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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Migration and Precipitation of Platinum in Anion‐Exchange Membrane Fuel Cells

Abstract Despite the recent progress in increasing the power generation of Anion‐exchange membrane fuel cells (AEMFCs), their durability is still far lower than that of Proton exchange membrane fuel cells (PEMFCs). Using the complementary techniques of X‐ray micro‐computed tomography (CT), Scanning Electron Microscopy (SEM) and Energy Dispersive X‐ray (EDX) spectroscopy, we have identified Pt ion migration as an important factor to explain the decay in performance of AEMFCs. In alkaline media Pt +2 ions are easily formed which then either undergo dissolution into the carbon support or migrate to the membrane. In contrast to PEMFCs, where hydrogen cross over reduces the ions forming a vertical “Pt line” within the membrane, the ions in the AEM are trapped by charged groups within the membrane, leading to disintegration of the membrane and failure. Diffusion of the metal components is still observed when the Pt/C of the cathode is substituted with a FeCo−N−C catalyst, but in this case the Fe and Co ions are not trapped within the membrane, but rather migrate into the anode, thereby increasing the stability of the membrane.

Raut, Aniket↗
DOE OSTI2023

Migration and Precipitation of Platinum in Anion–Exchange Membrane Fuel Cells

Despite the recent progress in increasing the power generation of Anion-exchange membrane fuel cells (AEMFCs), their durability is still far lower than that of Proton exchange membrane fuel cells (PEMFCs). Using the complementary techniques of X-ray micro-computed tomography (CT), Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) spectroscopy, we have identified Pt ion migration as an important factor to explain the decay in performance of AEMFCs. In alkaline media Pt+2 ions are easily formed which then either undergo dissolution into the carbon support or migrate to the membrane. In contrast to PEMFCs, where hydrogen cross over reduces the ions forming a vertical “Pt line” within the membrane, the ions in the AEM are trapped by charged groups within the membrane, leading to disintegration of the membrane and failure. Furthermore, diffusion of the metal components is still observed when the Pt/C of the cathode is substituted with a FeCo–N–C catalyst, but in this case the Fe and Co ions are not trapped within the membrane, but rather migrate into the anode, thereby increasing the stability of the membrane.

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

Atomic force microscopy and scanning electron microscopy characterization of the controlling of surface morphology of epoxy‐amine‐cured spin‐coated films

Abstract Atomic force microscopy (AFM) was successfully used to study spin‐coated, amine‐cured epoxy film microstructure and morphology. The air‐epoxy and epoxy‐substrate interfaces were examined using tapping‐mode height and phase imaging AFM. The impact of relative humidity on the morphology and microstructure of the surfaces was determined. AFM was able to elucidate the changes on the surface as relative humidity during processing increased. It was observed that large nodular formations formed on the epoxy surface expose to the air but not epoxy surface formed on the substrate in addition to varying regions of more or less compliant structures, which was attributed to carbamate formation caused by the amine curing agent reaction with atmospheric CO 2 . Scanning electron microscopy (SEM) was used to further elucidate interface and interphase morphology of spin‐coated epoxies. Experimentation also demonstrated that post‐curing above the glass transition did not change the morphology structure, suggesting surface structures are “locked‐in.” SEM was used to further elucidate how the interface and interphase change with changing environmental conditions at both the air‐epoxy and epoxy‐substrate interface/interphases, including the impact of atmospheric CO 2 on Marangoni cell formation.

Shenk, Timothy M.↗
DOE OSTI2023

Photoexcitation of Fe 3 O Nodes in MOF Drives Water Oxidation at pH=1 When Ru Catalyst Is Present

Abstract Artificial photosynthesis strives to convert the energy of sunlight into sustainable, eco‐friendly solar fuels. However, systems with light‐driven water oxidation reaction (WOR) at pH=1 are rare. Broadly used [Ru(bpy) 3 ] 2+ (bpy=2,2’‐bipyridine) photosensitizer has a fixed +1.23 V potential which is insufficient to drive most water oxidation catalysts (WOCs) in acid, while Fe 2 O 3 , featuring the highly oxidizing holes, is not stable at low pH. Here, the key examples of Fe‐based metal–organic framework (MOF) water oxidation photoelectrocatalysts active at pH=1 are presented. Fe‐MIL‐126 and Fe MOF‐dcbpy structures were formed with 4,4’‐biphenyl dicarboxylate (bpdc), 2,2’‐bipyridine‐5,5’‐dicarboxylate (dcbpy) linkers and their mixtures. Presence of dcbpy linkers allows integration of metal‐based catalysts via coordination to 2,2’‐bipyridine fragments. Fe‐based MOFs were doped with Ru‐based precursors to achieve highly active MOFs bearing [Ru(bpy)(dcbpy)(H 2 O) 2 ] 2+ WOC. Materials were analyzed with X‐ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infra‐red (FTIR) spectroscopy, resonance Raman, X‐ray absorption spectroscopy, fs optical pump‐probe, electron paramagnetic resonance (EPR), diffuse reflectance and electric conductivity measurements and were modeled by band structure calculations. It is shown that under reaction conditions, Fe III and Ru III oxidation states are present, indicating rate‐limiting electron transfer in MOF. Fe 3 O nodes emerge as photosensitizers able to drive prolonged O 2 evolution in acid. Further developments are possible via MOF's linker modification for enhanced light absorption, electrical conductivity, reduced MOF solubility in acid, Ru‐WOC modification for faster WOC catalysis, or Ru‐WOC substitution to 3d metal‐based systems. The findings give further insight for development of light‐driven water splitting systems based on Earth‐abundant metals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Chemical and Electrochemical Characterization of Hot–Pressed Li 6 PS 5 Cl Solid State Electrolyte: Operating Pressure–Invariant High Ionic Conductivity

Sulfide solid state electrolytes (SSE) are among the most promising materials in the effort to replace liquid electrolytes, largely due to their comparable ionic conductivities. Among the sulfide SSEs, Argyrodites (Li 6 PS 5 X, X=Cl, Br, I) further stand out due to their high theoretical ionic conductivity (~1×10 –2 S cm –1 ) and interfacial stability against reactive metal anodes such as lithium. Generally, solid state electrolyte pellets are pressed from powder feedstock at room temperature, however, pellets fabricated by cold pressing consistently result in low bulk density and high porosity, facilitating interfacial degradation reactions and allowing dendrites to propagate through the pores and grain boundaries. Here, we demonstrate the mechanical and electrochemical implications of hot-pressing standalone LPSCl SSE pellets with near-theoretical ionic conductivity, superior cycling performance, and enhanced mechanical stability. X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and x-ray diffraction spectroscopy (XRD) analysis reveal no chemical changes to the Argyrodite surface after hot pressing up to 250°C. Furthermore, we use electrochemical impedance spectroscopy (EIS) to understand mechanical stability of Argyrodite SSE pellets as a function of externally applied pressure, demonstrating for the first time pressed standalone Argyrodite pellets with near-theoretical conductivities at external pressures below 14 MPa.

25 ENERGY STORAGE↗
DOE OSTI2020

High-efficiency single-junction p-i-n GaAs solar cell on roll-to-roll epi-ready flexible metal foils for low-cost photovoltaics

We demonstrate the fabrication and characterization of high-efficiency, single-junction p-i-n GaAs solar cells, on flexible metal foil with epi-ready buffer via roll-to-roll fabrication. Single-junction p-i-n GaAs solar cells were fabricated using metal–organic chemical vapor deposition (MOCVD). Furthermore, an efficiency greater than 13% was obtained at 1 sun, which is the highest reported efficiency on GaAs photovoltaics directly deposited on metal tapes. This exceeds our previously reported study showcasing 11.5% efficiency on single-junction p-n solar cell structure. Improved morphology of p-i-n structure compared with p-n is explained by atomic force microscopy (AFM), scanning electron microscopy (SEM), and helium ion microscopy (HIM) measurements. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis showed reduced Zn diffusion in p-i-n cell compared with the p-n cell. We attribute the improvement in efficiency of p-i-n cells on flexible metal tapes to the quality of the junction, surface morphology, controlled diffusion of species within the active layers, and increase in absorption due to the optimized intrinsic layer thickness.

14 SOLAR ENERGY↗
DOE OSTI2025

Development of Parameters for the Particle Size Distribution of TATB

Laser light scattering (LLS), manual counting of scanning electron microscopy (SEM) images, and reduction of SEM images using ImageJ (open source program) to determine Feret (caliper) diameters were applied to determine particle size distribution (PSD) of four preparations of 1,3,5‐triamino‐2,4,6‐trinitrobenzene (TATB) and yttria‐stabilized zirconia (YSZ), an SEM certified standard. Mie theory was used to reduce the LLS data. The spherical nature of the YSZ made it a good candidate for LLS. Variations in n , the refractive index, and iκ, the imaginary component, produced very little change in the PSD. However, changing the carrier liquid from H 2 O to a 40% aqueous sucrose solution, thereby changing the carrier refractive index, n 0 , substantially affected the PSD. The Mie complex refractive indices for the YSZ were n = 2.200, iκ = 0.100, with a 40% aqueous sucrose solution, n 0 = 1.400. The triclinic crystal structure of TATB made refractive index determinations more difficult, so a study was conducted varying Mie parameters and comparing them to the same data reduced using the Fraunhofer theory. Changing the n and κ parameters produced PSD with a small concentration of particles less than 1 µm in size or none in this range. SEM images, Feret data, manual counting, and Fraunhofer data reduction indicate particles less than 1 µm are probably < 5% in concentration. The final selection of Mie parameters for TATB was n = 2.283, iκ = 0.1, and suspension medium, n 0 = 1.330. Finally, computations, using density functional theory produced similar parameters.

Feret diameter↗
DOE OSTI2023

Mitigating Heavy Ion Irradiation‐Induced Degradation in p‐type SnO Thin‐Film Transistors at Room Temperature

The study investigates the mitigation of radiation damage on p‐type SnO thin‐film transistors (TFTs) with a fast, room‐temperature annealing process. Atomic layer deposition is utilized to fabricate bottom‐gate TFTs of high‐quality p‐type SnO layers. After 2.8 MeV Au 4+ irradiation at a fluence level of 5.2 × 10 12 ions cm −2 , the output drain current and on/off current ratio ( I on / I off ) decrease by more than one order of magnitude, field‐effect mobility ( μ FE ) reduces more than four times, and subthreshold swing (SS) increases more than four times along with a negative shift in threshold voltage. The observed degradation is attributed to increased surface roughness and defect density, as confirmed by scanning electron microscopy (SEM), high‐resolution micro‐Raman, and transmission electron microscopy (TEM) with geometric phase analysis (GPA). A technique is demonstrated to recover the device performance at room temperature and in less than a minute, using the electron wind force (EWF) obtained from low‐duty‐cycle high‐density pulsed current. At a pulsed current density of 4.0 × 10 5 A cm −2 , approximately four times increase in I on / I off is observed, 41% increase in μ FE , and 20% decrease in the SS of the irradiated TFTs, suggesting effectiveness of the new annealing technique.

Al-Mamun, Nahid Sultan↗
DOE OSTI2021

Influence of Protection Layers on Thermal Stability of Nitride Thin Films

Nitrides are commonly studied for their properties relevant to numerous coating applications, and have been recently used to synthesize newly predicted materials in thin film form. However, thermodynamic stability of such nitride materials is difficult to experimentally evaluate, due to limited thermal budget of thin films. Here we show that thermal stability of nitride films can be extended using protection layers. Specifically, we find that zirconium nitride (ZrN) thin films are stable up to at least 1200°C annealing temperature in N2 atmosphere, if aluminum nitride (AlN) diffusion barriers and capping layers are used. X-ray diffraction (XRD) measurements show the expected thermodynamically stable rocksalt structure of ZrN, and scanning electron microscopy (SEM) confirms compact microstructure of these ZrN films. Without such protection layers, transient bixbyite Zr2ON2 phase and high-temperature ZrSi2 phase are observed after annealing by XRD, SEM, and auger electron spectroscopy (AES), due to side reaction with native surface oxide (ZrOx) and substrate (Si) respectively. These results demonstrate that protection layers are beneficial to increase the thermal budget of nitride thin films, for evaluating thermodynamic stability of new nitride materials, for capturing transient metastable phases during crystallization, and for using functional nitride coatings in extreme environments.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Pinhole‐Free Ultrathin Silicon Oxide Layer by Ozone‐Dissolved Deionized Water

The pinhole‐free silicon oxide (SiO x ) layer grown using dissolved ozone in deionized water (DI‐O 3 ) is demonstrated. An ultrathin SiO x layer of thickness 1.53 nm ± 1.5% is grown on silicon wafer using 7 ppm DI‐O 3 . A four‐step methodology, including 25 wt% aq. tetramethylammonium hydroxide (TMAH) solution at 80 °C, is employed to magnify the pinhole signatures in the underlying silicon and visualized with dark‐field optical microscopy (DFOM) and scanning electron microscopy (SEM). The DFOM images show spots on the surface of wafer that originate from airborne particles, contamination, etc. SEM images reveal the absence of etch pits in silicon even after etching of SiO x /silicon in TMAH for 300 s. The minority carrier lifetime and interface states density in AlO x ‐capped SiO x /Si structure are ≥2 ms at carrier density of 1 × 10 15 cm −3 and less than 2 × 10 11 cm −2 eV −1 , respectively.

42 ENGINEERING↗
DOE OSTI2023

Mixed Nanosphere Assemblies at a Liquid–Liquid Interface

The in-plane packing of gold (Au), polystyrene (PS), and silica (SiO 2 ) spherical nanoparticle (NP) mixtures at a water–oil interface is investigated in situ by UV–vis reflection spectroscopy. All NPs are functionalized with carboxylic acid such that they strongly interact with amine-functionalized ligands dissolved in an immiscible oil phase at the fluid interface. This interaction markedly increases the binding energy of these nanoparticle surfactants (NPSs). The separation distance between the Au NPSs and Au surface coverage are measured by the maximum plasmonic wavelength (λ max ) and integrated intensities as the assemblies saturate for different concentrations of non-plasmonic (PS/SiO 2 ) NPs. Further, as the PS/SiO 2 content increases, the time to reach intimate Au NP contact also increases, resulting from their hindered mobility. λ max changes within the first few minutes of adsorption due to weak attractive inter-NP forces. Additionally, a sharper peak in the reflection spectrum at NP saturation reveals tighter Au NP packing for assemblies with intermediate non-plasmonic NP content. Grazing incidence small angle X-ray scattering (GISAXS) and scanning electron microscopy (SEM) measurements confirm a decrease in Au NP domain size for mixtures with larger non-plasmonic NP content. The results demonstrate a simple means to probe interfacial phase separation behavior using in situ spectroscopy as interfacial structures densify into jammed, phase-separated NP films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Quantification of Swelling in Hematite Pellets Reduced Using Hydrogen–Nitrogen Gas Mixture

Iron ore pellets are reduced in a 50%H 2 –50%N 2 1 atm gas mixture at 750, 800, 850, 900, and 950 °C while simultaneously documenting swelling (change in pellet radius) and weight change. Swelling increases with increasing temperature, with catastrophic swelling (>20% of reduction swelling index) observed at 850, 900, and 950 °C. As the pellet is reduced, the pellet radius increases until 40–50% reduction is achieved, followed by a decrease in diameter beyond 40–50% reduction at 750 and 850 °C. At 950 °C, the pellet radius continues to increase with additional pellet reduction without any subsequent decrease in diameter. Scanning electron microscopy (SEM) analysis shows that the neighboring grains inside the pellet sinter together at 750 and 850 °C, whereas the individual grains sinter internally at 950 °C. SEM analysis and observations suggest that the reduction process at 750 and 850 °C can be approximated as a topochemical reaction process, while the reduction process at 950 °C can no longer be approximated as a topochemical reaction process. In conclusion, an empirical equation for the radius of the pellet is derived with fitting parameters dependent on temperature and the degree of reduction of the pellet undergoing reduction based on the experimental data.

08 HYDROGEN↗
DOE OSTI2020

Assessment of Dynamic Fracture in Ultra-High Performance Concrete Using Synchrotron X-ray Source

Ultra-high-performance concretes (UHPCs) retain higher ultimate (compressive) strengths and greater durability relative to traditional concrete materials. As a result, they are enabling construction materials for blast resistant structures, where a higher capacity for energy absorption is required. In past investigations, the strength of UHPCs was shown to retain a dependency on strain rate. Still, the failure mechanisms which govern this rate dependency have yet to be completely elucidated. In the current study, the dynamic fracture behavior of Cor-tuf UHPC was assessed, in-situ, using a Synchrotron X-ray source in phase contrast imaging (PCI) mode. Prior to testing, the material’s morphology was characterized using X-ray computed tomography (CT) and scanning electron microscopy (SEM). A polychromatic pulsed X-ray source, high-speed camera and Kolsky bar apparatus were used in tandem, to observe the transient failure modes. A pin was placed at the end of the incident bar to control the location of damage initiation, and tests were performed at a constant velocity of ~6 m/s. These test conditions were observed to yield cracks with median and/or cone like geometries. Despite the variation in the crack paths, a significant difference in peak load was not observed. The failure mode was also observed to depend on the microstructure of the concrete samples.

Kolsky bar↗
DOE OSTI2020

Computational Methods to Accelerate Development of Corrosion Resistant Coatings for Industrial Gas Turbines

Oxidation resistant overlay coatings protect the underlying superalloy component in industrial gas turbines from oxidation attack. Rate of depletion of the Al-rich β-phase in the bond coat governs the lifetime of these coatings. The applicability of a computational method in accelerating the development of corrosion resistant coatings and significantly reducing the extensive experimental effort to predict coating lifetimes and microstructural changes in three-coated Ni-based superalloys for real operational durations (20–40 kh) was undertaken in the present study. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and electron microprobe analysis (EPMA) were employed to characterize MCrAlY-coated superalloy substrates (1483, 247 and X4) after exposure at 900 °C in air + 10% H 2 O for up to 20,000 h. The model predicted the longest coating lifetime for the coating on X4 substrate. Precipitation of γ' in the coatings was correctly predicted for all three coating systems. Additionally, the model was able to predict the formation of topologically close packed (TCP)-phases in the investigated coating systems.

Pillai, Rishi R.↗
DOE OSTI2024

Nanocomposite Materials for Radionuclide Sequestration from Groundwater Environments

The half-lives of radionuclides range from fractions of a second to billions of years. Since no practical method of altering radioactive decay exists, and since exposure to either the energy emitted from radioactive decay or chemical properties of radionuclides poses dire health risks, radioactive materials must be segregated and controlled. The capture, treatment, and disposition of radioactive materials remain an extraordinary challenge. In here, we focus our attention on the synthesis and characterization of a unique class of nanocomposite materials that have potential for removal of radionuclide contamination. Specifically, we report a simple approach to decorate the surface of iron-based (Fe/FexOy) material with various nano-catalysts. Specifically, copper (Cu), tin (Sn), and silver (Ag) nanoparticles were prepared through two different reduction approaches, namely, citrate and cetyltrimethylammonium bromide (CTAB) methods, on the iron-based material surface. All samples were characterized by a variety of analytical tools, which included scanning electron microscopy (SEM), electron-dispersive X-ray microanalysis (EDS), and EDS mapping to elucidate materials’ morphology as well as nano-catalysts’ loading and location on the iron-based structures.

Hunyadi Murph, Simona E.↗
DOE OSTI2024

Smart manufacturing approach to manufacture bulk nanocrystalline aluminum for lightweight applications

In this research, a smart manufacturing approach was used to enhance the mechanical properties of aluminum (Al) for lightweight applications. The smart manufacturing involved cryomilling of Al powders with and without 5 wt.% magnesium (Mg) powders for varying durations followed by a high-pressure cold spray (HPCS) additive manufacturing process to prepare bulk components. The morphological changes, crystallite size, and composition of the cryomilled powders and cold sprayed (CS’ed) components were examined using scanning electron microscopy (SEM), x-ray diffraction (XRD), and transmission electron microscopy (TEM) techniques. The results showed that the crystallite size reduces with an increase in cryomilling time and the addition of Mg dopant. To test the mechanical properties of the bulk CS’ed components, microhardness tests were performed using a Vickers microhardness tester. Uniaxial tensile tests were also carried out to ascertain the material’s tensile properties. The mechanical testing results showed great improvement in the hardness and tensile strength of CS’ed Al–Mg samples as compared to pure Al samples. Subsequently, fractography analysis of the tensile failed samples was carried out to determine the nature of the failure. Here, the research article also discusses the inherent mechanisms for the improvement in mechanical properties of smart manufactured components as a result of Mg doping and cryomilling.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructural evolution in a precipitate-hardened (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 multi-principal element alloy during high-pressure torsion

Multi-principal element alloys demonstrate high strength, thermal stability, and irradiation resistance, making them excellent candidate materials for applications in nuclear reactors and other harsh environments. Some studies have examined the use of high-pressure torsion to strengthen MPEAs through grain size reduction and strain hardening. However, no studies have investigated the effect of HPT on secondary phases (precipitates) within an MPEA. Two alloys, (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 containing Ni(Ti, Al) B2 phase, and CrFe σ phase, and single-phase Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , were fabricated by casting and heat treatment. Both alloys were then processed with HPT to study microstructural evolution. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the alloys before and after HPT processing. HPT processing produced a nanocrystalline structure in both alloys, but (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 exhibited a significantly smaller grain size and higher dislocation density than Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , with corresponding higher hardness. Before HPT, the (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 alloy consisted of large grain (~ 400 μm) and precipitates, including B2 of ~ 38 μm average size, B2 of ~ 0.7 μm average size, and small amounts of σ of ~ 1.5 μm average size. After HPT, the larger B2 precipitates were decreased in size and volume fraction, while the smaller B2 precipitates were completely dissolved; the σ precipitates appeared unaffected by HPT, likely due to their much higher hardness. Finally, observation of the B2 precipitate distribution along radial distance indicates that the strain caused the precipitates to fracture at intermediate strain (γ = 125) and dissolve at high strain (γ = 280).

36 MATERIALS SCIENCE↗