel film cooling in the converging section and extend the hardware lifetime.

deGroot, Wim A.↗

NASA NTRS2014

Overview of NASA GRCs Green Propellant Infusion Mission Thruster Testing and Plume Diagnostics

The Green Propellant Infusion Mission (GPIM) is sponsored by NASA's Space Technology Mission Directorate (STMD) Technology Demonstration Mission (TDM) office. The goal of GPIM is to advance the technology readiness level of a green propulsion system, specifically, one using the monopropellant, AF-M315E, by demonstrating ground handling, spacecraft processing, and on-orbit operations. One of the risks identified for GPIM is potential contamination of sensitive spacecraft surfaces from the effluents in the plumes of AF-M315E thrusters. NASA Glenn Research Center (GRC) is conducting activities to characterize the effects of AF-M315E plume impingement and deposition. GRC has established individual plume models of the 22-N and 1-N thrusters that will be used on the GPIM spacecraft. The models describe the pressure, temperature, density, Mach number, and species concentration of the AF-M315E thruster exhaust plumes. The models are being used to assess the impingement effects of the AF-M315E thrusters on the GPIM spacecraft. The model simulations will be correlated with plume measurement data from Laboratory and Engineering Model 22-N, AF-M315E thrusters. The thrusters will be tested in a small rocket, altitude facility at NASA GRC. The GRC thruster testing will be conducted at duty cycles representatives of the planned GPIM maneuvers. A suite of laser-based diagnostics, including Raman spectroscopy, Rayleigh spectroscopy, Schlieren imaging, and physical probes will be used to acquire plume measurements of AFM315E thrusters. Plume data will include temperature, velocity, relative density, and species concentration. The plume measurement data will be compared to the corresponding simulations of the plume model. The GRC effort will establish a data set of AF-M315E plume measurements and a plume model that can be used for future AF-M315E applications.

green Propellants↗

NASA NTRS2020

Velocity, Temperature and Density Measurements in Supersonic Jets

Prediction of the flow field properties in supersonic jets using computational fluid dynamics (CFD) codes is challenging when there is a significant temperature difference between the jet core and the ambient air and/or compressibility effects are substantial. A benchmark set of flow field property data were obtained to assess current CFD capabilities and develop better modeling approaches for these turbulent flow fields where accurate calculation of turbulent heat flux is important. Three different convergent-divergent nozzles were investigated with exit Mach numbers of: 1.36, 1.63 and 2.0 at their perfectly expanded conditions. The conditions of the jet were set to obtain a temperature difference of zero between the jet core and the ambient air, and then the temperature difference was progressively increased, at the same jet Mach number. Particle Image Velocimetry (PIV), spontaneous rotational Raman scattering spectroscopy (SRS), Background Oriented Schlieren (BOS) and probe-based measurements were used to acquire high quality, spatially-resolved measurements of the mean and root mean square (rms) velocities as well as the mean and rms gas temperatures and densities in both hot and cold supersonic jet flows. The non-intrusive flow measurements are compared both against probe measurements and against standard Reynolds averaged Navier-Stokes (RANS) predictions of the supersonic jet flow properties.

Rotational Raman Spectroscopy↗

NASA NTRS2021

Melt Infiltration Studies of 2D Tyranno SA3(R) Ceramic Matrix Composite Preforms with CrSi2 Intermetallic Alloy

The present paper reports the results of melt infiltrating 2D Tyranno SA3@ fiber woven preforms with molten CrSi2 between 1768 and 1896 K under a vacuum of 1.3 x 10-4 Pa (10-6 torr). The infiltration times varied between 1800 and 7200 s, which did not have any significant effect on the volume fraction of voids filled with the metal. Optical and scanning electron microscopy, back scattered electron imaging, energy dispersion spectroscopy and Raman spectroscopy were used to characterize the infiltrated preforms. A plot of the volume fraction of open voids infiltrated against the absolute melt infiltration temperature showed a sharp peak at 1773 K with almost complete infiltration of the voids at this temperature. The extent of silicide infiltration of the preforms dropped steeply above 1773 K with increasing melt infiltration temperature irrespective of the amount of infiltration time. Above 1805 K, the volume fraction of voids infiltrated with the melt was nearly 0%. It is demonstrated that CrSi2 did not show evidence of a reaction with the SiC fibers. The possibility that a resisting force due to contact angle hysteresis (CAH) may have influenced the diminishing amount of voids filled with increasing temperature above 1773 K was examined. The resistance force was estimated to be extremely small to be consequential. Another possibility that the CrSi2 may have decomposed into Cr(g) and Si(g) in the vacuum melt infiltration furnace appeared to be more plausible based on thermodynamic analyses. An empirical equation is proposed to calculate the amount of remaining charge left to infiltrate the preforms at the infiltration temperature. It is shown that an initial charge of 10 g would rationalize the present observations. While the decomposition of the CrSi2 appeared to mostly explain the present results, some discrepancies were observed, which were inconsistent with the decomposition model.

CrSi2, chromium silicide, ceramic matrix composite↗

NASA NTRS2018

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation in a Single Injector Cooling Flow

Film cooling is used in a wide variety of engineering applications for protection of surfaces from hot or combusting gases. The design of more efficient thin film cooling geometries/configurations could be facilitated by an ability to accurately model and predict the effectiveness of current designs using computational fluid dynamics (CFD) code predictions. Hence, a benchmark set of flow field property data were obtained for use in assessing current CFD capabilities and for development of better turbulence models. Both Particle Image Velocimetry (PIV) and spontaneous rotational Raman scattering (SRS) spectroscopy were used to acquire high quality, spatially-resolved measurements of the mean velocity, turbulence intensity and also the mean temperature and normalized root mean square (rms) temperatures in a single injector cooling flow arrangement. In addition to flowfield measurements, thermocouple measurements on the plate surface enabled estimates of the film effectiveness. Raman spectra in air were obtained across a matrix of radial and axial locations downstream from a 68.07 mm square nozzle blowing heated air over a range of temperatures and Mach numbers, across a 30.48cm long plate equipped with a single injector cooling hole. In addition, both centerline streamwise 2-component PIV and cross-stream 3-component Stereo PIV data at 15 axial stations were collected in the same flows. The velocity and temperature data were then compared against Wind-US CFD code predictions for the same flow conditions. The results of this and planned follow-on studies will support NASA's development and assessment of turbulence models for heated flows.

Wernet, Mark P.↗

NASA NTRS2018

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation in a Single Injector Cooling Flow

Turbulence Modeling↗

NASA NTRS2020

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation of a Perforated Plate Cooling Flow Part I

Film cooling is used in a wide variety of engineering applications for protection of surfaces from hotor combusting gases. The design of more efficient film cooling geometries/configurations could be facilitated by an ability to accurately model and predict the effectiveness of current designs using computational fluid dynamics (CFD) code predictions. Hence, a benchmark set of flow field property data were obtained to assess current CFD capabilities and develop better modeling approaches for these turbulent flow fields where accurate calculation of turbulent heat flux is important. Both Particle Image Velocimetry (PIV) and spontaneous rotational Raman scattering (SRS) spectroscopy were used to acquire high quality, spatially-resolved measurements of the mean and root mean square (rms) velocities as well as the mean and rms temperatures in a film cooling flow field. In addition to off-body flow field measurements, infrared thermography (IR) and thermocouple measurements on the plate surface enabled estimates of the film effectiveness. Raman spectra in air were obtained across a matrix of axial locations downstream from a 68.07 mm square nozzle blowing heated air over a range of temperatures (up to TR =2.7) and Mach numbers (up to Mach 0.9), across a 30.48 cm long plate equipped with three patches of 45 small (~1 mm) diameter cooling holes arranged in a staggered configuration. In addition, both streamwise 2-component PIV (along the plate centerline) and cross-stream 3-component Stereo PIV data at 14 axial stations were collected in the same flows. Only a subset of the data collected in the test program is included in this Part 1 report. The rest of the data will be published in a future report, Part 2, along with planned CFD predictions of the complex cooling film flow.The entire data set of Raman temperature data, PIV velocity data and IR camera data covering the Set Points 23 and 49 in the test matrix in Table 1 is available in an accompanying DVD (available online from www.sti.nasa.gov) for those interested in further analysis.

Mark P Wernet↗

NASA NTRS2020

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation of a Perforated Plate Cooling Flow: Part I

Film cooling is used in a wide variety of engineering applications for protection of surfaces from hot or combusting gases. The design of more efficient film cooling geometries/configurations could be facilitated by an ability to accurately model and predict the effectiveness of current designs using computational fluid dynamics (CFD) code predictions. Hence, a benchmark set of flow field property data was obtained to assess current CFD capabilities and develop better modeling approaches for these turbulent flow fields where accurate calculation of turbulent heat flux is important. Both Particle Image Velocimetry (PIV) and spontaneous rotational Raman scattering (SRS) spectroscopy were used to acquire high quality, spatially-resolved measurements of the mean and root mean square (rms) velocities as well as the mean and rms temperatures in a film cooling flow field. In addition to off-body flow field measurements, infrared thermography (IR) and thermocouple measurements on the plate surface enabled estimates of the film effectiveness. Raman spectra in air were obtained across a matrix of axial locations downstream from a 68.07 mm square nozzle blowing heated air over a range of temperatures (up to TR = 2.7) and Mach numbers (up to Mach 0.9), across a 30.48 cm long plate equipped with three patches of 45 small (~1 mm) diameter cooling holes arranged in a staggered configuration. In addition, both streamwise 2-component PIV (on the plate centerline) and cross-stream 3-component Stereo PIV data at 14 axial stations were collected in the same flows. Only a subset of the data collected in the test program is included in this Part I report. The rest of the data will be published in a future report, Part II, along with planned CFD predictions of the complex cooling film flow. The entire data set of Raman temperature data, PIV velocity data and IR camera data covering the Set Points 23 and 49 in the test matrix in Table 1 is available in an accompanying DVD (available online from www.sti.nasa.gov) for those interested in further analysis.

Nozzle↗

NASA NTRS2019

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation of a Perforated Plate Cooling Flow: Part I

Film cooling is used in a wide variety of engineering applications for protection of surfaces from hot or combusting gases. The design of more efficient film cooling geometries/configurations could be facilitated by an ability to accurately model and predict the effectiveness of current designs using computational fluid dynamics (CFD) code predictions. Hence, a benchmark set of flow field property data were obtained for use in assessing current CFD capabilities and for development of better modeling approaches for these turbulent flow fields where accurate calculation of turbulent heat flux is important. Both Particle Image Velocimetry (PIV) and spontaneous rotational Raman scattering (SRS) spectroscopy were used to acquire high quality, spatially-resolved measurements of the mean velocity, turbulence intensity as well as the mean temperature and root mean square (rms) temperatures in a film cooling flow field. In addition to off-body flow field measurements, infrared thermography (IR) and thermocouple measurements on the plate surface enabled estimates of the film effectiveness. Raman spectra in air were obtained across a matrix of axial locations downstream from a 68.07 mm square nozzle blowing heated air over a range of temperatures (up to TR = 2.7) and Mach numbers (up to M0.9), across a 30.48 cm long plate equipped with three patches of 45 small (~1 mm) diameter cooling holes arranged in a staggered configuration. In addition, both centerline streamwise 2-component PIV and cross-stream 3-component Stereo PIV data at 14 axial stations were collected in the same flows. Only a subset of the data collected in the test program is included in this Part I report and are available from the NASA STI office. The final portion of the data will be published in a future report, Part II, along with CFD predictions of the complex cooling film flow.

IR camera Measurments↗

NASA NTRS2019

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation of a Perforated Plate Cooling Flow: Part 1

Film cooling is used in a wide variety of engineering applications for protection of surfaces from hot or combusting gases. The design of more efficient film cooling geometries/configurations could be facilitated by an ability to accurately model and predict the effectiveness of current designs using computational fluid dynamics (CFD) code predictions. Hence, a benchmark set of flow field property data were obtained for use in assessing current CFD capabilities and for development of better modeling approaches for these turbulent flow fields where accurate calculation of turbulent heat flux is important. Both Particle Image Velocimetry (PIV) and spontaneous rotational Raman scattering (SRS) spectroscopy were used to acquire high quality, spatially-resolved measurements of the mean velocity, turbulence intensity as well as the mean temperature and root mean square (rms) temperatures in a film cooling flow field. In addition to off-body flow field measurements, infrared thermography (IR) and thermocouple measurements on the plate surface enabled estimates of the film effectiveness. Raman spectra in air were obtained across a matrix of axial locations downstream from a 68.07 mm square nozzle blowing heated air over a range of temperatures (up to TR = 2.7) and Mach numbers (up to M0.9), across a 30.48 cm long plate equipped with three patches of 45 small (~1 mm) diameter cooling holes arranged in a staggered configuration. In addition, both centerline streamwise 2-component PIV and cross-stream 3-component Stereo PIV data at 14 axial stations were collected in the same flows. Only a subset of the data collected in the test program is included in this Part I report and are available from the NASA STI office. The final portion of the data will be published in a future report, Part II, along with CFD predictions of the complex cooling film flow.

Raman Scattering↗

DOE OSTI2023

Spatially resolved multimodal vibrational spectroscopy under high pressures

In this perspective, we discuss the potential impact on in situ studies under controlled environments of a novel multimodal spectroscopic technique, optical photothermal infrared + Raman spectroscopy, which enables the simultaneous collection of infrared and Raman scattering spectra, along with hyperspectral imaging and chemical imaging with wavelength-independent sub-500 nm spatial resolution. A brief review of the current literature regarding the O-PTIR technique is presented along with recent work from our own lab on determining the crystallinity of soft and inorganic materials. The results highlight the possibility of resolving differences in the crystallinity of soft materials associated with changes in material processing. Here, we also demonstrate the first reported use of a diamond anvil cell with simultaneous infrared and Raman measurements that showcases, using a high energy material as an example, the potential use of O-PTIR spectroscopy in diamond anvil cell techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Integration of Highly Luminescent Lead Halide Perovskite Nanocrystals on Transparent Lead Halide Nanowire Waveguides through Morphological Transformation and Spontaneous Growth in Water

The integration of highly luminescent CsPbBr 3 quantum dots on nanowire waveguides has enormous potential applications in nanophotonics, optical sensing and quantum communications. On the other hand, CsPb 2 Br 5 nanowires have also attracted a lot of attention due to their unique water stability and controversial luminescent property. Here we first report the growth of CsPbBr 3 nanocrystals on CsPb 2 Br 5 nanowires by simply immersing CsPbBr 3 powder into pure water, CsPbBr 3-γ X γ (X = Cl, I) nanocrystals on CsPb 2 Br 5-γ X γ nanowires are then synthesized for tunable light sources. Systematic structure and morphology studies, including in-situ monitoring, revealed that CsPbBr 3 powder was first converted to CsPb 2 Br 5 microplatelets in water, followed by a morphological transformation from CsPb 2 Br 5 microplatelets to nanowires, which is a kinetic dissolution-recrystallization process controlled by electrolytic dissociation and supersaturation of CsPb 2 Br 5 . CsPbB r3 nanocrystals are spontaneously formed on CsPb 2 Br 5 nanowires when nanowires are collected from the aqueous solution. Raman spectroscopy, combined photoluminescence and SEM imaging confirm that the bright emission originates from CsPbBr 3-γ X γ nanocrystals while CsPb 2 Br 5-γ X γ nanowires are transparent waveguides. In conclusion, the intimate integration of nanoscale light sources with a nanowire waveguide is demonstrated through the observation of the wave guiding of light from nanocrystals and Fabry-Perot interference modes of the nanowire cavity.

42 ENGINEERING↗

DOE OSTI2021

Heat-treated glassy carbon under pressure exhibiting superior hardness, strength and elasticity

Glassy carbon (GC) is a type of non-graphitizing disordered carbon material at ambient pressure and high temperatures, which has been widely used due to its excellent mechanical properties. Here we report the changes in the microstructure and mechanical properties of GC treated at high pressures (up to 5 GPa) and high temperatures. The formation of intermediate sp 2 –sp 3 phases is identified at moderate treatment temperatures before the complete graphitization of GC, by analyzing synchrotron X-ray diffraction, Raman spectra, and transmission electron microscopy images. The intermediate metastable carbon materials exhibit superior mechanical properties with hardness reaching up to 10 GPa and compressive strength reaching as high as 2.5 GPa, nearly doubling those of raw GC, and improving elasticity and thermal stability. The synthesis pressure used in this study can be achieved in the industry on a commercial scale, enabling the scalable synthesis of this type of strong, hard, and elastic carbon materials.

36 MATERIALS SCIENCE↗

DOE OSTI2020

The Prevalence of Anions at Plasmonic Nanojunctions: A Closer Look at P-Nitrothiophenol

We revisit the reductive coupling of p-nitrothiophenol (NTP) to form dimercaptoazobenzene (DMAB), herein monitored through gap-mode tip-enhanced Raman spectroscopy (TERS) and nano-imaging. We employ a plasmonic Au probe (100 nm diameter at its apex) illuminated with a 633 nm laser source (50 ?W/?m2 at the sample position) to image a NTP-coated faceted silver nanoparticle (~70 nm diameter). A detailed analysis of the recorded spectra reveals that anionic NTP species contribute to the recorded spectral images, in addition to the more thoroughly described DMAB product. Notably, the signatures of the anions are more pronounced than those of the DMAB product under our present experimental conditions. Our results thus demonstrate that anions and their spectral signatures must be considered in the analysis of plasmon-enhanced spectra and images.

Wang, Chih-Feng↗