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At least 325 records · Page 18

Analysis of Sample DUM002 (INL pin casting, 800C/48 hr, 500C 8 hr): Metallographic re-prep, FIB TEM foil extraction and (S)TEM analysis [Slides]

The scale of FIB foils versus the microstructure makes it likely that more than one feature of interest may be in each FIB foil prepared. Intergranular and intragranular silicides and carbides are present. It may be that the silicides are the more potent nuclea9on sites, by initial impressions without statistics. Non-statistical measurements of the lamellar spacing average approximately 300 to 500 nm. Measured U-Mo ratios via EDS were near expectations, even without the need for standards, simplifying analyses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mechanically Activated Combustion Synthesis of MoSi 2 -Based Composites

The thermal efficiency of gas-turbine power plants could be dramatically increased by the development of new structural materials based on molybdenum silicides and borosilicides, which can operate at temperatures higher than 1300 °C with no need for cooling. A major challenge, however, is to simultaneously achieve high oxidation resistance and acceptable mechanical properties at high temperatures. One approach is based on the fabrication of MoSi2-Mo5Si3 composites that combine high oxidation resistance of MoSi2 and good mechanical properties of Mo5Si3. Another approach involves the addition of boron to Mo-rich silicides for improving their oxidation resistance through the formation of a borosilicate surface layer. In particular, materials based on Mo5SiB2 phase are promising materials that offer favorable combinations of high temperature mechanical properties and oxidation resistance. However, the synthesis of Mo-Si-B multi-phase alloys is difficult because of their extremely high melting temperatures. Mechanical alloying has been considered as a promising method, but it requires long milling times, leading to large energy consumption and contamination of the product by grinding media. In the reported work, MoSi2-Mo5Si3 composites and several materials based on Mo5SiB2 phase have been obtained by mechanically activated self-propagating high-temperature synthesis (MASHS). Short-term milling of Mo/Si mixture in a planetary mill has enabled a self-sustained propagation of the combustion front over the mixture pellet, leading to the formation of MoSi2-T1 composites. Combustion of Mo/Si/B mixtures for the formation of T2 phase becomes possible if the composition is designed for the addition of more exothermic reactions leading to the formation of MoB, TiC, or TiB2. Upon ignition, Mo/Si/B and Mo/Si/B/Ti mixtures exhibited spin combustion, but the products were porous, contained undesired secondary phases, and had low oxidation resistance. It has been shown that use of SHS compaction (quasi-isostatic pressing after combustion) significantly improves oxidation resistance of the obtained MoSi2-Mo5Si3 composites. The “chemical oven” technique has been successfully employed to fabricate low-porous Mo5SiB2–TiC, Mo5SiB2–TiB2, and Mo–Mo5SiB2–Mo3Si materials. Among them, Mo5SiB2–TiB2 material possesses good mechanical properties and simultaneously exhibits excellent oxidation resistance at temperatures up to 1500 °C.

36 MATERIALS SCIENCE↗

AOI [3]: Smart Refractory Sensor Systems for Wireless Monitoring of Temperature, Health, and Degradation of Slagging Gasifiers

The objective of the work was to develop refractory “smart bricks”, which would contain embedded temperature, strain/stress, and spallation sensors throughout the volume of highchromia (-Cr 2 O 3 ) refractory brick. The proposed work included work to interconnect the sensors to the reactor exterior, where the sensor signals may be processed by low-power electronics and transmitted wirelessly to a central processing hub. The data processing and wireless transmitter hardware was specifically designed to be isolated (with low power consumption) and to be adaptable to future implementation of energy-harvesting strategies for extended life. Finally, the collected data was incorporated into a model to estimate refractory degradation, a technique that could help monitor the health of the refractory in real-time. The long-term goal of this program was to demonstrate high-temperature, wireless sensor arrays for in situ three-dimensional (3-D) refractory monitoring or mapping for slagging gasification systems. The research was in collaboration with HarbisonWalker International (HWI) Technology Center in West Mifflin, PA. HWI is a leading developer and manufacturer of ceramic refractory products for high-temperature applications. The work completed focused on the following areas: 1) Investigation of the chemical stability, microstructural evolution, grain growth kinetics, degree of homogeneity (quantitative image analysis), and electrical properties of refractory oxide-silicide composites at temperatures between 750-1450ºC; 2) Fabrication of silicide-alumina composite and oxide thermocouples and thermistor preforms and the development of techniques to embed them into high-chromia refractory bricks to form “smart bricks”; 3) Utilization of commercial off-the-shelf discrete components to prototype circuits for interfacing between smart brick sensors and the wireless sensor network. The prototypes were then used to design an integrated circuit for thermistor, thermocouple, and capacitive-based smart brick sensor interfacing; 4) Interfacing of the smart bricks with embedded sensors with wireless motes thus yielding a complete signal chain. This end-to-end data collection system was tested on a furnace heated to 1350°C; 5) Development of a slag penetration model and a nonlinear unknown input filter for the data from the embedded sensors for estimating temperature and extent of slag penetration.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Postirradiation Examination of the ATF-1 Experiments - 2018 Status

The Advanced Fuels Campaign in collaboration with industry are working to develop enhanced accident tolerant fuels for light water reactors. The initial irradiations of these concepts were performed in the Idaho National Laboratory Advanced Test Reactor using simple drop-in style irradiations. These irradiations are collectively referred to as ATF 1. The postirradiation examination of ATF 1 has begun and some concepts have now completed initial examination. This report describes the results of examinations on ATF 1 irradiations designed to test the feasibility of enhancing UO 2 thermal conductivity with additives, ATF 1 irradiations of uranium silicide, and the current status of ATF 1 irradiations that are in process at the hot cell. Enhanced thermal conductivity uranium dioxide composites containing silicon carbide (UO 2 SiC) and diamond (UO 2 diamond) have been irradiated to low burnup. The conditions of this irradiation test and subsequent postirradiation examinations are discussed. These irradiations evaluate fuel microstructure and potential fuel cladding interaction under representative light water reactor power conditions. Both non destructive and destructive techniques have been used to evaluate fuel integrity, fission gas release, fission product distribution, burnup, fuel swelling and cladding strain. Examination of the UO 2 SiC pellets revealed enhanced cracking when compared to a UO 2 rodlet also irradiated under similar conditions. Additionally, instability of the SiC whiskers in the uranium dioxide matrix was observed in the pellet central region, where the local temperatures exceeded 1300 °C. The microstructure of the diamond added UO 2 was severely disrupted during irradiation, resulting in local migration of cesium along the fuel stack and increased fission gas release when compared with the expected release from the Vitanza curve at corresponding values of burnup and irradiation temperature. The postirradiation examination results cast doubt on the suitability of these additives to improve UO 2 fuel performance in a way that would lead to enhanced accident tolerance. Additionally, postirradiation examination data of U 3 Si 2 fuels at low burnup (i.e., < 20 GWd/tHM) for application in advanced Light Water Reactor (LWR) is presented. The U 3 Si 2 pellets show limited cracking in comparison to the expected behavior of UO 2 at same power level. In addition, gamma scanning data did not reveal migration of fission products. Minor homogeneous hardening along the pellet radius due to accumulation of fission products and radiation damage was measured by microindentation. The fission gas release and swelling remains very low. Formation of fission gas bubbles resolvable with optical microscopy occurs from the pellets center outward to approximately 60% of the fuel pellet radius. The overall data suggest a good performance of this accident tolerant fuel candidate at low burnup. Finally, the current status of postirradiation examination on other ATF 1 irradiations will be discussed. These irradiations include UO 2 clad in an FeCrAl alloy, an alternative uranium silicide compound U 3 Si 5 also clad in a FeCrAl alloy, and an interaction test between UO 2 and different FeCrAl alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Assessment of the Viability of Scaled Annular Pellet Fabrication Technologies

The DOE-NE AFC program broadly supports the creation of novel fuel forms including intermetallics, composites, and dopants for high uranium density compounds. While data can be obtained for key performance indicators such as thermal expansion and oxidation resistance in steam, fuel qualification remains a time intensive process. As such, accelerated fuel qualification methods are a recent focus of the program. By first looking at systems with known historical irradiation testing information, like UO 2 , the method of accelerated burnup testing can be validated, followed by use on novel materials with less information available, like silicides and nitrides. The biggest time delay in doing irradiation testing is reaching a “high burnup” fuel, to effectively model how the fuel will behave when it has been fully used. Reaching this point conventionally could take upwards of 30 years. Accelerated burnup would be approaching the threshold of “high burnup”, something on the order or 50GWd/MTU, more quickly, which although achievable in test reactors requires a decade to achieve using current irradiation testing schemes. To achieve this faster rate, the fuel is likely going to be subject to thermal effects commiserate with the increased heat by more fission. In a normal fuel pellet, this increased temperature would operate less efficiently because the thermal diffusivity of the pellet only allows it to transfer heat so quickly, thus causing a high centerline temperature and noticeable stress along the diameter of the pellet. Solutions could include smaller pellets, which would have a greater surface area giving off heat relative to their volume, or “shaped” fuel designs modifying the thermal behavior. The concept that drives the annular pellet design is reduction of the thermal gradient caused from the high “centerline” temperature at the center of a normal pellet to its surface. By removing the center of the pellet, the new centerline will instead be closer to an edge (whether that be the inner or outer edge), allowing cooling to wick away more heat than the traditional design. In an ideal world, the center of the pellet could also have a heat wick running through it allowing heat to be transported away from throughout the pellet. This increase in heat removal would allow the pellet to be subjected to higher energy output, and thus accelerate the burn-up process. UO 2 has been the staple fuel form of nuclear energy for decades, and replacement of this functionally understood material can only be done with sufficient fuel qualification. Increasing the burnup allows us to characterize new fuels with limited to no operational experience behind them, including carbides, nitrides, and silicide’s. Production of the unique geometries detailed herein will allow us to cut qualification times from multi-decadal experiments into the sub-decadal range, vastly increasing the quantity and quality of information available.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High Level Gap Analysis for Accident Tolerant and Advanced Fuels for Storage and Transportation

This initial gap analysis considers proposed accident tolerant fuel (ATF) options currently being irradiated in commercial reactors, since these are most likely for future batch implementation. Also, advanced fuel (AF) options that may be likely for use in advanced reactors are considered. The cladding technologies considered were chromium-coated zirconium-based alloys, FeCrAl, and both monolithic and matrix composite Silicide carbide (SiC). The fuel technologies considered were chromium-doped uranium dioxide fuel, uranium alloys, uranium nitride, and uranium silicide. Numerous national labs, industry, and countries are performing significant testing and modeling on these proposed technologies to establish performance, but at this time none of the prototypes being irradiated have achieved end-of-life (EOL) burnup. There are some testing results after one burnup cycle to verify in-reactor performance, but little data beyond that. As the ATF prototypes acquire more burnup, data will be produced that is relevant to storage and transportation. The DOE:NE Spent Fuel and Waste Science and Technology (SWFST) Storage and Transportation (ST) Control Account will evaluate the performance data as it becomes available for application to the identified gaps for ST.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Oxidation-resistant coatings for refractory metals used in inert atmospheres

Test conditions and results are reported for various coatings on a 1 percent zirconium columbium alloy at a temperature of 2000 deg F. Molybdenum silicide over molybdenum is most effective coating, tin-aluminum coating is adequately protective, chromium-molybdenum silicides are not protective.

Phillips, W. M.↗

Basic factors controlling pest in high temperature systems

The catastrophic disintegration in air at intermediate temperatures of refractory materials which are very resistant to oxidation at high temperatures is known as pest. A study was undertaken to determine whether the mechanism proposed for pest failure in silicides might also be responsible for pest failure in NbAl3. The aim was to correlate oxidation kinetics in the range where disintegration of NbAl3 is observed with delayed failure data obtained under similar conditions. Studies were also undertaken to develop some understanding of deformation mechanisms in both silicides and aluminides.

Berkowitz-Mattuck, J.↗

Bend ductility of columbium alloys WC3015 and Cb752.

Bend angles for columbium-base alloys, WC3015 and Cb752, at temperatures between -300 F and +500 F are reported. WC3015 exhibited a bend transition temperature well below -100 F, but was severely embrittled by silicide coatings. Cb 752 exhibited a bend transition temperature below -300 F, and the silicide coating application did not influence bend angle of the substrate. However, coating failure on both alloys was observed at less than 60 deg bend, even at 500 F. The effect of electron beam welding and gas tungsten-arc welding on the properties of WC3015 and Cb752 are also reported. Both techniques are shown to produce a marked reduction in the bend angle of WC3015. Unlike WC3015, ductility is restored in Cb752 after a suitable postweld anneal. Microstructural and hardness tests results for both alloys are reported and discussed.

Tavassoli, A. A.↗

Degradation and reuse of radiative thermal protection system materials for the space shuttle

Three silicide coated columbium alloys and two cobalt alloys were subjected to identical simulated reentry profiling exposures in both static (controlled vacuum leak) and dynamic (hypersonic plasma shear) environments. Primary emphasis in the columbium alloy evaluation was on the Cb752 and C129Y alloys with a lesser amount on FS85. Commercial silicide coatings of the R512E and VH109 formulations were used. The coated specimens were intentionally defected to provide the types of coating flaws that are expected in service. Temperatures were profiled up to peak temperatures of either 2350 F or 2500 F for 15 minutes in each cycle.

Bartlett, E. S.↗

Outer skin protection of columbium Thermal Protection System (TPS) panels

A coated columbium alloy material system 0.04 centimeter thick was developed which provides for increased reliability to the load bearing character of the system in the event of physical damage to and loss of the exterior protective coating. The increased reliability to the load bearing columbium alloy (FS-85) was achieved by interposing an oxidation resistant columbium alloy (B-1) between the FS-85 alloy and a fused slurry silicide coating. The B-1 alloy was applied as a cladding to the FS-85 and the composite was fused slurry silicide coated. Results of material evaluation testing included cyclic oxidation testing of specimens with intentional coating defects, tensile testing of several material combinations exposed to reentry profile conditions, and emittance testing after cycling of up to 100 simulated reentries. The clad material, which was shown to provide greater reliability than unclad materials, holds significant promise for use in the thermal protection system of hypersonic reentry vehicles.

Culp, J. D.↗

Development and fabrication of improved Schottky power diodes, phases I and II

Reproducible methods for the fabrication of silicon Schottky diodes were developed for the metals tungsten, aluminum, conventional platinum silicide and low temperature platinum silicide. Barrier heights and barrier lowering were measured permitting the accurate prediction of ideal forward and reverse diode performance. Processing procedures were developed which permit the fabrication of large area (approximately 1 sqcm) mesa-geometry power Schottky diodes with forward and reverse characteristics that approach theoretical values.

Cordes, L. F.↗

Exploratory study on microanalysis of thin films by backscattering techniques

Solid phase epitaxial growth of Si layers was studied by backscattering spectrometry for controllable electrical characteristics. Samples were fabricated by vacuum deposition on a thin layer of Sb before deposition of the amorphous Si layer. Analysis of the resulting SPEG layer showed that Sb was present in the SPEG layer of Si. The characteristic of the SPEG layer against the Si substrate was rectifying. A scanning microprobe picture of a cleaved sample established the presence of a depletion region more than 1 micron below the surface. Hall effect data indicated that the SPEG layer was n-type, with average free carrier concentration of about 10 to the 19th power cm/3 and average electron mobility of about 40 sq cm/Vs. SPEG with Pd silicide or Ni silicide transport layers showed fast initial transient growth regimes with slower growth in the steady state regimes.

Mayer, J. W.↗

Development and fabrication of improved Schottky power diodes

Reproducible methods for the fabrication of silicon Schottky diodes have been developed for tungsten, aluminum, conventional platinum silicide, and low temperature platinum silicide. Barrier heights and barrier lowering under reverse bias have been measured, permitting the accurate prediction of forward and reverse diode characteristics. Processing procedures have been developed that permit the fabrication of large area (about 1 sq cm) mesageometry power Schottky diodes with forward and reverse characteristics that approach theoretical values. A theoretical analysis of the operation of bridge rectifier circuits has been performed, which indicates the ranges of frequency and voltage for which Schottky rectifiers are preferred to p-n junctions. Power Schottky rectifiers have been fabricated and tested for voltage ratings up to 140 volts.

Cordes, L. F.↗

Interaction of metal layers with polycrystalline Si

Solid-phase reactions of metal films deposited on 0.5-micron-thick polycrystalline layers of Si grown by chemical vapor deposition at 640 C were investigated by MeV He-4 backscattering spectrometry, glancing angle X-ray diffraction, and SEM observations. For the metals Al, Ag, and Au, which form simple eutectics, heat treatment at temperatures below the eutectic results in erosion of the poly-Si layer and growth of Si crystallites in the metal film. Crystallite formation is observed at temperatures exceeding 550 C for Ag, at those exceeding 400 C for Al, and at those exceeding 200 C for Au films. For Pd, Ni, and Cr, heat treatment results in silicide formation. The same initial silicides (Pd2Si, Ni2Si, and CrSi2), are formed at similar temperatures on single-crystal substrates.

Nakamura, K.↗

Friction and wear properties of three hard refractory coatings applied by radiofrequency sputtering

The adherence, friction, and wear properties of thin hard refractory compound coatings applied to 440C bearing steel by radiofrequency sputtering were investigated. Friction and wear tests were done with nonconforming pin on disk specimens. The compounds examined were chromium carbide, molybdenum silicide, and titanium carbide. The adherence, friction, and wear were markedly improved by the application of a bias voltage to the bearing steel substrate during coating deposition. Analysis by X-ray photoelectron spectroscopy indicated that the improvement may be due to a reduction in impurities in bias deposited coatings. A fivefold reduction in oxygen concentration in MoSi2 coating by biasing was noted. Chromium carbide was not effective as an antiwear coating. Molybdenum silicide provided some reduction in both friction and wear. Titanium carbide exhibited excellent friction and antiwear properties at light loads. Plastic flow and transfer of the coating material onto the pin specimen appears to be important in achieving low friction and wear.

Brainard, W. A.↗

Metallization of Large Silicon Wafers

A metallization scheme was developed which allows selective plating of silicon solar cell surfaces. The system is comprised of three layers. Palladium, through the formation of palladium silicide at 300 C in nitrogen, makes ohmic contact to the silicon surface. Nickel, plated on top of the palladium silicide layer, forms a solderable interface. Lead-tin solder on the nickel provides conductivity and allows a convenient means for interconnection of cells. To apply this metallization, three chemical plating baths are employed.

Pryor, R. A.↗

XPS study of the chemical structure of the nickel/silicon interface

The chemical nature of the Ni/Si, Ni/Ni2Si, and Si/Ni2Si interfaces is studied using X-ray photoelectron spectroscopy. Two approaches are employed: (1) the Ni/silicide and Si/silicide interfaces are examined by dynamically monitoring the advancing reaction front during in situ growth and (2) as-deposited Ni/Si interfacial properties are analyzed by sequential evaporating monolayer Ni films on Si. These experiments show that the Ni/Ni2Si interface consists of a Ni-rich silicide phase, while the Si/Ni2Si interface has a transitional region that is correspondingly Si-rich silicide.

Grunthaner, P. J.↗