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NASA NTRSDate not supplied

Analysis of Cryogenic Propellant Liquefaction Rates in Cooled Constant-Wall-Temperature Tanks

NASA has been focused on developing technology that would allow the production of cryogenic propellants on the Lunar and Martian surfaces. Utilizing Lunar/Martian resources, the produced gaseous propellants must first be liquefied and stored prior to use on the Moon or Mars ascent vehicle. Liquefaction of cryogenic propellant is a necessary technical development to enable NASA’s future spaceflight goals. This paper presents an overview of the effect of spacecraft propellant system parameters on cryogenic propellant liquefaction rates. The propellant system was assumed to be a receiver of a gas from an In-Situ Resource Utilization (ISRU) harvester and condensed the gas by cooling the tank walls. First, the general thermodynamic principles pertinent to condensation are summarized, followed by an overview of the model which performed the analysis, including a summary of the Fortran implementation. Comparisons between the model results and test data are discussed, as well as sensitivity of the condensation rate to various parameters.

Anson Koch↗

NASA NTRSDate not supplied

Analysis of Cryogenic Propellant Liquefaction Rates in Cooled Constant-Wall-Temperature Tanks

cryogenics↗

DOE OSTI2021

The controlling role of atmosphere in dawsonite versus gibbsite precipitation from tetrahedral aluminate species

In highly alkaline solution, aluminum speciates as the tetrahedrally coordinated aluminate monomer, Al(OH)4- and/or dimer Al2O(OH)62-, yet precipitates as octahedrally coordinated gibbsite (Al(OH)3). This tetrahedral to octahedral transformation governs Al precipitation, which is crucial to worldwide Al production, and to the processing of caustic high-level radioactive wastes. Despite its significance, the transformation pathway remains unknown. Here we explore the roles of atmospheric water and carbon dioxide in mediating the transformation of the tetrahedrally coordinated potassium aluminate dimer salt (K2Al2O(OH)6) to gibbsite versus potassium dawsonite (KAl(CO3)(OH)2). A combination of in-situ attenuated total reflection infrared spectroscopy, ex-situ micro X-ray diffraction, and multivariate curve resolution-alternating least squares chemometrics analysis reveals that humidity plays a key role in the transformation by limiting the amount of alkalinity neutralization by dissolved CO2. Lower humidity favors higher alkalinity and incorporation of carbonate species in the final Al product to form KAl(CO3)(OH)2. Higher humidity enables more acid generation that destabilizes dawsonite and favors gibbsite as the solubility limiting phase. Because the transformation was restricted to occur in thin water films, the results suggest that transition from tetra- to octahedrally coordinated Al does not have to occur in bulk solution, as has often been hypothesized, but may instead appear on the source mineral surface.

Dembowski, Mateusz↗

DOE OSTI2020

In situ high-temperature X-ray diffraction study of Sc-doped titanium oxide nanocrystallites

Titanium dioxide is an inexpensive wide-gap highly ionic semiconductor with striking photocatalytic capabilities in several heterogeneous photoredox reactions. A small crystal size is desirable to maximize the surface area, since photocatalytic reactions occur at the surface of a photocatalyst. Presented in this work are the synthesis and microstructural characterization of 4 at.% Sc-doped TiO 2 (4SDT) prepared by water-based co-precipitation. The crystal structure of 4SDT was examined via in situ high-temperature powder X-ray diffraction experiments from 25 to 1200°C. Rietveld analysis revealed single-phase anatase up to 875°C, while at 900°C the anatase-to-rutile phase transformation occurred and at higher temperatures additional reflections of Sc-rich phases (Sc 2 TiO 5 from 975°C and Ti 3 Sc 4 O 12 or Sc 2 O 3 at 1200°C) were observed. Debye function analysis (DFA) was applied to model the total scattering pattern directly in reciprocal space, allowing the reconstruction of Ti vacancies. Both Rietveld and DFA methods were applied to estimate the nanocrystallite size and shape with consistent growth in crystallite size with temperature: an ellipsoid shape with equatorial ~4.7 nm / axial (001) ~6.9 nm at 25°C to equatorial ~27.9 nm / axial (001) ~39.6 nm at 900°C refined by Rietveld analysis, versus a cylinder shape with D a , b = 4.3 nm and size dispersion σ ab = 1.5 nm, L c = 4.9 nm and σ c = 2.3 nm at 25°C to D a , b = 21.4 nm, σ ab = 8.3 nm, L c = 23.9 and σ c = 10.9 nm at 900°C estimated by DFA. The microstructural changes obtained by Rietveld and DFA methods were supported by high-resolution transmission electron microscopy image analysis, as well as by the less direct nitrogen sorption techniques that provide information on the size of non-agglomerated and dense particles. The Ti site-occupancy factor showed a linear increase from 0.6–0.8 at 25°C to unity at 900°C for anatase, and from ~0.7 at 900°C to unity at 1200°C for rutile, via Rietveld analysis and DFA.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Rain on snow (ROS) understudied in sea ice remote sensing: a multi-sensor analysis of ROS during MOSAiC (Multidisciplinary drifting Observatory for the Study of Arctic Climate)

Abstract. Arctic rain on snow (ROS) deposits liquid water onto existing snowpacks. Upon refreezing, this can form icy crusts at the surface or within the snowpack. By altering radar backscatter and microwave emissivity, ROS over sea ice can influence the accuracy of sea ice variables retrieved from satellite radar altimetry, scatterometers, and passive microwave radiometers. During the Arctic Ocean MOSAiC (Multidisciplinary drifting Observatory for the Study of Arctic Climate) expedition, there was an unprecedented opportunity to observe a ROS event using in situ active and passive microwave instruments similar to those deployed on satellite platforms. During liquid water accumulation in the snowpack from rain and increased melt, there was a 4-fold decrease in radar energy returned at Ku- and Ka-bands. After the snowpack refroze and ice layers formed, this decrease was followed by a 6-fold increase in returned energy. Besides altering the radar backscatter, analysis of the returned waveforms shows the waveform shape changed in response to rain and refreezing. Microwave emissivity at 19 and 89 GHz increased with increasing liquid water content and decreased as the snowpack refroze, yet subsequent ice layers altered the polarization difference. Corresponding analysis of the CryoSat-2 waveform shape and backscatter as well as AMSR2 brightness temperatures further shows that the rain and refreeze were significant enough to impact satellite returns. Our analysis provides the first detailed in situ analysis of the impacts of ROS and subsequent refreezing on both active and passive microwave observations, providing important baseline knowledge for detecting ROS over sea ice and assessing their impacts on satellite-derived sea ice variables.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2015

Surface characterization studies on the interaction of V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst for low temperature SCR of NO with NH{sub 3}

This study aimed at elucidating the surface characterization of V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst to investigate the interaction of V, W and Ti species for the improvement of the catalytic activity in the SCR reaction at low-temperature. Analysis by XRD, UV–vis, PL spectra and DFT theoretical calculations, XPS, EPR and in situ DRIFT showed that WO{sub 3} could interact with TiO{sub 2} to improve the electrons transfer, and the WO{sub 3} hybridization with V{sub 2}O{sub 5} could also improve the reducibility and formation of reduced V{sub 2}O{sub 5} species for the V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst. These aspects resulted in the NO oxidation and NO{sub 3}{sup −} decomposition that were responsible for the high catalytic activity of V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst. - Graphical abstract: Interaction of V, W and Ti species improved the formation of reduced V{sub 2}O{sub 5} and O{sub 2}{sup −}, NO oxidation and NO{sub 3}{sup −} decomposition to enhance the catalytic activity of VWTi catalyst. - Highlights: • Interaction of V, W and Ti species improved the SCR reaction at low-temperature. • Hybridization between WO{sub 3} and V{sub 2}O{sub 5} improved the reducibility and reduced V{sub 2}O{sub 5} species formation of V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst. • The interaction improved the NO oxidation and NO{sub 3}{sup −} decomposition over V{sub 2}O{sub 5}–WO{sub 3}/TiO{sub 2} catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Influence of Structural Defects on Biomineralized ZnS Nanoparticle Dissolution: An In-Situ Electron Microscopy Study

The dissolution of metal sulfides, such as ZnS, plays an important role in the fate of metal contaminants in the environment. Here we have examined the dissolution behavior of ZnS nanoparticles synthesized via several abiotic and biological pathways. Specifically, the biogenic ZnS nanoparticles were produced by an anaerobic, metal-reducing bacterium Thermoanaerobacter sp. X513 in a Zn-amended, thiosulfate-containing growth medium, whereas the abiogenic ZnS nanoparticles were produced by mixing an aqueous Zn solution with either H 2 S-rich gas or Na 2 S solution. For biogenic synthesis, we prepared two types of samples, in the presence or absence of trace silver (Ag). The size distribution, crystal structure, aggregation behavior, and internal defects of the synthesized ZnS nanoparticles were primarily examined using high-resolution transmission electron microscopy coupled with X-ray energy dispersive spectroscopy. The characterization results show that both the biogenic and abiogenic samples were dominantly composed of sphalerite. In the absence of Ag, the biogenic ZnS nanoparticles were significantly larger (i.e., ~10 nm) than the abiogenic ones (i.e., ~3–5 nm) and contained structural defects (e.g., twins and stacking faults). The presence of trace Ag showed a restraining effect on the particle size of the biogenic ZnS, resulting in quantum-dot-sized nanoparticles (i.e., ~3 nm). In situ dissolution experiments for the synthesized ZnS were conducted with a liquid-cell coupled to a transmission electron microscope (LCTEM), and the primary factors (i.e., the presence or absence structural defects) were evaluated for their effects on the dissolution behavior using the biogenic and abiogenic ZnS nanoparticle samples with the largest average particle size. Analysis of the dissolution results (i.e., change in particle radius with time) using the Kelvin equation shows that the defect-bearing biogenic ZnS nanoparticles (γ = 0.799 J/m 2 ) have a significantly higher surface energy than the abiogenic ZnS nanoparticles (γ = 0.277 J/m 2 ), suggesting that larger defect-bearing ZnS nanoparticles may be more reactive than the smaller quantum-dot-sized ZnS nanoparticles. These findings provide new insight into the factors that govern the dissolution of metal sulfide nanoparticles in relevant natural and engineered scenarios, and have implication for tracking the fate of zinc at contaminated sites. Moreover, our study exemplified the use of an in situ method (i.e., LCTEM) to investigate nanoparticle behavior (e.g., dissolution) in aqueous solutions.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2015

Direct Evidence of a Chemical Conversion Mechanism of Atomic-Layer-Deposited TiO 2 Anodes During Lithiation Using LiPF 6 Salt

Titanium dioxide has been identified as a prospective anode material for use in lithium ion batteries. The higher lithiation potential of TiO 2 versus other common anodes is more electrochemically compatible with most organic electrolytes, thus leading to reduced solid electrolyte interphase formation and overall more stable battery systems. However, in this study TiO 2 has exhibited poor cycling stability with common electrolytes containing lithium hexafluorophosphate (LiPF 6 ) salt. Combined electrochemical and spectroscopic analyses have revealed this to be due to the onset of reversible fluorination of the anode and chemical conversion of TiO 2 to TiOF 2 during lithiation. Comparison of electrochemical cycling of atomic-layer-deposited TiO2 anodes using LiPF6 with and without a hydrofluoric acid scavenger, tributylamine, to cycling using a nonfluorinated lithium perchlorate (LiClO 4 ) salt indicates that the in situ formation of hydrofluoric acid in the electrolyte from decomposition of the PF$_{6^–}$ anion alters the lithiation electrochemistry. X-ray photoelectron spectroscopy (XPS) analysis and time-of-flight secondary-ion mass spectrometry (ToF SIMS) depth profiling measurements confirmed the presence of TiF 2 and TiOF surface and bulk phases, respectively, in the electrode upon lithiation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Microfluidic electrochemical cell for in situ structural characterization of amorphous thin-film catalysts using high-energy X-ray scattering

Porous, high-surface-area electrode architectures are described that allow structural characterization of interfacial amorphous thin films with high spatial resolution under device-relevant functional electrochemical conditions using high-energy X-ray (>50 keV) scattering and pair distribution function (PDF) analysis. Porous electrodes were fabricated from glass-capillary array membranes coated with conformal transparent conductive oxide layers, consisting of either a 40 nm–50 nm crystalline indium tin oxide or a 100 nm–150 nm-thick amorphous indium zinc oxide deposited by atomic layer deposition. These porous electrodes solve the problem of insufficient interaction volumes for catalyst thin films in two-dimensional working electrode designs and provide sufficiently low scattering backgrounds to enable high-resolution signal collection from interfacial thin-film catalysts. For example, PDF measurements were readily obtained with 0.2 Å spatial resolution for amorphous cobalt oxide films with thicknesses down to 60 nm when deposited on a porous electrode with 40 µm-diameter pores. This level of resolution resolves the cobaltate domain size and structure, the presence of defect sites assigned to the domain edges, and the changes in fine structure upon redox state change that are relevant to quantitative structure–function modeling. The results suggest the opportunity to leverage the porous, electrode architectures for PDF analysis of nanometre-scale surface-supported molecular catalysts. In addition, a compact 3D-printed electrochemical cell in a three-electrode configuration is described which is designed to allow for simultaneous X-ray transmission and electrolyte flow through the porous working electrode.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Final Scientific/Technical Report, Multi-Sensor Inspection and Robotic Systems for Dry Storage Casks

Once removed from service, fuel rod assemblies are cooled in a pool and then placed in dry storage until they can be transported to a repository for disposal. The extended duration that used nuclear fuel spends in dry storage makes it prudent to be able to nondestructively inspect the dry storage casks. The degradation mechanisms of most concern are chloride-induced stress corrosion cracking of the stainless steel canister that confines the spent fuel and distributed cracking of the concrete in the overpack structure. Multi-sensor inspection and robotic systems were researched, developed, built, and tested. One system operates completely outside the cask to inspect the concrete. The other system, known as the PRINSE system, for Proactive Robotic Inspection of Nuclear Storage Enclosures, enters the cask through an outlet vent and navigates around the outer surface of the stainless steel canister. The PRINSE system delivers sensors for: (i) real-time characterization of the canister surface in order to assess whether chlorides are present, (ii) detecting the presence of cracks using shear-horizontal ultrasonic guided waves, (iii) measuring the temperature of the canister surface, and (iv) a gamma radiation counter. The four sensing modalities are applicable to any cask containing a stainless steel canister, however the robotic delivery system is designed specifically for Holtec’s HI-STORM family of casks. Horizontal axis casks have exposed concrete surfaces. A fully contactless air-coupled scanning ultrasonic test platform and a frequency-wavenumber domain data analysis method are used for these concrete structures. Analysis, numerical simulation and experimental results demonstrate that distributed cracks in concrete can be detected and cracked regions localized within a scanned region of concrete. Vertical axis casks (like the HI-STORM family) have steel-clad concrete overpacks. In a separate effort, a semi-coupled test platform and a guided wave attenuation-based data analysis method are used for disbond detection. Analysis, numerical simulation and experimental results show that the bonding conditions of steel-concrete interfaces can be quantitatively characterized using the guided wave signal analysis scheme. The PRINSE system is designed for vertical axis dry storage casks, specifically the HI-STORM family. The double pulse laser-induced breakdown spectroscopy (LIBS) system takes advantage of an optical fiber to deliver intense light to the canister surface that enables surface composition characterization in-situ in real time. Chlorine concentrations as low as 10 mg/m2 were detected on stainless steel. Additionally, a simpler laser setup was created to detect sodium as a surrogate for chlorine, and sodium was detectable when the chlorine concentration was as low as 0.5 mg/m2. The electromagnetic acoustic transducers (EMATs) enable detection of stress corrosion cracks. The EMATs generate shear-horizontal waves that propagate around the canister and are reflected by cracks enabling 100% of the canister weld lines to be inspected. The EMAT-based crack detection system was tested at the Pacific Northwest National Laboratory on a canister containing blind defects and was shown to detect the crack sizes it was designed to detect. The PRINSE system is a novel marsupial robot. The command center and winch outside the cask control the delivery arm and train of cars that traverse the outside of the canister from the cask ventilation system. The sensors are housed in the cargo bays of three cars that comprise the train, which is lowered to the bottom of the canister by the winch. Encoders on the winch enable the sensors to be delivered to a prescribed location, e.g., for re-inspection of a problem area. The PRINSE system does not mar the canister surface, can be extracted manually in the case of a power failure, and is designed for an elevated temperature and gamma radiation environment, although not all components of the prototype are made from the final materials. The PRINSE system was tested on a full canister that was placed inside a HI-STORM cask at the Holtec Manufacturing Division. It was also demonstrated on a full-height mockup at Penn State to a live audience.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1981

Volcanism on Mars

In situ chemical analyses of Martian soil by the Viking lander indicate mafic to ultramafic source rocks, consistent with both remote sensing data indicating the presence of pyroxene and olivine and with petrologic modeling which suggests that Martian lavas are iron-rich and ultramafic. Photogeological analysis of the Martian surface reveals two types of volcanic morphology: (1) central volcanoes, developed by continued and prolonged eruption from a point source vent; and (2) volcanic plains, recognized by mare ridges and flow lobes. When these volcanic morphologies are combined with relative age data, a volcanic history may be derived that is consistent with a moonlike thermal history involving a lithosphere of increasing thickness with time which gradually suppresses the volcanism.

Greely, R.↗

NASA NTRS1986

Emission FTIR analyses of thin microscopic patches of jet fuel residues deposited on heated metal surfaces

The relationship of fuel stability to fuel composition and the development of mechanisms for deposit formation were investigated. Fuel deposits reduce heat transfer efficiency and increase resistance to fuel flow and are highly detrimental to aircraft performance. Infrared emission Fourier transform spectroscopy was chosen as the primary method of analysis because it was sensitive enough to be used in-situ on tiny patches of monolayers or of only a few molecular layers of deposits which generally proved completely insoluble in any nondestructive solvents. Deposits of four base fuels were compared; dodecane, a dodecane/tetralin blend, commercial Jet A fuel, and a broadened-properties jet fuel particularly rich in polynuclear aromatics. Every fuel in turn was provided with and without small additions of such additives as thiophene, furan, pyrrole, and copper and iron naphthenates.

Lauer, J. L.↗

NASA NTRS2000

Investigation of Mesoscale Variability in Convective Boundary Layer Development Using LASE

Throughout this research effort we have analyzed data collected from the Southern Great Plains 1997 (SGP) experiment to evaluate terms in the budget of water vapor in the atmospheric boundary layer (ABL). The analysis is centered on using data obtained from the Lidar Atmospheric Sensing Experiment (LASE) downward-looking differential absorption lidar (DIAL) that was flown on the NASA-P3 aircraft. The DIAL is able to measure vertical profiles of water vapor, as well as aerosol backscatter, throughout the ABL. Initial work on using the DIAL is summarized in the attached meeting preprint, which discusses results from a segment of the 12 July 1997 flight. Additional analysis has been carried out using both the DIAL data and in situ measurements to obtain more complete and detailed estimates of terms in the ABL water vapor budget. This includes data from the Canadian National Research Council Twin Otter aircraft, as well as from a spectrum of surface-based instruments. This work is expected to lead to a refereed article planned for submission to the Journal.

Lenschow, Donald H.↗

NASA NTRS2014

Climate Forcing Datasets for Agricultural Modeling: Merged Products for Gap-Filling and Historical Climate Series Estimation

The AgMERRA and AgCFSR climate forcing datasets provide daily, high-resolution, continuous, meteorological series over the 1980-2010 period designed for applications examining the agricultural impacts of climate variability and climate change. These datasets combine daily resolution data from retrospective analyses (the Modern-Era Retrospective Analysis for Research and Applications, MERRA, and the Climate Forecast System Reanalysis, CFSR) with in situ and remotely-sensed observational datasets for temperature, precipitation, and solar radiation, leading to substantial reductions in bias in comparison to a network of 2324 agricultural-region stations from the Hadley Integrated Surface Dataset (HadISD). Results compare favorably against the original reanalyses as well as the leading climate forcing datasets (Princeton, WFD, WFD-EI, and GRASP), and AgMERRA distinguishes itself with substantially improved representation of daily precipitation distributions and extreme events owing to its use of the MERRA-Land dataset. These datasets also peg relative humidity to the maximum temperature time of day, allowing for more accurate representation of the diurnal cycle of near-surface moisture in agricultural models. AgMERRA and AgCFSR enable a number of ongoing investigations in the Agricultural Model Intercomparison and Improvement Project (AgMIP) and related research networks, and may be used to fill gaps in historical observations as well as a basis for the generation of future climate scenarios.

Climate Forcing Data↗

NASA NTRS2016

Snow Process Estimation Over the Extratropical Andes Using a Data Assimilation Framework Integrating MERRA Data and Landsat Imagery

A data assimilation framework was implemented with the objective of obtaining high resolution retrospective snow water equivalent (SWE) estimates over several Andean study basins. The framework integrates Landsat fractional snow covered area (fSCA) images, a land surface and snow depletion model, and the Modern Era Retrospective Analysis for Research and Applications (MERRA) reanalysis as a forcing data set. The outputs are SWE and fSCA fields (1985-2015) at a resolution of 90 m that are consistent with the observed depletion record. Verification using in-situ snow surveys showed significant improvements in the accuracy of the SWE estimates relative to forward model estimates, with increases in correlation (0.49-0.87) and reductions in root mean square error (0.316 m to 0.129 m) and mean error (-0.221 m to 0.009 m). A sensitivity analysis showed that the framework is robust to variations in physiography, fSCA data availability and a priori precipitation biases. Results from the application to the headwater basin of the Aconcagua River showed how the forward model versus the fSCA-conditioned estimate resulted in different quantifications of the relationship between runoff and SWE, and different correlation patterns between pixel-wise SWE and ENSO. The illustrative results confirm the influence that ENSO has on snow accumulation for Andean basins draining into the Pacific, with ENSO explaining approximately 25% of the variability in near-peak (1 September) SWE values. Our results show how the assimilation of fSCA data results in a significant improvement upon MERRA-forced modeled SWE estimates, further increasing the utility of the MERRA data for high-resolution snow modeling applications.

SWE↗

NASA NTRSDate not supplied

Future Orbiting and In-Situ Exploration of Venus: Mount Etna as Terrestrial Analog

The exploration of Venus will soon experience a new golden era thanks to the recently selected NASA Deep Atmosphere of Venus Investigation of Noble gases, Chemistry and Imaging (DAVINCI) mission, NASA Venus Emissivity, Radio Science, InSAR, Topography & Spectroscopy (VERITAS) mission, and ESA EnVision mission. The DAVINCI mission will focus on the analysis of the the atmospheric vertical structure and composition of Earth’s twin planet and on the geologic structure of a tesserae terrain. The VERITAS mission will investigate the geologic features of its surface as well as geodynamic characteristics of the subsurface, providing high-resolution emissivity data, a global radar map at an approximate resolution of 30 meters/pixel, and estimation of the gravity anomaly of the shallow crust of the planet. The ESA EnVision mission will be complementary to the two NASA missions, providing high resolution 0.8-2.5 micron emissivity data, Synthetic Aperture Radar (SAR) data, and Subsurface Radar Sounder (SRS) data. Beyond those, the proposed Roscosmos-NASA Venera-D mission will also be equipped with an orbiter that will investigate the atmospheric composition and circulation, as well as a lander that will analize the in-situ chemical composition and the surface-atmosphere interactions.

P. D’Incecco↗

DOE OSTI2017

Understanding the nanoscale redox-behavior of iron-anodes for rechargeable iron-air batteries

Iron-air cells provide a promising and resource-efficient alternative battery concept with superior area specific power density characteristics compared to state-of-the-art Li-air batteries and potentially superior energy density characteristics compared to present Li-ion batteries. Understanding charge-transfer reactions at the anode-electrolyte interface is the key to develop high-performance cells. By employing in-situ electrochemical atomic force microscopy (in-situ EC-AFM), in-depth insight into the electrochemically induced surface reaction processes on iron in concentrated alkaline electrolyte is obtained. The results highlight the formation and growth of the redox-layer on iron over the course of several oxidation/reduction cycles. By this means, a direct correlation between topography changes and the corresponding electrochemical reactions at the nanoscale could unambiguously be established. Here in this paper, the twofold character of the nanoparticulate redox-layer in terms of its passivating character and its contribution to the electrochemical reactions is elucidated. Furthermore, the evolution of single nanoparticles on the iron electrode surface is evaluated in unprecedented and artifact-free detail. Based on the dedicated topography analysis, a detailed structural model for the evolution of the redox-layer which is likewise elementary for corrosion science and battery research is derived.

25 ENERGY STORAGE↗

DOE OSTI2024

In-situ hydrogen microstructural characterization of Si heterojunction passivation: Addressing V OC degradation and mitigation pathways

Si heterojunction (SHJ) solar cells have demonstrated record efficiency >27%, approaching the theoretical limit of ≈ 29%, primarily due to best surface/interface defect passivation provided by deposited thin layers of hydrogenated amorphous silicon (a-Si:H). Such excellent surface/interface passivation reduces recombination loss and result in >100 mV improvement of cell open circuit voltage (V OC ) to ≈ 750 mV, thus the cell efficiency. However, fielded SHJ modules exhibit loss of V OC and hence efficiency over time in years, presumably due to degradation related to a-Si:H layers. This adversely affects the technology’s market acceptance, and levelized cost of energy (LCOE). It is hypothesized that the origin of a-Si:H degradation is somehow related to the presence of weak Si–Si bonds and hydrogen in a-Si:H films. The objective of this project is to test this hypothesis by directly measuring chemical and structural changes occurring within SHJ component layers and solar cells. This is achieved by developing an innovative in-situ Fourier transform infrared (FTIR) spectrometry apparatus to monitor hydrogen microstructural changes occurring within amorphous silicon and decipher hydrogen evolution kinetics over time when samples are exposed to heat and/or light stress. These in-situ measured hydrogen microstructural changes are correlated to the changes in effective minority carrier lifetime (τ eff ), implied V OC (iV OC ), surface recombination velocity (S), and cell V OC . These mechanistic understandings will provide critical guidance to mitigate the V OC -driven degradation of SHJ solar cell performance. Passivation optimization and degradation analysis of individual SHJ component structures were achieved through systematic deposition of three symmetric structures and the completed SHJ solar cell structure. The three symmetric structures used were intrinsic a-Si:H [(i)a-Si:H] layers in a bilayer structure, intrinsic and p-type doped stacked layers [(i-p)a-Si:H] representing the front heterojunction in the SHJ cell, and intrinsic and n-typed doped stacked layers [(i-n)a-Si:H] representing the back-side back surface field (BSF) in the SHJ cell. State-of-the-art passivation qualities are demonstrated by a champion iV OC of 740 mV for the (i)a-Si:H layers, and the (i-n)a-Si:H symmetric structure. A 725 mV iV OC is observed for the (i-p)a-Si:H symmetric structure. These symmetric passivated SHJ component structures were subsequently subjected to different accelerated lifetime (ALT) stressors to identify which conditions contribute the most to iV OC degradation. Degradation of the thin (10 nm) (i)a-Si:H passivation layers without any additional overlying layers is minimal; complexity of this study arises due to unavoidable surface oxidation of (i)a-Si:H layer during most of the stress application, which is likely irrelevant for a full SHJ cell configuration with overlying protective layers. The iV OC degradation of symmetric structures is found to occur primarily at the (i-p)a-Si:H passivation stack under dark heat stress with associated hydrogen loss from the (p)a-Si:H layer. An activation energy for increase in S (defect creation) of 0.65 eV can be correlated to the activation energy of ≈ 0.4 eV for hydrogen loss from the (i-p)a-Si:H stack. This also suggests the presence of weakly bonded hydrogen in the (p)a-Si:H films, which effuses out of the film stack at such low activation energy. When light and heat stress are applied together, similar hydrogen loss from (i-p)a-Si:H stack is observed, however, does not appreciably degrade iV OC or increase S. This is an important result and departure from direct correlation between hydrogen loss and defect creation. This perhaps indicates additional defect chemistries or annealing that might be occurring in the presence of light requiring further detailed defect measurements. The full SHJ cell structure used for this project is depicted in Fig.1(d). SHJ cells with an initial V OC ≈ 700 mV were fabricated and subjected to similar ALT stress conditions. Cell V OC is found to degrade the most under dark heat stress and is confirmed by observed hydrogen migration out of the (i-p)a-Si:H stack. However, hydrogen cannot escape from the cell stack, it accumulates near the (p)a-Si:H/ITO contact interface, where ITO acts as a barrier preventing hydrogen loss. Furthermore, light-heat combined stress does not degrade V OC appreciably, confirming the occurrence of a defect annealing process.

14 SOLAR ENERGY↗