Search NASA⌕ Search

SEARCH · Search NASA

Results for “Scanning Electron Microscopy”

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 181 records · Page 10

A green degumming approach for lignocellulosic kenaf bast using ethanolamine deep eutectic solvent

Traditional chemical degumming methods for lignocellulosic bast fibers pose substantial challenges, especially when dealing with kenaf bast, which has a high lignin content. Here, these challenges include severe pollution and low efficiency, etc. Therefore, this study developed a novel, green, and efficient degumming approach for lignocellulosic kenaf bast, leveraging choline chloride-ethanolamine (ChCl-ETA) alkaline deep eutectic solvent (DES). The efficacy of the ChCl-ETA DES based degumming method was validated through comprehensive chemical composition analysis, scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TG), and two-dimensional (2D) nuclear magnetic resonance (NMR) spectroscopy. Subsequently, the optimal degumming conditions, with a choline chloride to ethanolamine ratio of 1:6 and a degumming temperature of 120 °C, were determined based on the results of the residual gum content. Significantly, the recycled ChCl-ETA DES mixtures could maintain a degumming capacity (revealed by the residual gum content of degummed fibers) comparable to that of the conventional double-boiling method for at least five degumming cycles without purification. Given its low-pollution process and high efficiency, this developed method holds great potential for industrial-scale applications of lignocellulosic bast fibers.

Choline chloride↗

Impacts of irregularly-distributed acidified brine flow on geo-chemo-mechanical alteration in an artificial shale fracture under differential stress

The efficacy of geological carbon sequestration is reliant on the integrity of the caprock and its resistance to physical and chemical alteration. Caprocks with high abundance of reactive carbonates like calcite are susceptible to acid-promoted dissolution and can result in structural weakening. This work investigates the effect of acidified brine flow through an artificially fractured, high-carbonate (30 % by XRD) shale under differential compressive stress. Cylindrical samples were cut in half vertically and milled to create an artificial fracture with interlocking asperities and open channels. Samples were sheared with a single applied stress in a custom flow cell housed within an industrial CT scanner. Further, either acidic (pH 4) or reservoir-simulated (pH 9.5) brine was flowed through the artificial fracture for 7–8 days under reservoir pressure and room temperature. Model simulations indicate flow mainly occurred in open channels, with limited flow between overlapping asperities. Analysis of fracture surfaces by optical and scanning electron microscopy show increased surface alteration and roughness after exposure to pH 4 versus pH 9.5 brine indicating mineral dissolution/loss, and this effect is greater in areas that receive the highest brine flows. Similarly, surface analysis by scratch testing shows fracture toughness decreases more after exposure to acidic versus reservoir-simulated brine, with the greatest alteration in areas of highest acidic brine flows. Despite weakening, no shear slip occurred. Overall, the results indicate that acidified brine can result in significant physical and geomechanical alteration of irregular fracture surfaces in shale caprock, with greatest effects in preferential flow regions.

58 GEOSCIENCES↗

Mechanism of H 2 plasma-enabled reduction of hematite thin films

Hydrogen plasma is gaining significant interest as a promising pathway for direct iron ore reduction and for lowering process temperatures but the reduction mechanism remains poorly understood. In this work we analyzed the plasma and thermal reduction of thin-film hematite (Fe 2 O 3 ) at temperatures below 340 °C using X-ray diffraction and scanning electron microscopy with energy-dispersive X-ray spectroscopy. Plasma reduced the incubation period by an order of magnitude and increased the reduction rate by a factor of 2.6 compared to thermal reduction. Plasma-produced H-atoms facilitate the formation of numerous iron nucleation sites, bypassing the energetically unfavorable dissociative adsorption of H 2 on iron oxide. These iron nuclei can autocatalyze the reduction of the surrounding hematite via a hydrogen spillover mechanism. Our results demonstrate that plasma-derived H-atoms primarily impact the initial nucleation-limited stage. These new insights provide a mechanistic framework that can aid the implementation and optimization of hydrogen plasma-assisted iron oxide reduction at reduced temperatures.

08 HYDROGEN↗

Microwave-assisted pyrolysis of liquid hydrocarbons using iron-based alumina catalysts obtained by solution combustion synthesis: The effect of synthesis parameters

The microwave-absorbing and catalytic properties of iron-based alumina (FeAl x O y ) materials have enabled their use as catalysts for the microwave-assisted generation of hydrogen and carbon via pyrolysis of hydrocarbons. Solution combustion synthesis (SCS) is a promising method to fabricate these materials, but the pyrolysis performance still needs to be improved. The present work investigated how altering the SCS parameters affects the pyrolysis of diesel fuel, gasoline, and crude oil. Two fuels (citric acid and glycine), four Fe:Al molar ratios, and two heating modes (hotplate and furnace) were tested. Fe/γ-Al 2 O 3 and Fe/β-SiC catalysts were prepared via incipient wetness impregnation for comparison. Among the three fossil fuels tested, diesel fuel yielded the highest amounts of H 2 and least amounts of CO x . The choice of fuel for the SCS process and the Fe/Al ratio strongly affected pyrolysis performance as they influence properties important for both catalysis and microwave absorption. The use of glycine resulted in catalysts that exhibited high H 2 yield and low CO 2 generation, which is explained by the revealed structural differences. The increase in the Fe:Al molar ratio accelerated microwave heating by adding more magnetic loss but also increased the amount of CO x . When the optimal SCS parameters were used, FeAl x O y catalysts outperformed Fe/γ-Al 2 O 3 and Fe/β-SiC. The high H 2 generation efficiency of the SCS catalysts is explained by their enhanced microwave-absorption properties. Scanning electron microscopy and energy dispersive X-ray spectroscopy revealed the formation of large-diameter CNTs via the tip-growth mechanism. The regeneration of SCS catalysts was demonstrated via the Boudouard reaction.

Carbon nanotubes↗

The evolution of coal porosity during pyrolysis

Gasification of coal, municipal waste, or other organic materials is a potential hydrogen source that entails complex thermal decomposition and transport processes. This study provides a multiscale analysis of these processes for sub-bituminous (Usibelli, Healy, Alaska) and lignite (Center, North Dakota) coals and provides data useful for process design. The chemistry, mineralogy, and pore structures of pyrolyzed coal and their evolution with thermal decomposition are discussed. Samples pyrolyzed at 200–1000 °C were analyzed by small-angle neutron scattering; ultra-small, small-, and wide-angle X-ray scattering; and other complementary techniques. Scanning electron microscopy showed new pores in the high-temperature-pyrolyzed material. Upon heating, the coals became progressively denser, and the concentration of hydrogen decreased. Changes in pore volume fell into three temperature ranges: an initial, low-temperature range that, for the Usibelli coal, involved an increase in overall porosity; a mid-temperature range associated with pore volume loss; and a high-temperature range associated with significant porosity increase and char formation. This transformation was paralleled by changes in fractal dimension and correlation length. The higher the pyrolysis temperature the greater the small-pore-volume fraction and overall surface area became. Pyrolysis increased the lateral size of coal crystallites, decreased the amorphous fraction, and increased the aromatics fraction and overall coal rank. Comparisons of neutron and X-ray scattering data and subsequent water uptake studies showed that pre-dried coals can re-hydrate relatively rapidly upon exposure to air, which can significantly affect the porosity calculated from small-angle-scattering data. Fits to the cumulative porosity curves provide a method for modeling the physical and chemical transformation of hydrogen-containing feedstock during gasification.

Anovitz, Lawrence {Larry} [ORNL] (ORCID:0000000226↗

Microstructural features underpinning the mechanical behavior of powder metallurgy Cr-based alloys

Refractory materials such as Cr-based alloys offer the potential of enhanced elevated temperature performance but have been limited by their poor formability. However, powder metallurgy has been shown to be a viable pathway to fabricate these alloys. Nanophase separation sintering (NPSS) in particular has been used in the literature to accelerate the densification of powder metallurgy Cr- and W-based alloys. Here, we explore microstructure evolution during NPSS in a binary Cr 85 Ni 15 alloy consolidated via (i) cold pressing & pressureless sintering and (ii) hot isostatic pressing followed by hot extrusion & hot upsetting, and the role of these different processing routes on resulting material properties. The alloy lacked room temperature tensile ductility regardless of consolidation process, with multi-length scale characterization, including scanning electron microscopy, transmission electron microscopy, atom probe tomography, X-ray diffraction, and uniaxial tensile testing, revealing that brittleness was due to intrinsically poor Cr grain boundary cohesion. Tensile testing conducted at 760 °C showed marked strength reduction for the extruded & upset (94 %) condition compared to the pressed & sintered (18 %). The formation of orthorhombic CrNi 2 intermetallics functioned as precipitate strengtheners and prevented elevated temperature softening in the pressed and sintered condition. The findings offer foundational insights into aiding the future development of Cr-based alloys.

36 MATERIALS SCIENCE↗

Diffusion and phase formation in the γ-uranium-technetium system

Phase formation in the U-Tc binary system at 800 °C was investigated using a diffusion couple experiment. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) identified four novel potential intermetallic phases - U 7 Tc 3 , U 13 Tc 12 , U 3 Tc 5 , and UTc 4 . Diffusion coefficients were calculated for the intermetallic phases using the Boltzmann-Matano method and were respectively found to be – 120, 38.2, 15.6, and 1.51 × 10 −18 m 2 /s. Tc also exhibits a solid-solution phase with high penetration into the U with a diffusion coefficient of ∼ 10 −14 m 2 /s. Furthermore, these findings expand the number of known U-Tc phases and provide the first diffusion coefficients for the U-Tc system, and contribute valuable data to the broader field of actinide metallurgy.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Fabrication of yeast engineered porous 13X adsorbent layers for CO 2 capture

This study investigates a novel environmentally friendly coating technique using yeast fermentation to obtain super porous Zeolite 13X adsorbent layers through freeze-drying technique for CO 2 capture applications. Several mass ratios of sugar to yeast were used to control the porosity and pore sizes in the adsorbent layer. A unique peeling process was integrated to obtain foamy, hollow structures to have deeper layer accessibility of adsorbent for adsorption applications. These coated adsorbent layers were experimentally characterized as a function of the mass ratio of sugar to yeast and adsorbent solid fraction. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and Fourier-transform infrared spectroscopy (FT-IR) are used to analyze the coated layers. Here, the void fraction for coated samples is found to vary between 0.48 and 0.56, making the samples applicable for adsorption applications. Adsorption performance experiments are performed to test the coated samples' performance compared to 13X powder. Due to their simplistic fabrication, cost-effectiveness, rapid pore formation, and high adsorption capacity, these porous 13X layers hold potential for large-scale fabrication and CO 2 capture applications.

Adsorbent coating↗

Enhanced grindability of bastnaesite ore by ex-situ CO 2 treatment under the partial pressure of 0-100 psi

High grinding energy consumption has long constrained the sustainable development of mineral processing. This study introduces an innovative technology that employs ex-situ CO 2 treatment to enhance the grindability of bastnaesite ore. The grinding aid effect was evaluated under CO 2 partial pressures ranging from 0 psi to 100 psi using particle size distribution and the Bond work index (BWI), while the underlying mechanism was elucidated with various characterization techniques including inductively coupled plasma (ICP), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Brunauer-Emmett-Teller (BET). The optimal grinding aid effect was achieved at 100 psi partial pressure, 50% slurry concentration, and 3 h reaction duration. Correspondingly, the P80 of the grinding product decreased from 81.76 μm to 72.73 μm and the BWI of bastnaesite ore decreased from 6.96 kW·h/t to 6.30 kW·h/t, a reduction of 9.48%. The grinding aid effect primarily resulted from the transformation of sparingly soluble carbonates like calcite and dolomite into more soluble bicarbonates, which created substantial cracks and pores, thereby reducing the ore's hardness and improving its grindability. By significantly saving grinding energy consumption while delivering environmental benefits, this technology exhibits great promise for further optimization and widespread adoption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Automated SEM analysis of particles in Hanford tank waste

Multiple bench-scale filtration campaigns of Hanford tank waste supernatant on a backpulseable dead-end filtration skid have provided greater insight into the solids that cause fouling and reduce filter performance. The solids collected during each campaign were concentrated from the backpulse solutions and examined using automated particle analysis (APA) methods with scanning electron microscopy (SEM) and x-ray energy dispersive spectroscopy (EDS), to categorize particle types and their morphological characteristics. Finally, we show that with APA, thousands of particles can be analyzed that can provide accurate insight into the phases that may be impacting filter performance.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Microbial reduction of low-crystallinity tripuhyite (FeSbO 4 ): Implications for Sb(V) cycling in contaminated environments

Tripuhyite (FeSbO 4 ) is an important antimony (Sb)-bearing mineral that controls Sb mobility in contaminated environments, yet its structural stability during microbial reduction remains unresolved. Understanding how FeSbO 4 behaves under anoxic conditions is therefore necessary to predict natural Sb cycling. Here, this study examined how an anaerobic microbial community interacts with FeSbO 4 and alters its structural and redox behavior. Across all conditions, FeSbO 4 released measurable Sb(V), demonstrating that the mineral undergoes partial dissolution in anoxic environment even without microbial activity. However, when extensive microbial Fe(III) reduction occurred in the presence of the electron shuttle anthraquinone-2,6-disulfonate (AQDS), the released Sb was re-immobilized. This indicates that microbial reduction processes modulate Sb mobility. Microbial community analysis showed the enrichment of acetate-utilizing Fe(III)-reducing bacteria as key drivers of Fe reduction. Although secondary Fe minerals were not detected, X-ray absorption fine structure measurements and scanning electron microscopy images revealed the formation of an Sb(III)-bearing phase consistent with valentinite (Sb 2 O 3 ) in the AQDS-amended treatment. This transformation suggests that AQDS not only enhances Fe(III) reduction but is also linked to Sb(V) reduction, and facilitates the immobilization of reduced Sb(III) as Sb 2 O 3 . Overall, this work provides the first evidence that FeSbO 4 is susceptible to microbially mediated redox transformations, and that these processes can significantly alter the mobility and speciation of Sb in reducing environments.

Electron transfer mediator↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

Recycling of additively printed anisotropic Nd-Fe-B bonded magnets

A high potential cost-effective and environmentally friendly method has been applied for recycling anisotropic Nd-Fe-B bonded magnets. Waste additively printed Hydrogenation-Disproportionation-Desorption-Recombination (HDDR) Nd-Fe-B anisotropic bonded magnet was pulverized into composite powder containing Nd-Fe-B particles and nylon binder through cryomilling at a liquid nitrogen temperature (~77 K) under Ar inert atmosphere. Then, the cryomilled composite powder was warm compacted into a bonded magnet. Further, the magnetic particles were aligned during post-compaction annealing under a magnetic field of 30 kOe. The recycled bonded magnets have a higher density (3% enhancement), but slightly inferior magnetic properties compared to the original magnets, i.e., the magnetic remanence, coercivity and maximum energy product are reduced by 2%, 3% and 8%, respectively. The scanning electron microscopy revealed that some HDDR Nd-Fe-B powder crumbled into fine particles during cryomilling. Powder X-ray diffraction showed a small amount of Nd-oxide impurity in the cryomilled powder. The slightly deteriorated magnetic properties are ascribed to the oxidation of Nd-Fe-B particles due to formation of fresh fracture surface during cryomilling. The approach enables the direct reuse of end-of-life bonded magnets in an economical and environmentally friendly way.

36 MATERIALS SCIENCE↗

Damage evolution and ductile fracture of commercially-pure titanium sheets subjected to simple tension and cyclic bending under tension

This paper describes a study into the evolution of damage in commercial-purity titanium (CP–Ti) sheets subjected to cyclic bending under tension (CBT) and uniaxial tension (simple tension, ST). Sections were taken from sheets that were strained to various levels under both methods and were imaged using X-ray computed tomography (XCT) to reveal insights into the size, density, and distribution of microvoids in the sheets. Digital image correlation (DIC) was also used to observe the surface strain of CBT and ST sheets during testing. These results showed that elongation to failure (ETF) for CBT deformation is about 2.5× higher than for ST, local longitudinal strains in the bulk of the CBT sample are around 1.3× higher than the peak strain in the ST necked region, and 1.7× higher in the localized region of CBT failure. It was found that the volume-density of voids in both sheets followed a similar exponential increase with strain, reaching nearly 45× higher in the CBT than the ST sheets before the onset of failure, mainly due to the higher strain levels achieved. A higher volume density of voids developed in the center of sheets at high levels of strain, for both processes, with the density in the sheet center becoming approximately double that found near the edges. Scanning electron microscopy (SEM) was used to examine the fracture surface of CBT and ST sheets after failure. The observations are presented and discussed highlighting the CBT process as effective to delay ductile fracture of the CP-Ti sheets.

Commercially pure titanium↗

In situ high-temperature Raman spectroscopy for online EAF slag analysis

Real-time monitoring of slag chemistry is critical for optimizing Electric Arc Furnace (EAF) steelmaking operations, where dynamic variations in slag composition directly influence slag foaming, refractory degradation, and thermal efficiency. Conventional techniques such as X-ray fluorescence (XRF), Fourier-transform infrared (FTIR), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) are commonly used to analyze slag composition, but their offline nature and equipment constraints limit their applicability for online monitoring in harsh industrial environments. To address this challenge, we present an in situ, high-temperature analytical approach that integrates Raman spectroscopy with a custom designed fiber-optic probe for real-time slag characterization at 1550 °C. The system enables non destructive spectral acquisition from molten slags, providing molecular-level insights into silicate polymerization and iron oxidation states. Eight synthetic slag samples were evaluated, and key Raman features—such as Q n silicate units and FeO₄/FeO₆ coordination environments—were identified and quantitatively correlated with slag basicity and Fe₂O₃ content. The results demonstrate agreement between Raman spectral ratios and bulk slag chemistry, validating the method’s capability to track compositional and structural changes under molten temperature. This work establishes the feasibility of deploying fiber-optic Raman probe for online EAF slag monitoring and highlights their potential to support closed-loop control strategies, thereby enhancing process stability, refractory protection, and steel quality in industrial steelmaking applications.

47 OTHER INSTRUMENTATION↗

Insight into the interfacial microstructure and chemistry of hot isostatically pressed AA6061-AA6061 bonds for U-10Mo fuel cladding application

Here, in the present study, hot isostatic pressing (HIP) bonding was carried out using AA6061-AA6061 plates for U-10Mo monolithic fuel cladding application. HIP was performed at 560°C with an applied isostatic pressure of 103 MPa for 90 min. Interfacial microstructure characterizations were performed using scanning electron microscopy (SEM) combined with electron backscatter diffraction (EBSD) to quantify precipitate fractions and study recrystallization, grain growth, and orientation relationships across the interface. EBSD results confirmed that no interfacial grain growth occurred during the HIP process. Transmission electron microscopy (TEM) was also employed to quantify composition and identify phases of various precipitates and an oxide layer that formed at the interface during HIP bonding. Microstructural analyses revealed the formation of a large fraction of Mg 2 Si precipitate and a ~50 nm thick Mg-oxide layer at the interface. Further TEM analysis confirmed that the oxide layer was not continuous, and Mg 2 Al 2 O 5 oxide particles with an average size of 18 nm were present in the oxide layer. Finite element modeling analysis was performed to study the stress distribution at the interface during HIP processing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Investigation of UO 2 doped with Fe 2 O 3 sintered under a reducing atmosphere

Nuclear fuel produced with trace amounts of transition metal additives is of potential interest for introducing intentional signatures for accelerating nuclear forensics. In this work, we investigate the effects on microstructure, grain size, crystal structure, and stoichiometry when trace amounts of Fe in the form of Fe 2 O 3 are added to UO 2 . Sintering of compacts with different concentrations, from 250 to 3000 ppmw, was performed under a reducing atmosphere at 1773 K. The persistence of the taggant during the fuel fabrication process as well as its impact on grain size, crystal lattice, and first-neighbor chemistry was evaluated using inductively coupled plasma–optical emission spectroscopy, powder X-ray diffraction (pXRD), Raman spectroscopy, scanning electron microscopy–backscatter electron spectroscopy, energy dispersive spectroscopy, and thermogravimetric analysis. We observed that a negligible amount of Fe was lost during sintering. Our results indicate that the feedstock, Fe 2 O 3 transforms into Fe and FeO under the test sintering conditions. For all compositions, metallic Fe precipitate was found in grain boundaries as a secondary phase. In conclusion, the potential incorporation of ionic Fe into the UO 2 unit cell was determined by pXRD and Raman spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Statistical fracture behavior of doped UO 2 using a ball-on-ring equibiaxial flexure test method

Metal oxide dopants, such as titanium and chromium oxides, have garnered considerable attention for their potential to increase grain size (≥ 30 µm) in UO 2 fuel, purportedly enhancing fission gas retention during reactor operation. Fuel performance is significantly impacted by fuel fracture behavior, so it is important to understand the effects of enhanced grain size and dopant content on UO 2 fuel fracture. UO 2 pellets were doped with 0.1 wt% TiO 2 and 0.3 wt% Cr 2 O 3 to alter density and grain size. Inductively coupled plasma mass spectroscopy measured dopant levels pre- and post-sintering. X-ray diffraction revealed lattice changes and microstrain via Rietveld refinement. Field emission scanning electron microscopy determined grain sizes of approximately 30 µm for TiO 2 doping and 7 µm for Cr 2 O 3 doping. Transverse rupture strength tests were performed on over 30 samples per dataset to obtain characteristic strength and Weibull modulus. Results indicate no statistical difference in fracture strength between 0.1 wt% TiO 2 doped UO 2 and undoped UO 2 , while 0.3 wt% Cr 2 O 3 doped UO 2 exhibited a 20% decrease in fracture strength. Doped UO 2 samples also showed reduced Weibull modulus compared to undoped UO 2 , suggesting increased scatter in fracture strength. This study's findings suggest that titanium and chromium oxide doping in UO 2 , regardless of grain size, induce residual stresses, decreasing fracture strength and increasing variability in fracture behavior.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗