Search NASA⌕ Search

SEARCH · Search NASA

Results for “scanning electron microscopy (SEM)”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 325 records · Page 18

Reliability Analysis of Large-Area, Low Pressure-Assisted Silver Sintering for Medium-Voltage Power Modules

Multi-layer insulating ceramic substrates can enable medium-voltage (MV) power modules with reduced peak electric field. This benefit is particularly important for MV silicon carbide (SiC) MOSFETs due to their higher operating voltages. Large-area, low-pressure assisted silver sintering is a potential solution for bonding substrates to create a multi-layer structure. The voiding content and defect density of the bond used to create the multi-layer substrate stack-up is critical to the reliability of the power module and the thermal performance, as this bond is in the primary path for heat dissipation in the power module structure. Here, samples of two-layer direct bonded aluminum (DBA) stacks have been fabricated and subjected to thermal cycling to analyze their reliability. Passive thermal cycling from -40 degrees C to 200 degrees C was performed. Cross-sections were cut at pre-determined intervals and imaged with Scanning Electron Microscopy (SEM). After 1000 thermal cycles, adhesive failures are observed between the sintered silver and the DBA surface. Cross-sections were cut and imaged via optical microscope and SEM. Thermal analyzer measurements are recorded on a 10-kV SiC power module utilizing the sintered DBA substrate stacks.

30 DIRECT ENERGY CONVERSION↗

Characterization of Field-Exposed Photovoltaic Modules Featuring Signs of Contact Degradation

Here, this work investigates several photovoltaic (PV) modules that have shown signs of metal contact corrosion due to field exposure in a hot and humid climate. This includes two multicrystalline silicon aluminum back surface field systems with 10 and 14 years of exposure and one monocrystalline silicon passivated emitter and rear cell system with four years of exposure. A comprehensive, multiscale characterization process is used to evaluate these PV modules in great detail. Current–voltage (I−V), Suns-V OC measurements, electroluminescence imaging, infrared imaging, and ultraviolet fluorescence imaging were performed, and locations of interest were cored and analyzed using cross-sectional scanning electron microscopy (SEM). A rigorous, quantitative analysis procedure for the cross-sectional SEM images is proposed and implemented. Careful characterization does reveal that some of these PV modules do indeed exhibit the same classic signs of acetic-acid-based corrosion of the glass frit that is present at the silver/silicon interface, which have been observed previously in PV modules exposed to damp heat in an environmental chamber.

14 SOLAR ENERGY↗

Copper Electrode on Flexible Substrate by Intense Pulsed Light Sintering of Microsized Copper Particles

Metal electrodes deposited in a grid pattern onto flexible polymer substrates have been shown to be a viable alternative to replace indium tin oxide (ITO) as the transparent anode for organic photovoltaics. copper may be a better alternative in terms of cost and stability for large area low-cost solar modules, specifically on roll-to-roll platforms. These customized electrode patterns can be fabricated from copper nanoparticles through various printing techniques applicable to solution phase processing. The Intense Pulsed Light (IPL) technique has been used to sinter copper nanoparticles (~100nm) to fabricate conductive copper electrodes on flexible polymer substrates. However, compared to nanosized (~100 nm) copper particles, microsized (~2 um) copper is much cheaper. In this work, microsized (~2 um) copper is used to produce high conductive copper inks. The conductivity of the print can be adjusted through the use of surfactant. IPL sintering was optimized to obtain high conductivity copper films. In conclusion, several microscopic and electrical spectroscopic characterization techniques such as scanning electron microscopy (SEM), x-ray diffraction (XRD), 4-point probe resistivity measurements were employed to characterize the copper electrodes.

14 SOLAR ENERGY↗

Tape casting and characterizations of MgO ceramics

Herein we report a high density MgO ceramic substrate produced by the tape casting technology. The tape casting formulation and process produced a uniform tape free of cracking. Y 2 O 3 and SiO 2 were used as the sintering aid for the pressureless sintering of the green tape. X-ray diffraction phase identification indicates that MgO is the main phase, while both Y 2 O 3 and SiO 2 sintering aids react with MgO to form MgY 4 Si 3 O 13 as the second phase. Liquid phase sintering occurs in the temperature range from 1030°C to ~1500°C, which is confirmed by the simultaneous Thermal Gravitation Analysis/ Differential Scanning Calorimeter (TGA/DSC) and the percent linear shrinkage and densification. A 96.5% theoretical density was achieved by presureless sintering at 1650°C for 2 hours, which was further increased to a fully dense structure using hotisostatic- pressing(HIP) at 1650°C and 207 MPa in argon. Scanning electron microscopy (SEM) and energy dispersive(EDS) spectroscopic analysis on the HIP’ed sample show that MgY 4 Si 3 O 13 is located at the MgO grain boundary and the sample has a fully dense structure. The refractive indices and extinction coefficient were measured on the HIP’ed sample along with thermal properties and dielectric properties. Thermal diffusivity and heat capacity were measured to calculate the thermal conductivity.

36 MATERIALS SCIENCE↗

Direct selective laser sintering of hexagonal barium titanate ceramics

Abstract A direct selective laser sintering (SLS) process was combined with a laser preheating procedure to decrease the temperature gradient and thermal stress, which was demonstrated as a promising approach for additive manufacturing of BaTiO 3 ceramics. The phase compositions in BaTiO 3 ceramics fabricated by SLS were investigated by X‐ray and neutron diffractions. The surface morphologies and cross‐section microstructures were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). A dense hexagonal h‐BaTiO 3 layer was formed on the surface and extended to a depth of 500 μm, with a relative density higher than 97% and absence of pores or microcracks. SLS resulted in the formation of the high‐temperature phase, h‐BaTiO 3 , which was retained at room temperature possibly due to the high cooling rate. The grain boundaries of SLSed h‐BaTiO 3 ceramics consist of a Ti‐rich secondary phase. Compared with that of the pressureless sintered t‐BaTiO 3 ceramics, the Vickers hardness of SLSed h‐BaTiO 3 is 70% higher.

Zhang, Xiang↗

Relationship of Chemical Composition and Moisture Sensitivity in LiNi x Mn y Co 1-x-y O 2 for Lithium-Ion Batteries

Chemical composition–moisture sensitivity relationship of LiNi x Mn y Co 1-x-y O 2 (NMC) cathode materials was investigated by exploring crystal structures, surface properties, and electrochemical performance behaviors of various commercial NMC powders: LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NMC111), LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811). The NMC powders were stored in different moisture conditions: moisture-free, humidified air, or immersed in water. Rietveld refinement analysis of X-ray diffraction (XRD) data and scanning electron microscopy (SEM) were used to characterize the crystal structure changes and the evolution of particle surfaces morphologies. The effect of moisture contamination on the electrochemical properties of NMC cathodes was studied by galvanostatic cycling and electrochemical impedance spectroscopy (EIS). The moisture contamination resulted in either structural disorder or unwanted surficial deposition products, which increased a charge-transfer impedance and consequent performance degradation of battery cells. The results showed that NMC’s moisture vulnerability increased with Ni content (x) despite protective coatings on commercial particles, which stressed the necessity of alternative surface passivation strategies of Ni-rich NMC for broad applications such as electric vehicles and electrified aircraft propulsion.

25 ENERGY STORAGE↗

Effect of Oil Viscosity and Impact of Ionic Liquid Additive on Electrically Induced Pitting in Rolling Contact

Electrically induced bearing damage (EIBD) is a growing concern in electric drivetrains, where electrical discharge currents generate localized pitting that accelerates wear and premature failure. While ionic liquids (ILs) have shown promise as lubricant additives due to their natural physical adsorption, strong capabilities of tribofilm formation, and high molecular tunability, their role in mitigating EIBD is little known. This gap is especially evident because lubricant viscosity and film thickness affect discharge behavior, and additive performance in these regimes has not been well explored. In this study, tribological tests were performed using a ball-on-disk pure rolling-contact system under an applied voltage on polyalphaolefin oils of three viscosities (4, 10, and 150 cSt measured at 100 °C), with and without the addition of a phosphonium-phosphate IL. Surface damage was analyzed using scanning electron microscopy (SEM) and stylus profilometry. Damage quantification was based on pit morphology analysis of SEM images. The results provide new insights into how oil viscosity governs the discharge behavior and how an IL additive could influence the pit formation. While viscosity seems to play a significant role, an IL additive shows potential to reduce EIBD and deserves further study.

electrically induced bearing damage (EIBD)↗

Independence of Environmental and Mechanical Damages on Silicone Adhesive Stored in a Thermo-Oxidative Environment

Abstract Elastomeric polymer materials hold a special place in today’s industrial sectors with respect to structural application needs. Low quality materials are detrimental to industries like aerospace, and automotive engineering. Assessment of the durability of elastomers for structural applications has been of much interest among the literary circles for decades and new materials keep outperforming the existing ones. Polymeric adhesives are one of the most abundantly used materials in these industries. All polymeric materials get damaged when in contact with aggressive environments in presence of high temperature and oxygen. Commonly referred to as thermo-oxidation, this environment exposes the material to heat and oxidation reactions in presence of oxygen. Resultantly, during service life, the damage to the polymer matrix is primarily caused by two factors: mechanical damage and environmental aging. Environmental aging is an irreversible phenomenon caused by changes in the molecular structure while mechanical damage maintains the shape of the polymer matrix, and the deterioration is mostly due to polymer chain mobility. Environmental aging can be caused by a single environmental agent or by a synergized impact of several environmental elements. Increasing temperature is found to be proportional to decreasing tensile strength and toughness of material. The rate and extent of degradation can be accessed by scrutinizing the changes in constitutive behavior of material through mechanical and chemical properties. Accelerated thermal aging is among the most common modes of process related degradation, leading generally to chain scission, and crosslinking phenomena and reduced resistance to fracture stress, and strain. In this experimental study, our goal is to separate the environmental degradation from mechanical damage. A silicone-based adhesive was aged in thermo-oxidative at (0%RH) aging environment. The damage and decay mechanisms have been used to draw a distinction between environmental degradation and mechanical damage. Material characterization included uniaxial tensile test (failure and cyclic) and scanning electron microscopy (SEM) tests on as-received and aged samples. Aging was conducted at three different temperatures (60°C, 80°C and 95°C) and six different exposure durations (1, 3, 10, 30, 90 and 200 days). This work confirms that environmental damage is superposed on top of the mechanical damage, and thus, they are separable. The total mechanical and environmental damage is a synergized effect of all exposure conditions and parameters involved i.e., aging time, temperature, and oxygen. The chemistry and mechanics of the polymer degradation were found to be in good agreement with each other.

Alazhary, Sharif↗

A crystal plasticity finite element method modeling of Zircaloy with hydride phases based on scanning electron micrographs

This work developed a microstructure-based finite element model to predict the stress state of alloys with second phase inclusions. Quantitative microstructural details extracted from scanning electron microscopy (SEM) images were used to generate heterogeneous microstructures including the morphology and spatial distribution of hydrides. Generation of digital microstructure was achieved through two steps of tessellations using software Neper and Matlab. The process is demonstrated using an example of Zircaloy material with secondary phases of hydrides dispersed within and stress-strain response of Zircaloy containing hydrides was predicted. The constitutive material model for Zircaloy in this study was based on crystal plasticity theory which considers the hexagonal close-packed (HCP) atomic structure of Zircaloy material. The hydrides were modeled as isotropic elasto-plastic material. A parametric study had been conducted to understand the effect of volume fraction, and lamellae thickness of the hydride phase on the mechanical properties of the overall material. Results can help designers to alter the manufacturing process to obtain the enhanced mechanical properties for components used in nuclear applications made by Zircaloy material.

Kulkarni, Shank S.↗

Mechanical responses of 316L stainless steel printed by wire arc additive manufacturing with different thermal histories

In this paper, 316L stainless steel walls were printed using single-bead pass and multiple-bead pass wire arc additive manufacturing (WAAM), which represent the internal basket wall and external wall of a spent nuclear fuel (SNF) canister; respectively. Scanning electron microscopy (SEM) microstructure characterization and tensile tests at room temperature (21 °C) and elevated temperature (250 °C) were performed on specimens extracted along the length and height directions of the printed walls. Results showed that grain morphology, grain angles, and retained ferrite are different between the two printed walls, which received different heat input in WAAM. The single-bead pass printed wall exhibited higher yield strength than the multiple-bead pass printed wall because of more retained ferrite and larger portion of random-high angle boundaries (RHAB) grains.

Tang, Wei↗

In situ , in vivo , and in operando imaging and spectroscopy of liquids using microfluidics in vacuum

This review offers a succinct overview of the development of a vacuum-compatible microfluidic reactor system for analysis at the liquid vacuum interface (SALVI), and its diverse applications in in situ, in vivo, and in operando imaging of liquid surfaces as well as the air-liquid (a-l), liquid-liquid (l-l), and solid-liquid (s-l) interfaces in the past decade. SALVI is one of the first microfluidics-based reactors that has enabled direct analysis of volatile liquids in vacuum surface tools such as scanning electron microscopy (SEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Its integration into ambient and vacuum spectroscopy and microscopy is illustrated. Several applications are highlighted including (1) imaging nanoparticles in liquid using in situ SEM; (2) mapping the evolving l-l interface using in situ x-ray absorption spectroscopy and ToF-SIMS; (3) following complex a-l interfacial oxidation reaction products using in situ ToF-SIMS; (4) capturing biological interfaces of cells and microbes via in vivo multimodal and correlative imaging; and (5) monitoring the dynamic solid electrode and liquid electrolyte interface using in operando molecular imaging. Finally, outlook and recommendations are presented. Besides showing the holistic information volume obtained by real-time multiplexed imaging, this review intends to convey the importance of tool development in revolutionizing surface and interface analysis using vacuum platforms previously limited to solid surfaces. Microfluidics is manifested to be not limited to ambient conditions in many examples in this review. Moreover, fundamental interfacial phenomena underpinning mass and charge transfer can now be pursued in real time via innovated chemical imaging and spectroscopy.

42 ENGINEERING↗

Evolution of Metastable Phases During Mg Metal Corrosion: An In Situ Cryogenic X-ray Photoelectron Spectroscopy Study

Magnesium and its alloys are potential structural materials candidates for a wide variety of applications due to their high strength-to-weight ratio. However, ductility and poor corrosion resistance under ambient environmental conditions are the bottleneck for industrial deployment. Designing passivation layers and/or corrosion resistant alloys requires fundamental understanding of the corrosion process. The traditional ex-situ spectroscopic measurements of polycrystalline metal surface with ubiquitous surface impurities and grain boundaries only provided an indistinct view of the corrosion process. To clearly distinguish the mechanism and sequence of corrosion process, we employed in-situ cryo-based x-ray photoelectron spectroscopy (XPS) measurements on Mg single crystal surface exposed to aqueous salt solution. Clean Mg (0001) surfaces were exposed to pure D2O and NaCl aqueous solution (5 wt% NaCl+95 wt% D2O). The interfacial reactions were studied using multimodal analysis including XPS, x-ray diffraction (XRD) and scanning electron microscopy (SEM). In contrast to previous studies, our experiments demonstrated the formation of magnesium chloride hydroxide hydrate during aqueous salt corrosion processes. Evidence of metastable ClO* radicals were also found during the initial aqueous salt solution exposure.

Shutthanandan, Vaithiyalingam↗

Quantitative Characterization of the Microstructure-Property Relationships in Ni and MIEC Nanocatalyst-Infiltrated Ni/YSZ Anodes

The performance of solid oxide fuel cell (SOFC) anodes can be improved by infiltration of nanoscale electrocatalysts, which increases triple phase boundary (TPB) density, but only when the added TPBs are active. Quantitative characterization of the microstructure of infiltrated nanocatalysts remains a critical challenge in understanding their role in improved performance. This paper explores the relationship between electrochemical performance and microstructure for Ni/YSZ anodes infiltrated with Ni, gadolinium-doped-ceria (GDC), and Ni/GDC nanocatalysts using a combination of electrochemical impedance spectroscopy (EIS), distribution of relaxation times (DRT) analysis, scanning electron microscopy (SEM) microstructural characterization, and three-dimensional (3-D) anode reconstruction. Estimated polarization resistance improvements as a result of nickel nanoparticle infiltration are discussed.

Rix, Jillian↗

Conformal Pressure and Fast-Charging Li-Ion Batteries

Batteries capable of extreme fast-charging (XFC) are a necessity for the deployment of electric vehicles. Material properties of electrodes and electrolytes along with cell parameters such as stack pressure and temperature have coupled, synergistic, and sometimes deleterious effects on fast-charging performance. We develop a new experimental testbed that allows precise and conformal application of electrode stack pressure. We focus on cell capacity degradation using single-layer pouch cells with graphite anodes, LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532) cathodes, and carbonate-based electrolyte. In the tested range (10–125 psi), cells cycled at higher pressure show higher capacity and less capacity fading. Additionally, Li plating decreases with increasing pressure as observed with scanning electron microscopy (SEM) and optical imaging. While the loss of Li inventory from Li plating is the largest contributor to capacity fade, electrochemical and SEM examination of the NMC cathodes after XFC experiments show increased secondary particle damage at lower pressure. We infer that the better performance at higher pressure is due to more homogeneous reactions of active materials across the electrode and less polarization through the electrode thickness. Our study emphasizes the importance of electrode stack pressure in XFC batteries and highlights its subtle role in cell conditions.

25 ENERGY STORAGE↗

Facile Electrodeposition and Aging to Generate 3-Dimensional α-MnO 2 Battery Cathodes

Conventional tape casting forms 2-dimensional (2D) electrodes containing active material, conductive additive, and binder with restricted ion access as electrodes increase in thickness. To improve the transport properties, 3D architectures were developed using electrodeposition to ensure contact between the active material with the substrate, and provide enhanced electrolyte access. This paper investigates electrodeposition of cryptomelane ( α -MnO 2 ) as a model cathode material to efficiently accommodate (de)lithation and increase areal capacity vs conventional 2D coatings. Electodeposited samples on titantium (Ti) foil substrates were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) and show a linear increase of the average oxidation of Mn (3.5–3.8) and active mass loading (1.27–9.9 mg) with deposition and aging times (0–120 min). The initial deposition is amorphous and forms the crystalline material during the elevated temperature aging step. The active material, α -MnO 2 , was also deposited on C-cloth and these cathodes at deposition times of 3, 6, and 9 min deliver 9, 36, and 69% higher areal capacities, respectively, at 0.2 mA cm −2 compared to conventional 2D electrodes with a mass loading equal to the 3 min sample. These results demonstrate the benefit of α -MnO 2 within a porous architecture providing enhanced transport properties.

Electrochemistry↗

Modeling and Analysis of Polarization Losses in Solid Oxide Fuel Cells with Siloxane Contamination

In this study, the degradation of the solid-oxide fuel cell (SOFC) nickel-yttria stabilized zirconia anode under decamethyltetrasiloxane (L4) contamination is examined with experiments and modeling. A model is developed for the polarization losses based on the charge transfer coefficient,α, and diffusion layer thickness,δ, and fitted to the experimental data to understand how the siloxane degrades the SOFC performance with time. The results of the model indicate that the total polarization losses increase approximately 44% over the course of the 180 min experiment at 350 mA cm −2 . Activation losses dominate the polarization losses initially but decrease in their total contribution while concentration losses increase. Scanning electron microscopy (SEM) with wavelength dispersive X-ray spectroscopy (WDS) elemental mapping indicates that silicon deposition is highest at the outer edge of the anode and forms a barrier layer to fuel diffusion, increasing concentration losses. When the model is applied to other previous D4 and L4 siloxane experiments conducted over a period of 40 h, similar trends in polarization losses are observed. Polarization losses increase more rapidly with D4 compared to L4 siloxane contamination, with concentration losses increasing the fastest with both types of siloxane.

Electrochemistry↗

Fracture, Dissolution, and Cementation Events in Ordovician Carbonate Reservoirs, Tarim Basin, NW China

Ordovician carbonate rocks of the Yijianfang Formation in the Tabei Uplift, Tarim Basin, contain deeply buried (>6000 m), highly productive oil and gas reservoirs associated with large cavities (>10 m). Previous workers inferred that large cavities are paleocaves (paleokarst) formed near the surface and subsequently buried. Alternately, caves may have formed by dissolution at depth along faults. Using 227 samples from 16 cores, we document textures and cement compositions bearing on cavity histories with petrographic, high-resolution scanning electron microscopy (SEM), isotopic, and fluid inclusion microthermometric observations. Results show that dissolution occurred at depth and was caused by (1) acidic fluids derived from Middle-Late Silurian and/or Devonian-Permian hydrocarbon generation and maturation, (2) high-temperature fluids, of which some were associated with Late Permian igneous activity, and (3) Mg-rich fluids that accompanied Jurassic-Cretaceous deformation and the formation of partially open fractures and stylobreccias (fault breccias). The relative paragenetic sequence of the structure-related diagenesis suggests seven stages of fracturing, dissolution, and cementation. Mottle fabrics in the Yijianfang Formation contain argillaceous carbonate-rich silt and are bioturbation features formed within the marine environment. Those mottled fabrics differ from clearly karstic features in the overlying Lianglitage Formation, which formed by near-surface dissolution and subsequent infilling of cavities by allochthonous sediment. Mottle fabrics are crosscut by compacted fractures filled with phreatic-vadose marine cements and followed by subsequent generations of cement-filled fractures and vugs indicating that some fractures and vugs became cement filled prior to later dissolution events. Calcite cements in fractures and vugs show progressively depleted values of δ18O documenting cement precipitation within the shallow (~220 m), intermediate (~625 m), and deep (~2000 m) diagenetic environments. Deep (mesogenetic) dissolution associated with fractures is therefore the principal source of the high porosity-permeability in the reservoir, consistent with other pieces of evidence for cavities localized near faults.

58 GEOSCIENCES↗

Characterization of Nanoscale Pores in Tight Gas Sandstones Using Complex Techniques: A Case Study of a Linxing Tight Gas Sandstone Reservoir

Pore structures with rich nanopores and permeability in tight gas reservoirs are poorly understood up to date. Advanced techniques are needed to be employed to accurately characterize pore structures, especially tiny pores which include micron and nanopores. In this study, various experimental techniques such as scanning electron microscopy (SEM), nuclear magnetic resonance (NMR) T 2 , nitrogen adsorption method, and NMR cryoporometry (NMRC) are combined to interrogate the complex pore systems of the tight gas reservoir in the Linxing formation, Ordos Basin, China. Results show that tight gas sandstones are primarily comprised of residual interparticle and clay-dominated pores. Clay and quartz are two dominate minerals while pyrite occupies a nontrivial amount as well. The permeability of tight gas sandstones is very low, exhibiting an extremely poor positive correlation with porosity. While pore types and relative pore contents are more influential factors on the permeability, accurate characterization of pore size distribution is critical for the permeability of tight gas sandstones. Therefore, complementary characterization methods are carried out, indicating that neither small pores with radii < 100 nm (around peak 1 in NMR T 2 distribution) nor large pores with radii > 5 μ m (around peak 3 in NMR T 2 distribution) control the permeability by analyzing the connectivity of the pores in various size ranges, but rather pores averaging approximately 350 ± X nm (around peak 2 in NMR T 2 distribution) have sufficient connectivity to host and transmit hydrocarbons. The pore size of tight gas sandstones is dominated by the clay-rich mineral assemblage. The study shows that the NMRC technique can be a very promising method, especially when referred to as a promising “roadmap” on how to interrogate tight formations such as the tight gas sands or even shale especially for the nanopore characterization.

15 GEOTHERMAL ENERGY↗