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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 1,531 records · Page 85
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Facile synthesis of α-MoO{sub 3} nanorods with high sensitivity to CO and intrinsic sensing performance

Highlights: • α-MoO{sub 3} nanorods were synthesized by facile hydrothermal method at 85 °C for 1.5 h. • α-MoO{sub 3} nanorods exhibit the highest sensitivity of 239.6–40 ppm CO at 292 °C. • XPS and PL confirmed that the gas sensing arises from stoichiometric defect of α-MoO{sub 3}. • The sensing mechanism of α-MoO{sub 3} to CO was postulated from bulk defect of material. - Abstract: Orthorhombic molybdenum trioxide (α-MoO{sub 3}) nanorods with well-defined morphology and high crystalline have been synthesized by a facile and fast hydrothermal method under 85 °C for 1.5 h without employing surfactants or templates. The controlling of stirring time, thermostatic time and HNO{sub 3} amount is crucial for the growth of α-MoO{sub 3} nanorods. The morphology and structure of α-MoO{sub 3} were characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The obtained α-MoO{sub 3} nanorods as a novel sensing material exhibit high sensitivity, the highest response to 40 ppm CO is 239.6 at operating temperature of 292 °C. The intrinsic sensing performance arises from the non-stoichiometry of the α-MoO{sub 3} due to the presence of Mo{sup 5+} in MoO{sub 3} lattice, that is, the molecular formula of MoO{sub 3} should be expressed as MoO{sub 3−x} (x = 0.08), which has been confirmed by X-ray photoelectron spectroscopic (XPS) analysis and room temperature photoluminescence (PL). The sensing mechanism of α-MoO{sub 3} to CO was also discussed in terms of lattice oxygen in MoO{sub 3}.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

A contrastive study of three graphite anodes in the piperidinium based electrolytes for lithium ion batteries

Graphical abstract: The fitting results of R{sub sei} and R{sub ct} of three graphite/Li cells. Besides three graphite/Li cells show the similar R{sub sei}, the NG198/Li cell demonstrates a higher R{sub ct} value in all test temperatures. Especially, the R{sub ct} at 333 K is even up to 355.8 Ω cm{sup 2}. Obviously, the narrow distribution of edge plane for NG198 caused this result, and then greatly restricts its cell capacity. By contrast, CMB with bigger specific surface area and more Li{sup +} insertion points shows lower resistance at room temperature, which should help to improve its capacity. - Highlights: • SEI film is closely related to graphite structures and formation temperature. • The graphite with bigger surface area and more Li{sup +} insertion points behaves better. • The graphite with narrow edge plane is uncompetitive for ionic liquid electrolyte. - Abstract: The electrochemical behaviors of natural graphite (NG198), artificial graphite (AG360) and carbon microbeads (CMB) in an ionic liquid based electrolyte are investigated by cyclic voltammetry (CV). The surface and structure of three graphite materials are characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) before and after cycling. It is found that solid electrolyte interface (SEI) is closely related to graphite structure. Benefiting from larger specific surface area and more dispersed Li{sup +} insertion points, CMB shows a better Li{sup +} insertion/de-insertion behavior than NG198 and AG360. Furthermore, electrochemical impedance spectra (EIS) prove that the SEI of different graphite electrodes has different intrinsic resistance and Li{sup +} penetrability. By comparison, CMB behaves better cell performances than AG360, while the narrow edge plane makes NG198 uncompetitive as a potential anode for the ionic liquids (ILs)-type Li-ion battery.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The atomic structure of low-index surfaces of the intermetallic compound InPd

The intermetallic compound InPd (CsCl type of crystal structure with a broad compositional range) is considered as a candidate catalyst for the steam reforming of methanol. Single crystals of this phase have been grown to study the structure of its three low-index surfaces under ultra-high vacuum conditions, using low energy electron diffraction (LEED), X-ray photoemission spectroscopy (XPS), and scanning tunneling microscopy (STM). During surface preparation, preferential sputtering leads to a depletion of In within the top few layers for all three surfaces. The near-surface regions remain slightly Pd-rich until annealing to ∼580 K. A transition occurs between 580 and 660 K where In segregates towards the surface and the near-surface regions become slightly In-rich above ∼660 K. This transition is accompanied by a sharpening of LEED patterns and formation of flat step-terrace morphology, as observed by STM. Several superstructures have been identified for the different surfaces associated with this process. Annealing to higher temperatures (≥750 K) leads to faceting via thermal etching as shown for the (110) surface, with a bulk In composition close to the In-rich limit of the existence domain of the cubic phase. The Pd-rich InPd(111) is found to be consistent with a Pd-terminated bulk truncation model as shown by dynamical LEED analysis while, after annealing at higher temperature, the In-rich InPd(111) is consistent with an In-terminated bulk truncation, in agreement with density functional theory (DFT) calculations of the relative surface energies. More complex surface structures are observed for the (100) surface. Additionally, individual grains of a polycrystalline sample are characterized by micro-spot XPS and LEED as well as low-energy electron microscopy. Results from both individual grains and “global” measurements are interpreted based on comparison to our single crystals findings, DFT calculations and previous literature.

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

Realignment and suppression of charge density waves in the rare-earth tritellurides 𝑅⁢Te 3 (𝑅 = La, Gd, Er)

The rare-earth tritellurides have a rich phase diagram that includes charge density waves (CDWs), superconductivity, and magnetic order, offering a platform to study the interplay between these phases on a square-net system. Prior studies have shown that defects can affect the CDW characteristics in these materials, yet coupling between the CDW order and the underlying microstructure has not been studied at the nanoscale. Here we use scanning transmission electron microscopy at cryogenic temperatures to directly visualize the effects of defects on the CDW order and provide a spatially resolved microscopic correlation between the CDW transition and structural defects. Here, we show that in the presence of extended defects, such as dislocations and stacking faults, the weak orthorhombicity of the rare-earth tritellurides is lost and the material becomes pseudotetragonal. Since the orthorhombicity acts as a symmetry breaking field for the CDW transitions in rare-earth tritellurides, the presence of these extended defects modulates the energetics of the CDWs and suppresses the ground-state CDW phase at low temperature.

Charge density waves↗
DOE OSTI2019

Influence of Ba Substitutions on Microstructure and Magnetic Properties of La–Ca–Co System Permanent Ferrite

La{sub 0.6}Ca{sub 0.4−x}Ba{sub x}O⋅n/2(Fe{sub 1−y}Co{sub y}){sub 2}O{sub 3}(x = 0, 0.05, 0.1, 0.15 and 0.2) permanent ferrite materials were prepared by ceramic technique. The topography and the structure were characterized by scanning electron microscopy (SEM) and x-ray diffraction (XRD), respectively. The magnetic properties were measured using vibrating sample magnetometer (VSM) and digital magnetometer. Single M-phase and flake-like grains were obtained for samples without Ba substitution(x = 0), and the magnetic properties of the pre-sintering La–Ca–Co ferrite were as follows: B{sub r} = 440 mT, H{sub cb} = 296 kA/m, H{sub cj} = 426 kA/m, (BH){sub max} = 36.6 kJ/m{sup 3} and H{sub k}/H{sub cj} = 0.83. When Ca was substituted by Ba, pre-sintered powder presents single M-phase structure and close three-dimensional size of grains, resulting in an improved rectangle ratio of sintered magnet. The rectangle ratio of sintered magnet reaches a maximum of 0.93 when x = 0.1. By optimizing process parameters, M-type La–Ca–Ba–Co sintered magnet was prepared with B{sub r} = 445 mT, H{sub cb} = 337 kA/m, H{sub cj} = 420 kA/m, (BH){sub max} = 38.6 kJ/m{sup 3} and H{sub k}/H{sub cj} = 0.95.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Structural analysis of bioceramic materials for denture application

Structural analysis has been performed on bioceramic materials for denture application by using X-ray diffraction (XRD), X-ray fluorescence (XRF), and Scanning Electron Microscopy (SEM). XRF is using for analysis chemical composition of raw materials. XRF shows the ratio 1 : 1 : 1 : 1 between feldspar, quartz, kaolin and eggshell, respectively, resulting composition CaO content of 56.78 %, which is similar with natural tooth. Sample preparation was carried out on temperature of 800 °C, 900 °C and 1000 °C. X-ray diffraction result showed that the structure is crystalline with trigonal crystal system for SiO{sub 2} (a=b=4.9134 Å and c=5.4051 Å) and CaH{sub 2}O{sub 2} (a=b=3.5925 Å and c=4.9082 Å). Based on the Scherrer’s equation showed the crystallite size of the highest peak (SiO{sub 2}) increase with increasing the temperature preparation. The highest hardness value (87 kg/mm{sup 2}) and match with the standards of dentin hardness. The surface structure was observed by using SEM also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy

Statistically significant crystal structure and composition identification of nanocrystalline features such as nanoparticles/nanoprecipitates in materials chemistry and alloy designing using electron microscopy remains a grand challenge. In this paper, we reveal that differing crystallographic phases of nanoprecipitates in alloys can be mapped with unprecedented statistics using transmission Kikuchi diffraction (TKD), on typical carbon-based electron-transparent samples. Using a case of multiphase, multicomponent nanoprecipitates extracted from an improved version of 9% chromium Eurofer-97 reduced-activation ferritic-martensitic steel we show that TKD successfully identified more than thousand M 23 C 6 , MX, M 7 C 3 , and M 2 X ( M =Fe, Cr, W, V, Ta; X = C, N) nanoprecipitates in a single scan, something that is currently unachievable using a transmission electron microscope (TEM) without incorporating a precision electron diffraction (PED) system. Precipitates as small as ~20–25 nm were successfully phase identified by TKD. We verified the TKD phase identification using high-resolution transmission electron microscopy (HRTEM) and convergent beam electron diffraction (CBED) pattern analysis of a few precipitates that were identified by TKD on same sample. TKD study was combined with state-of-art analytical scanning transmission electron microscopy (STEM)-energy dispersive X-ray (EDX) spectroscopy and multivariate statistical analysis (MVSA) which provided the complete crystal structure and distinct chemistries of the precipitates in the steel in a high throughput automated way. This technique should be applicable to characterizing any multiphase crystalline nanoparticles or nanomaterials. Furthermore the results highlight that combining phase identification by TKD with analytical STEM and modern data analytics may open new pathways in big data material characterization at nanoscale that may be highly beneficial for characterizing existing materials and in designing new materials.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Arsenic detection in water: YPO{sub 4}:Eu{sup 3+} nanoparticles

This work reports on the novel technique of detection of arsenic in aqueous solution utilising the luminescence properties of lanthanide doped nanomaterials. Eu{sup 3+} (5%) doped YPO{sub 4}nanorodswere utilised for the said experiment. Co-precipitation method was used for the synthesis of the materials and characterised them with different instrumental techniques like X-ray diffraction (XRD), Infra-red (IR), UV-absorption, scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and photoluminescence studies. This nanoparticle can adsorb both arsenic and arsenious acids. We studied the effect of arsenic adsorption on the luminescence behaviour of the nanoparticles. Arsenic acid enhanced the luminescence intensity whereas arsenious acid quenched the luminescence. This luminescence enhancement or quenching is related with arsenic concentration. This relation of luminescence property with concentration of arsenic can be used to detect arsenic in industrial waste. - Graphical abstract: Novel technique of detection of Arsenic ion in aqueous solution utilising the luminescence properties of lanthanide doped nanomaterials. Potential application for detection of arsenic in drinking and industrial waste water. - Highlights: • Novel technique of detection of Arsenic in aqueous solution by YPO{sub 4}:Eu{sup 3+} nanomaterials. • The effect of arsenic adsorption on the luminescence behaviour of the nanoparticles was studied. • Arsenic acid enhance whereas arsenious acid quenches the luminescence intensity. • This technique can be used to detect arsenic in industrial waste.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Effect of solvent ratio on the optoelectronic properties of fluorine doped tin oxide thin films

Fluorine doped tin oxide (FTO) thin films were deposited on to the well cleaned microscopic glass substrates using nebulized-spray pyrolysis (n-SP) technique by varying the water to ethanol solvent proportion. The deposited thin films were characterized by X-ray diffraction (XRD), UV-Vis-NIR spectroscopy, field emission scanning electron microscopy and Hall measurements to study the structural, optical, surface morphological and electrical properties of the films, respectively. Results of the analyzes show that the films are polycrystalline, having tetragonal structure with the preferred orientation along (110) plane. The grain size varies between 7 to 20 nm. The optimized films exhibit the optical transparency of 85 % at the wavelength of 580 nm. The optical bandgap lies in the range of 3.94 to 4 eV. The optimized films, deposited with 40 % of ethanol proportion are having the mean resistivity 4.72×10{sup −3} Ω-cm, carrier concentration 1.79×10{sup 20} cm{sup 3} and the mobility 7 cm{sup 2}/Vs.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Studies on structural properties of clay magnesium ferrite nano composite

Magnesium ferrite-bentonite clay composite was prepared by sol-gel combustion method employing citric acid as complexing agent and fuel. The effect of clay on the structural properties was studied with X-ray diffraction (XRD), Fourier transform infrared (FT-IR) Spectroscopy, Scanning electron microscopy (SEM), SEM- Energy dispersive Spectroscope (EDS) and BET surface area analyzer. Decrease in particle size and density was observed on addition of bentonite clay. The BET surface area of nano composite containing just 5 percent clay was 74.86 m{sup 2}/g. Whereas porosity increased from 40.5 per cent for the pure magnesium ferrite to 81.0 percent in the composite showing that nano-composite has potential application as an adsorbent.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Preparation and Characterization of Mn Doped ZnO Nanorods

Mn doped ZnO nanorods were prepared by chemical precipitation method. The micro-structural and structural properties of the nanorods were calculated from the X-ray diffraction technique. The formed nanorods was seen in the scanning electron microscopy. The purity of the sample was confirmed by the energy dispersive X-ray analysis (EDX). The optical properties were studied using UV-Vis spectroscopy and photoluminescence. In the photoluminescence spectrum, the peaks due to recombination of free electrons, oxygen vacancy and intrinsic defects were observed. The magnetic properties were studied using vibrating sample magnetometer (VSM) and the paramagnetic nature of the material was confirmed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Thermodynamic understanding of Sn whisker growth on the Cu surface in Cu(top)-Sn(bottom) bilayer system upon room temperature aging

Sn whiskers are observed by scanning electron microscope on the Cu surface in Cu(top)-Sn(bottom) bilayer system upon room temperature aging. Only Cu{sub 6}Sn{sub 5} phase appears in the X-ray diffraction patterns and no Sn element is detected in the Cu sublayer by scanning transmission electron microscopy. Based on the interfacial thermodynamics, the intermetallic Cu{sub 6}Sn{sub 5} compound phase may form directly at the Sn grain boundary. Driven by the stress gradient during the formation of Cu{sub 6}Sn{sub 5} compound at Sn grain boundaries, Sn atoms segregate onto the Cu surface and accumulate to form Sn whisker.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Mechanisms of ultrafine-grained austenite formation under different isochronal conditions in a cold-rolled metastable stainless steel

The primary objective of this work is to obtain fundamental insights on phase transformations, with focus on the reaustenitization process (α′→γ transformation), of a cold-rolled (CR) semi-austenitic metastable stainless steel upon different isochronal conditions (0.1, 1, 10 and 100 °C/s). For this purpose, an exhaustive microstructural characterization has been performed by using complementary experimental such as scanning and transmission electron microscopy (SEM and TEM), electron backscattered diffraction (EBSD), electron probe microanalysis (EPMA), micro-hardness Vickers and magnetization measurements. It has been detected that all microstructural changes shift to higher temperatures as the heating rate increases. The reaustenitization occurs in two-steps for all heating rates, which is attributed to the chemical banding present in the CR state. The α′→γ transformation is controlled by the migration of substitutional alloying elements across the austenite/martensite (γ/α′) interface, which finally leads to ultrafine-grained reaustenitized microstructures (440–280 nm). The morphology of the martensite phase in the CR state has been found to be the responsible for such a grain refinement, along with the presence of χ-phase and nanometric Ni{sub 3}(Ti,Al) precipitates that pin the austenite grain growth, especially upon slowly heating at 0.1 °C/s. - Highlights: •Ultrafine-grained austenite structures are obtained isochronally at 0.1–100 °C/s •The α′→γ transformation occurs in two steps due to the initial chemical banding •A diffusional mechanism governs the α′→γ transformation for all heating rates •The dislocation-cell-type of martensite promotes a diffusional mechanism •Precipitates located at α′/γ interfaces hinder the austenite growth.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Lunar resources: Oxygen from rocks and soil

The first set of hydrogen reduction experiments to use actual lunar material was recently completed. The sample, 70035, is a coarse-grained vesicular basalt containing 18.46 wt. percent FeO and 12.97 wt. percent TiO2. The mineralogy includes pyroxene, ilmenite, plagioclase, and minor olivine. The sample was crushed to a grain size of less than 500 microns. The crushed basalt was reduced with hydrogen in seven tests at temperatures of 900-1050 C and pressures of 1-10 atm for 30-60 minutes. A capacitance probe, measuring the dew point of the gas stream, was used to follow reaction progress. Experiments were also conducted using a terrestrial basalt similar to some lunar mare samples. Minnesota Lunar Simulant (MLS-1) contains 13.29 wt. percent FeO, 2.96 wt. percent Fe2O3, and 6.56 wt. percent TiO2. The major minerals include plagioclase, pyroxene, olivine, ilmenite, and magnetite. The rock was ground and seived, and experiments were run on the less than 74- and 500-1168-micron fractions. Experiments were also conducted on less than 74-micron powders of olivine, pyroxene, synthetic ilmenite, and TiO2. The terrestrial rock and mineral samples were reduced with flowing hydrogen at 1100 C in a microbalance furnace, with reaction progress monitored by weight loss. Experiments were run at atmospheric pressure for durations of 3-4 hr. Solid samples from both sets of experiments were analyzed by Mossbauer spectroscopy, petrographic microscopy, scanning electron microscopy, tunneling electron microscopy, and x-ray diffraction. Apollo 17 soil 78221 was examined for evidence of natural reduction in the lunar environment. This sample was chosen based on its high maturity level (I sub s/FeO = 93.0). The FeO content is 11.68 wt. percent and the TiO2 content is 3.84 wt. percent. A polished thin section of the 90-150 micron size fraction was analyzed by petrographic microscopy and scanning electron microscopy.

Allen, C. C.↗
DOE OSTI2018

Residual stresses distribution, correlated with bending tests, within explosively welded Ti gr. 2/A1050 bimetals

Highlights: • Ti gr.2/A1050 clad was slightly affected by the explosive welding since negative sign values of stress tensor were detected. • Upon bending higher negative compression stresses were detected in this area. • Twins morphology changed from parallel to cross-shaped arrangement as a consequence of bending. • The compressive twinning was the dominant system before and after three point bending. - Abstract: Synchrotron radiation and XRD{sup 2} method were used to investigate the residual stress distribution before and after three point bending tests within an explosively welded composite composed of two light metals, namely: Ti gr. 2 and A1050. The analysis has shown that the bimetal is slightly affected by the explosive welding process since negative sign values of stress tensor were detected only in the immediate vicinity of interface of Ti gr. 2 characterized by a width of about 0.25 mm. Upon bending higher negative compression stresses are detected in this area as the σ{sub 11} value changes from −500 MPa to −1200 MPa. Additionally, the analysis of microstructure has revealed significant changes in twins morphology with primary and conjugate twinning before and after bending, respectively. However, the compressive twinning was the dominant system in both cases. Bending has changed the initial bimodal texture developing more spread basal components towards the transverse direction. The sample surface has been also significantly affected as the presence of compressive residual stress (−500 MPa) after bending was measured.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Exploring the interfacial structure and crystallinity for direct growth of Mn 3 Sn(0001) on sapphire (0001) by molecular beam epitaxy

The Kagome antiferromagnet Mn 3 Sn has garnered a lot of attention due to the presence of interesting properties such as anomalous Hall effects and Nernst effects. Until now, few papers have been reported to grow using molecular beam epitaxy with a buffer layer or on other substrates. In this paper, we discuss the synthesis of crystalline Mn 3 Sn layers, prepared on Al 2 O 3 (0001) without a buffer layer using molecular beam epitaxy. The growth is monitored in-situ using reflection high energy electron diffraction and measured ex-situ using X-ray diffraction, Rutherford back-scattering, and cross-sectional scanning transmission electron microscopy. The samples were deposited at 524 ± 5 °C, with an Mn: Sn atomic flux ratio of 3.2:1 for 90 minutes. Orientation relationships between the Mn 3 Sn films and the sapphire substrates are determined from in-plane and out-of-plane measurements. Our analysis indicates that the resulting film is predominantly c−plane oriented. Lastly, the samples prepared in this way were found to be discontiguous, showing a 3-dimensional morphology. According to first-principles calculations, the Mn 3 Sn exhibits a displaced Kagome structure in the very first stages of growth, for 2ML and 4ML growth on Al 2 O 3 (0001). This result is corroborated by calculating the surface formation energies and explains the observed RHEED patterns.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Molybdenum Disilicide Oxidation Kinetics in High Temperature Steam

The Fuel Cycle Research and Development program’s Advanced Fuels Campaign is currently supporting a range of experimental efforts aimed at the development and qualification of ‘accident tolerant’ nuclear fuel forms. One route to enhance the accident tolerance of nuclear fuel is to replace the zirconium alloy cladding, which is prone to rapid oxidation in steam at elevated temperatures, with a more oxidation-resistant cladding. Several cladding replacement solutions have been envisaged. The cladding can be completely replaced with a more oxidation resistant alloy, a layered approach can be used to optimize the strength, creep resistance, and oxidation tolerance of various materials, or the existing zirconium alloy cladding can be coated with a more oxidation-resistant material. Molybdenum is one candidate cladding material favored due to its high temperature creep resistance. However, it performs poorly under autoclave testing and suffers degradation under high temperature steam oxidation exposure. Development of composite cladding architectures consisting of a molybdenum core shielded by a molybdenum disilicide (MoSi 2 ) coating is hypothesized to improve the performance of a Mo-based cladding system. MoSi 2 was identified based on its high temperature oxidation resistance in O 2 atmospheres (e.g. air and “wet air”). However, its behavior in H 2 O is less known. This report presents thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and x-ray diffraction (XRD) results for MoSi 2 exposed to 670-1498 K water vapor. Synthetic air (80-20%, Ar-O 2 ) exposures were also performed, and those results are presented here for a comparative analysis. It was determined that MoSi 2 displays drastically different oxidation behavior in water vapor than in dry air. In the 670-1498 K temperature range, four distinct behaviors are observed. Parabolic oxidation is exhibited in only 670-773 K water vapor, a temperature range in which the material pests in dry O 2 environments. From 877-1084 K in water vapor, MoSi 2 undergoes rapid mass gain resulting in oxidation throughout the bulk of the sample at 980 K and 1084 K. The resulting material displays swelling and warping after the 980-1084 K exposures. A pre-passivation heat treatment performed at 1395 K was found capable of producing a coarse SiO 2 layer that limited pesting at lower temperatures in water vapor over the time periods investigated.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Effect of Preparation Conditions of Fe@SiO2 Catalyst on Its Structure Using High-Pressure Activity Studies in a 3D-Printed SS Microreactor

Fischer–Tropsch synthesis (FTS) in a 3D-printed stainless steel (SS) microchannel microreactor was investigated using Fe@SiO2 catalysts. The catalysts were prepared by two different techniques: one pot (OP) and autoclave (AC). The mesoporous structure of the two catalysts, Fe@SiO2 (OP) and Fe@SiO2 (AC), ensured a large contact area between the reactants and the catalyst. They were characterized by N2 physisorption, H2 temperature-programmed reduction (H2-TPR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron microscopy (XPS), and thermogravimetric analysis–differential scanning calorimetry (TGA-DSC) techniques. The AC catalyst had a clear core–shell structure and showed a much greater surface area than that prepared by the OP method. The activities of the catalysts in terms of FTS were studied in the 200–350 °C temperature range at 20-bar pressure with a H2/CO molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher selectivity and higher CO conversion to olefins than Fe@SiO2 (OP). Stability studies of both catalysts were carried out for 30 h at 320 °C at 20 bar with a feed gas molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher stability and yielded consistent CO conversion compared to the Fe@SiO2 (OP) catalyst.

Biochemistry & Molecular Biology↗