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At least 505 records · Page 28

Microstructural analysis of tristructural isotropic particles in high-temperature steam mixed gas atmospheres

High-temperature gas-cooled reactors (HTGRs) use tristructural isotropic (TRISO) particles embedded in a graphitic matrix material to form the integral fuel element. Potential off-normal reactor conditions for HTGRs include steam ingress with temperatures above 1,000 °C. Fuel element exposure to steam can cause the graphitic matrix material to evolve, forming an atmosphere composed of oxidants and oxidation products and potentially exposing the TRISO particles to these conditions. Investigating the oxidation response of TRISO particles exposed to a mixed gas atmosphere will provide insight into the stability under off-normal conditions. In this study, surrogate TRISO particles were exposed to high temperatures (T = 1,200 °C) in flowing steam (3% < pH 2 O < 21%) and CO (pCO < 1%) to determine the oxidation behavior of the SiC layer when exposed to various mixed gas atmospheres. Scanning electron microscopy, x-ray diffraction, and focused ion beam milling was used to determine the impact of CO and steam on the oxidation behavior of the SiC layer. Therefore, the data presented demonstrates how the SiC layer showed strong oxidation resistance due to limited SiO 2 growth and maintained its structural integrity under these off-normal conditions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Role of intensive milling in the processing of barium ferrite/magnetite/iron hybrid magnetic nano-composites via partial reduction of barium ferrite

In this research a mixture of barium ferrite and graphite was milled for different periods of time and then heat treated at different temperatures. The effects of milling time and heat treatment temperature on the phase composition, thermal behavior, morphology and magnetic properties of the samples have been investigated using X-ray diffraction, differential thermal analysis, high resolution transmission electron microscopy and vibrating sample magnetometer techniques, respectively. X-ray diffraction results revealed that BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} nanocomposites form after a 20 h milling due to the partial reduction of BaFe{sub 12}O{sub 19}. High resolution transmission electron microscope images of a 40 h milled sample showed agglomerated structure consisting of nanoparticles with a mean particle size of 30 nm. Thermal analysis of the samples via differential thermal analysis indicated that for un-milled samples, heat treatment up to 900 °C did not result in α-Fe formation, while for a 20 h milled sample heat treatment at 700 °C resulted in reduction process progress to the formation of α-Fe. Wustite was disappeared in an X-ray diffraction pattern of a heat treated sample at 850 °C, by increasing the milling time from 20 to 40 h. By increasing the milling time, the structure of heat treated samples becomes magnetically softer due to an increase in saturation magnetization and a decrease in coercivity. Saturation magnetization and coercivity of a sample milled for 20 h and heat treated at 850 °C were 126.3 emu/g and 149.5 Oe which by increasing the milling time to 40 h, alter to 169.1 emu/g and 24.3 Oe, respectively. High coercivity values of milled and heat treated samples were attributed to the nano-scale formed iron particles. - Graphical abstract: Display Omitted - Highlights: • Barium ferrite and graphite were treated mechano-thermally. • Increasing milling time increases reduction progress after heat treatment. • Composites including iron nano-crystals forms by milling and heat treatment. • Shorter milling time results in higher H{sub C} of the milled and heat treated samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A facile route to synthesize core/shell structured carbon/magnetic nanoparticles hybrid and their magnetic properties

Graphical abstract: Controllable synthesis of core/shell structured carbon/magnetic nanoparticles hybrid and their tunable magnetic properties. - Highlights: • The paper reports a simple route for core/shell structured carbon/magnetic nanoparticles hybrid. • By controlling the temperature, Fe{sub 3}O{sub 4}@CNCs, Fe@HCNTs and Fe@LCNTs were produced selectively. • The magnetic properties of the obtained core/shell structured hybrid could be tuned effectively. - Abstract: By controlling the pyrolysis temperature, core/shell structured Fe{sub 3}O{sub 4}/carbon nanocages, Fe/helical carbon nanotubes and Fe/low helicity of carbon nanotubes could be synthesized selectively over Fe{sub 2}O{sub 3} nanotubes generated by a hydrothermal method. The transmission electron microscopic and scanning electron microscopic investigations revealed that the efficiency of generating core/shell structured hybrid was high, exceeding 90%. Because of the magnetic nanoparticles tightly wrapped in graphitic layers, the obtained core/shell structured hybrids showed high stability and good magnetic properties. And the magnetic properties of the obtained core/shell structured hybrid could be tuned by the decomposition temperature and time. Therefore, a simple, inexpensive and environment-benign route was proposed to produce magnetism-tunable core/shell structured hybrid in large quantities.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Correlation of photothermal conversion on the photo-induced deformation of amorphous carbon nitride films prepared by reactive sputtering

The photo-induced deformation of hydrogen-free amorphous carbon nitride (a-CN{sub x}) films was investigated under visible-light illumination. The films gave rise to photothermal conversion by irradiation. In this study, we investigated the effects of thermal energy generated by irradiation on the deformation of a-CN{sub x}/ultrathin substrate bimorph specimens. The films were prepared on both ultrathin Si and SiO{sub 2} substrates by reactive radio-frequency magnetron sputtering from a graphite target in the presence of pure nitrogen gas. The temperature of the film on the SiO{sub 2} substrate increased as the optical band-gap of the a-CN{sub x} was decreased. For the film on Si, the temperature remained constant. The deformation degree of the films on Si and SiO{sub 2} substrates were approximately the same. Thus, the deformation of a-CN{sub x} films primarily induced by photon energy directly.

36 MATERIALS SCIENCE↗

Calorimetry, activity, and micro-FTIR analysis of CO chemisorption, titration, and oxidation on supported Pt

The value of in situ analysis on CO chemisorption, titration and oxidation over supported Pt catalysts using calorimetry, catalytic and micro-FTIR methods is illustrated using silica- and titania-supported samples. Isothermal CO-O and O2-CO titrations have not been widely used on metal surfaces and may be complicated if some oxide supports are reduced by CO titrant. However, they can illuminate the kinetics of CO oxidation on metal/oxide catalysts since during such titrations all O and CO coverages are scanned as a function of time. There are clear advantages in following the rates of the catalyzed CO oxidation via calorimetry and gc-ms simultaneously. At lower temperatures the evidence they provide is complementary. CO oxidation and its catalysis of CO oxidation have been extensively studied with hysteresis and oscillations apparent, and the present results suggest the benefits of a combined approach. Silica support porosity may be important in defining activity-temperature hysteresis. FTIR microspectroscopy reveals the chemical heterogeneity of the catalytic surfaces used; it is interesting that the evidence with regard to the dominant CO surface species and their reactivities with regard to surface oxygen for present oxide-supported Pt are different from those seen on graphite-supported Pt.

Sermon, Paul A.↗

Effects of a noncoplanar biphenyldiamine on the processing and properties of addition polyimides

Addition curing polyimides, prepared from noncoplanar 2,2'-bis(trifluoromethyl) 4,4' diaminobiphenyl (BTDB) with various dianhydrides were evaluated as high temperature polymer matrix materials. T sub g of these polymers were measured by mechanical methods as well as by thermal mechanical analysis. Physical and mechanical properties as well as the thermo-oxidative stability of neat resins and the corresponding G40-600 graphite fiber reinforced composites were compared to that of PMR-II-50 and V-CAP-75.

Chuang, Kathy C.↗

Cation-substituted spinel oxide and oxyfluoride cathodes for lithium ion batteries

The present invention includes compositions and methods of making cation-substituted and fluorine-substituted spinel cathode compositions by firing a LiMn.sub.2-y-zLi.sub.yM.sub.zO.sub.4 oxide with NH.sub.4HF.sub.2 at low temperatures of between about 300 and 700.degree. C. for 2 to 8 hours and a .eta. of more than 0 and less than about 0.50, mixed two-phase compositions consisting of a spinel cathode and a layered oxide cathode, and coupling them with unmodified or surface modified graphite anodes in lithium ion cells.

25 ENERGY STORAGE↗

Soft-Bake Purification of SWCNTs Produced by Pulsed Laser Vaporization

The "soft-bake" method is a simple and reliable initial purification step first proposed by researchers at Rice University for single-walled carbon nanotubes (SWCNT) produced by high-pressure carbon mon oxide disproportionation (HiPco). Soft-baking consists of annealing as-produced (raw) SWCNT, at low temperatures in humid air, in order to degrade the heavy graphitic shells that surround metal particle impurities. Once these shells are cracked open by the expansion and slow oxidation of the metal particles, the metal impurities can be digested through treatment with hydrochloric acid. The soft-baking of SWCNT produced by pulsed-laser vaporization (PLV) is not straightforward, because the larger average SWCNT diameters (.1.4 nm) and heavier graphitic shells surrounding metal particles call for increased temperatures during soft-bake. A part of the technology development focused on optimizing the temperature so that effective cracking of the graphitic shells is balanced with maintaining a reasonable yield, which was a critical aspect of this study. Once the ideal temperature was determined, a number of samples of raw SWCNT were purified using the soft-bake method. An important benefit to this process is the reduced time and effort required for soft-bake versus the standard purification route for SWCNT. The total time spent purifying samples by soft-bake is one week per batch, which equates to a factor of three reduction in the time required for purification as compared to the standard acid purification method. Reduction of the number of steps also appears to be an important factor in improving reproducibility of yield and purity of SWCNT, as small deviations are likely to get amplified over the course of a complicated multi-step purification process.

Yowell, Leonard↗

Electrochemical Transfer of S Between Molten Steel and Molten Slag

S transfer between molten steel and molten slag was investigated in view of the electrochemical character of S transfer. C-saturated molten steel containing S was allowed to react with CaO-SiO{sub 2}-Al{sub 2}O{sub 3}-MgO slag at 1673 K (1400 °C) until the two phases arrive at a chemical equilibrium. The application of an electric field of constant current through graphite electrodes lowered the S content in the molten steel below its chemical equilibrium level, and the system arrived at a new equilibrium level (electrochemical equilibrium). However, subsequent shutting off of the electric field did not lead to the system reverting to the original chemical equilibrium: reversion of S was observed but to a limited extent. The application of an electric field of opposite direction or flowing of CO gas allowed significant reversion of S. Side reactions (decomposition of oxide components) were observed, and these were considered to be coupled to the transfer of S. An electrochemical reaction mechanism was proposed based on the experimental observations found in the present study.

36 MATERIALS SCIENCE↗

Effective Strategy for Improving Electrocatalyst Durability by Adhesive Immobilization of Catalyst Nanoparticles on Graphitic Carbon Supports

We have found that Ta-based additive films in our catalyst system act as adhesives, which improves electrocatalyst durability by immobilizing the catalyst Pt NPs on the graphitic Vulcan carbon support. Furthermore, we suggest that this can be a general design principle in producing higher-durability electrocatalysts on graphitic supports. By electrochemically probing the contributing roles of the tantalum oxide (Ta 2 O 5 ) and the polyphosphate (PPA) components in separate samples, we show that these combine to produce the observed improvement in activity and durability of our best catalyst, the tantalum polyphosphate (TaOPO 4 )-treated sample. To control variables for a valid electrochemical comparison, such as dissimilar catalyst particle size distributions and variations in surface coverage, four new catalyst samples closely matched in every way were prepared: (1) Pt/VC, (2) Pt/[PPA/VC], (3) Pt/[Ta 2 O 5 /VC], and (4) Pt[TaOPO 4 /VC]. We present HR-TEM/HAADF-STEM, EDS elemental mapping, PXRD, XPS, and electrochemical activity and durability evidence, showing that the TaOPO4 and Ta2O5 additives act as adhesives, effectively tethering the NPs to the VC graphitic support surface. Pt/[Ta 2 O 5 /VC] exhibited 3× better durability as compared with the Pt/VC control because of better catalyst nanoparticle immobilization by the Ta 2 O 5 adhesive. Pt[TaOPO 4 /VC] is the overall best performer, exhibiting both a high MA of 0.82 A mg Pt –1, the highest ORR MA after heat treatment, as well as 1.75× greater durability over the Pt/VC control.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Prussian blue derived catalysts

Prussian blue analog derived catalysts having a composition of highly porous transition metal (“TM”) oxides with nano particle size. Such OER catalysts are synthesized from the PBA, containing cobalt, iron, nickel, copper, manganese, zinc, magnesium etc., as secondary building units (“SBUs”) coordinated by hexacyano-based ligands. Furthermore, the PBA-derived catalysts may also integrated into a highly graphitized carbon network to further improve the conductivity, mass transport and durability against oxidative corrosion.

Liu, Di-Jia↗

Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure and chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m{sup 2}/g, 1170 to 210 m{sup 2}/g and 1180 to 480 m{sup 2}/g for acetonitrile, butylamine and pyridine precursors, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Oxo dicopper anchored on carbon nitride for selective oxidation of methane

Abstract Selective conversion of methane (CH 4 ) into value-added chemicals represents a grand challenge for the efficient utilization of rising hydrocarbon sources. We report here dimeric copper centers supported on graphitic carbon nitride (denoted as Cu 2 @C 3 N 4 ) as advanced catalysts for CH 4 partial oxidation. The copper-dimer catalysts demonstrate high selectivity for partial oxidation of methane under both thermo- and photocatalytic reaction conditions, with hydrogen peroxide (H 2 O 2 ) and oxygen (O 2 ) being used as the oxidizer, respectively. In particular, the photocatalytic oxidation of CH 4 with O 2 achieves >10% conversion, and >98% selectivity toward methyl oxygenates and a mass-specific activity of 1399.3 mmol g Cu −1 h −1 . Mechanistic studies reveal that the high reactivity of Cu 2 @C 3 N 4 can be ascribed to symphonic mechanisms among the bridging oxygen, the two copper sites and the semiconducting C 3 N 4 substrate, which do not only facilitate the heterolytic scission of C-H bond, but also promotes H 2 O 2 and O 2 activation in thermo- and photocatalysis, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of fiber reinforcement on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermooxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. The polyimide PMR-15 was the matrix material used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-4OR graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, K. J.↗

An evaluation of candidate oxidation resistant materials

Ground based testing of materials considered for Kapton solar array blanket protection, graphite epoxy structural member protection, and high temperature radiators was performed in an RF plasma asher. Ashing rates for Kapton were correlated with rates measured on STS-8 to determine the exposure time equivalent to one year in low Earth orbit (LEO) at a constant density space station orbital flux. Protective coatings on Kapton from Tekmat, Andus Corporation, and LeRC were evaluated in the plasma asher and mass loss rates per unit area were measured for each sample. All samples evaluated provided some protection to the underlying surface but ion beam sputter deposited samples of SiO2 and SiO2 with 8% polytetrafluoroethylene (PTFE) showed no evidence of degradation after 47 hours of exposure. Mica paint was evaluated as a protective coating for graphite epoxy structural members. Mica appears to be resistant to attack by atomic oxygen but only offers some limited protection as a paint because the paint vehicles evaluated to date were not resistant to atomic oxygen. Four materials were selected for evaluation as candidate radiator materials: stainless steel, copper, niobium-1% zirconium, and titanium-6% aluminum-4% vanadium. These materials were surface textured by various means to improve their emittance. Emittances as high as 0.93 at 2.5 microns for stainless steel and 0.89 at 2.5 microns for Nb-1 Zr were obtained from surface texturing. There were no significant changes in emittance after asher exposure.

Rutledge, Sharon↗

Production of Carbon Nanomaterials and Sorbents from Domestic U.S. Coal (Final Report)

The main goal of this project was to produce high-value carbon nanomaterials and carbon sorbents from domestic coal resources in a cost-effective manner. Four types of domestic coal samples were processed through a combination of deashing, devolatilization, oxidation, reduction, and activation treatments to produce graphene oxide (GO), reduced graphene oxide (RGO), and activated carbon (AC). The precursors and developed materials were extensively characterized by various methods to investigate the impact of the coal feedstock type on the yield and quality of each product. A commercial graphite-based GO sample was included in the experimental work as the baseline material for comparison with the coal-based materials developed in this work. The performed work also included a technoeconomic analysis and cost estimation for a plant processing 20 tons/day coal, a market evaluation for the graphene materials, and a technology gap analysis. A simple process by concentrated nitric acid oxidation is used to oxidize coal precursors for the production of GO. Fine oxidized coal particles that were separated from larger oxidized coal particles had significantly higher oxygen contents and were identified as coal-based GO samples. Coarse oxidized coal particles were used as precursors for production of AC. Based on the Raman spectroscopy results, coal-based GO samples exhibited G and D bands similar to those of graphite-based GO samples. X-ray photoelectron spectroscopy revealed that coal-based GO samples had surface oxygen contents of ~26-35% that were higher than the oxygen contents of graphite-based GO samples. Larger particles of oxidized coal samples were activated under different conditions to produce high surface area functionalized AC. Prepared materials had surface areas exceeding 1,500 m 2 /g and pore volumes more than 1 cm 3 /g with different pore size distributions. Reduced graphene oxide samples were prepared by thermal reduction of both coal-based and graphite-based GO samples at 170-2800 ºC. Coal-based and graphite-based RGO samples exhibited similar carbon contents, Raman spectra, and XRD profiles. Heat treatment above 1500 ºC shifted RGO to synthetic graphite. Among anthracite, bituminous, subbituminous, and lignite coals tested, anthracite was the best precursor to produce carbon nanomaterials exhibiting properties similar to those of graphite-based materials. Anthracite-based carbon nanomaterials also had the highest production yields. Technoeconomic analysis estimated the production cost of GO and RGO for anthracite-based samples at about 2,600 and 4,200 $/ton, respectively, which is about two orders of magnitude lower than the current estimated price of graphite-based materials. Several gaps to further develop the proposed technology were identified and discussed that include process and equipment optimization, process integration, need for additional bench- and pilot-scale experiments, and other items to reduce the scale up risk. Market analysis reports suggested a compound annual growth rate of 40% for graphene and related materials. Short-term applications include composites, inks, and coatings. However, energy storage applications appear to be the dominant potential long-term applications. Different applications of coal-based GO and RGO need to be explored and clear metrics and standards for each application need to be developed.

01 COAL, LIGNITE, AND PEAT↗

Micro-Laser-Induced Breakdown Spectroscopy: A Novel Approach Used in the Detection of Six Rare Earths and One Transition Metal

Laser-induced breakdown spectroscopy (LIBS) was undertaken using an instrument which used a high-powered microscope to deliver the light and tightly focused the low energy laser beam onto the surface of a solid sample. A micro-plasma was generated on the surface of the sample under test even though the amount of energy/pulse from a beam of 532 nm was <1 mJ. Rare earth elements such as europium, gadolinium, lanthanum, neodymium, praseodymium, samarium, and a transition metal, yttrium, were tested. These elements are important in nuclear fission reactions especially for estimation of actinide masses for non-proliferation “safeguards”. Each element was mixed in the graphite matrix in different percentages from 1% to 50% by weight and the LIBS spectra were obtained for each composition as well as after mixing each element in the same amount using oxides of the elements. The data for the 5% mixture of the rare earth elements with graphite powder along with the transition metal has been presented in this article. A micro-LIBS approach was used to demonstrate that these rare earth elements can be identified individually and in a complex mixture in glove boxes in which the microscope LIBS instrument is housed in a nuclear research environment.

36 MATERIALS SCIENCE↗

AGR Fuel Oxidation Testing Summary and Plans

This presentation describes the goals, scope, and plans for oxidation testing of (primarily irradiated) AGR TRISO fuels and related materials (such as graphite and graphitic matrix material). This presentation will be given at the annual program review meeting for the Gas-cooled Reactor program hosted at INL starting on July 16.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗