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At least 289 records · Page 16

Electrochemical study of the dissolution of oxide films grown on type 316L stainless steel in molten fluoride salt

The corrosion behavior of oxide films grown on Type 316L stainless steel (SS) in molten FLiNaK (LiF-NaF-KF: 46.5−11.5−42 mol.%) salt was investigated. The results show that the oxide film formed on Type 316L SS is unstable and can only temporarily protect materials from corrosion in molten FLiNaK salt. Based on the electrochemical impedance spectroscopy, the oxide dissolution rate is calculated to be 0.85 nm/h at 700 °C in molten FLiNaK salt. Finally, after the oxide film dissolved, Cr and Fe are selective dealloyed from the steel, leading to intergranular corrosion of Type 316L SS in molten fluoride salt.

EIS↗

Determination of the electrical conductivity of liquid Ge(0.95)Si(0.05)

We have measured the electrical conductivity of molten germanium-silicon Ge(0.95)Si(0.05) from the liquidus temperature (1050 C) up to 1220 C. The data were acquired with a unique apparatus which utilizes the standard four-probe technique. The basic unit consists of a fused silica enclosure that contains hermetic glass-to-tungsten seals that can support vacuum pressures down to 10(exp -7) Torr. With calibration, the measurement error for the low vapor pressure materials of this study was typically less than 7%. The temperature dependence of the electrical conductivity of a Ge(0.95)Si(0.05) melt was found to vary from approximately 22,300/ohm/cm at the liquidus temperature down to approximately 16,000/ohm/cm at 1220 C. The negative temperature coefficient as well as the magnitude of these data clearly indicate that the molten material is metallic in nature despite the semiconducting properties of the solid.

Rolin, T. D.↗

Solid structure of Li 2 BeF 4 (FLiBe) from room temperature to melting studied by neutron and X-ray diffraction

Molten fluoride salts such as Li 2 BeF 4 (FLiBe) are used in molten salt reactors, fluoride-salt-cooled high-temperature reactors and fusion reactors as a fuel solvent, coolant and/or tritium breeding medium. In engineered systems that use molten salt, solid-state material will be present during melting and freezing scenarios, and therefore the temperature-dependent properties of the solid and solid/liquid phase transition merit investigation. To observe the behavior of the solid state of Li 2 BeF 4 from room temperature to melting, this work used neutron and X-ray diffraction to measure the changes in the lattice parameters and volume of the crystalline unit cell and compared the results with prior low-temperature data for solid Li 2 BeF 4 . From neutron diffraction data it is also possible to identify anisotropy: centimetre-scaled crystals align preferentially with the a axes parallel to the direction of freezing front propagation, and the c axes expand 54% more than the a axes. This work provides the lattice constants as a function of temperature, quantifies the thermal expansion, and determines the equation describing the change in density for solid Li 2 BeF 4 from room temperature to 459°C to be ρ solid (kg m −3 ) = 2182 (3) − 0.115 (2) T (°C) and the volume expansion upon melting to be less than 5%. This density changes depending on molecular weight and enrichment.

36 MATERIALS SCIENCE↗

Corrosion and Mechanical Durability Testing in High Temperature Molten Sulfur (CRADA Final Report)

The overall goal of the project is to explore and identify suitable candidate materials for high-temperature molten sulfur thermal energy storage (TES) operating up to a maximum temperature of 400°C–420°C for industrial process heat applications. A detailed corrosion and strength analysis of coupons subjected to long-term thermal testing in molten sulfur will be conducted to characterize the fundamental corrosion mechanism, corrosion rates, and mechanical durability. The results from the project contribute to the engineering design of sulfur TES systems with desired longevity and lower construction and maintenance costs. The research outcome benefits the TES research and development community by providing detailed corrosion and degradation information for more effective engineering design of the molten sulfur TES containment. It improves the diversity and reliability of the renewable technologies available for the U.S. industries and U.S. power grid.

14 SOLAR ENERGY↗

Experimental Demonstration of the Molten Oxide Electrolysis Method for Oxygen and Iron Production from Simulated Lunar Materials

This paper presents the results of a Marshall Space Flight Center funded effort to conduct an experimental demonstration of the processing of simulated lunar resources by the molten oxide electrolysis (MOE) process to produce oxygen and metal from lunar resources to support human exploration of space. Oxygen extracted from lunar materials can be used for life support and propellant, and silicon and metallic elements produced can be used for in situ fabrication of thin-film solar cells for power production. The Moon is rich in mineral resources, but it is almost devoid of chemical reducing agents, therefore, molten oxide electrolysis, MOE, is chosen for extraction, since the electron is the most practical reducing agent. MOE was also chosen for following reasons. First, electrolytic processing offers uncommon versatility in its insensitivity to feedstock composition. Secondly, oxide melts boast the twin key attributes of highest solubilizing capacity for regolith and lowest volatility of any candidate electrolytes. The former is critical in ensuring high productivity since cell current is limited by reactant solubility, while the latter simplifies cell design by obviating the need for a gas-tight reactor to contain evaporation losses as would be the case with a gas or liquid phase fluoride reagent operating at such high temperatures. In the experiments reported here, melts containing iron oxide were electrolyzed in a low temperature supporting oxide electrolyte (developed by D. Sadoway, MIT).

Curreri, P. A.↗

Numerical Prediction of Oscillation Behaviors of a Multiphase Core–Shell Droplet During Interfacial Tension Measurement

Interfacial tension between molten high-temperature materials is to be measured using the electrostatic levitation furnace (ELF) and the electromagnetic levitator (ISS-EML) aboard the International Space Station. A levitated compound droplet of a concentric core–shell structure is excited either by an impulsive electromagnetic field or by a superimposed electrostatic field. The oscillation behavior of the compound droplet is analyzed to measure interfacial tension at the interface of the two phases. In support of the space experiments, a computational fluid dynamic model was developed to characterize the oscillation behavior of multiphase core–shell droplet. The developed model predicted the interfacial tension between molten copper-rich and cobalt-rich phases with a difference of 3.3 pct compared to the values reported in literature. The developed model is being utilized to investigate the influence of various test parameters on measured surface tension and also being extended for molten steel–molten slag systems.

36 MATERIALS SCIENCE↗

Residual Gas Effects on Detached Solidification in Microgravity

Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long-term goal is to make such detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Detached solidification is more likely when the contact angle for the melt on the ampoule wall is high, i.e. non-wetting. It has been claimed that impurities increase the contact angle. The objective of the current project is to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. We are focusing on determining the influence of oxygen on the contact angle of molten InSb on clean silica ('quartz'), including the advancing and retreating contact angles in addition to the usual equilibrium contact angle. We have created a gas flow system that allows us to control the oxygen partial pressure over a sessile drop of InSb on a horizontal quartz surface. The cell is slowly tilted while videotaping to reveal the contact angles on the two sides of the drop just prior to it rolling down the surface. Thus far, we have learned the following: (1) Molten InSb readily forms an oxide layer in the presence of the trace amounts of oxygen found in high purity argon; (2) This oxide contains a substantial amount of Ga, which presumably is a trace contaminant that is not detectable in the starting material; (3) The addition of 10% hydrogen to the argon gas is sufficient to reduce the oxide and produce a clean drop; (4) An infrared filter must precede the video camera in order to produce a sharp image of the drop for later image analysis; (5) Tilting the surface on which the drop rests causes the two sides of the drop to display different contact angles, reflecting contact line sticking; (6) Vibration strongly accelerates the approach of the drop to its final shape on a horizontal surface by helping to overcome sticking of the contact line; (7) Oscillation of the drop surface due to vibration appears to increase as the surface is inclined from horizontal. Presumably, the angle at which the drop rolls down the surface is also reduced by vibration. This observation is particularly significant, as the meniscus must move along the ampoule wall during detached solidification.

Regel, Liya L.↗

Measure the effect of molten halide salt exposure on creep rupture lifetime

Recent resurgence in the research and commercial interests in molten salt reactors (MSRs) as a viable advanced reactor concept to achieve the short- and long-term climate goals has resulted in ongoing efforts to demonstrate their commercial potential. These are relying on a combination of the extensive legacy knowledge from the molten salt reactor experiment (MSRE) and relatively recent data on materials compatibility of structural materials of interest such as 316H in molten salts environments. However, there is a critical lack of data on the mechanical behavior of alloys of interest for MSRS such as 316H, 617 and 709 in molten fluoride (FLiNaK or FLiBe) or chloride (NaCl-MgCl 2 ) salts. Limited legacy data from the molten salt reactor experiment (MSRE) program showed a significant reduction in creep rupture strength of a Ni-base alloy (Ni-15Cr-7Fe wt.%) in the molten fluoride NaF-ZrF4-UF4 (50-46-4 mol.%) salt. With ongoing efforts to commercialize different molten salt reactor concepts, the industry can considerably benefit from quantitative information on the impact of molten halide salts on the engineering properties such as creep and fatigue strength of materials of interest. Creep tests for 316H were conducted with fluoride (FLiNaK) and chloride (NaCl-MgCl 2 ) salts tat 650°C/150 MPa while alloys 709 and 617 were tested with FLiNaK at 700C/158 MPa and 750C.146 MPa respectively. Baseline tests were conducted in air to assess the impact of the molten salts on the creep behavior.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

In situ measurement of phase transformations and residual stress evolution during welding using spatially distributed fiber-optic strain sensors

Welding of high-strength steels can result in large tensile strains as the base metal and filler material cool from their molten state. To combat these large tensile strains, low-transformation-temperature (LTT) metal fillers have been proposed. These fillers undergo a martensitic phase transformation at a lower temperature which can ultimately reduce the tensile strain or can even introduce compressive strain adjacent to the weld metal. However, the process for optimizing the composition of the LTT material, as well as various weld parameters for each unique weld geometry, can be quite expensive, especially if the acceptance criterion requires using neutrons, x-ray beams, or destructive techniques to characterize residual stresses. This work describes a simple, low-cost method for quantifying residual stresses and phase transformations in situ during welding. Spatially distributed fiber-optic sensors were bonded to a cast iron plate, along with tack-welded thermocouples, to measure temperature and strain during multiple passes with LTT filler metals. Results show that the fiber-optic sensors can successfully resolve compressive strain adjacent to the weld region caused by the martensitic phase transformations in the LTT filler material.

47 OTHER INSTRUMENTATION↗

Study program to develop and evaluate die and container materials for the growth of silicon ribbons

The development and evaluation of proprietary coatings of pure silicon carbide, silicon nitride, and aluminum nitride on less pure hot pressed substrates of the respective ceramic materials, is described. Silicon sessile drop experiments were performed on coated test specimens under controlled oxygen partial pressure. Prior to testing, X-ray diffraction and SEM characterization was performed. The reaction interfaces were characterized after testing with optical and scanning electron microscopy and Auger electron spectroscopy. Increasing the oxygen partial pressure was found to increase the molten silicon contact angle, apparently because adsorbed oxygen lowers the solid-vapor interfacial free energy. It was also found that adsorbed oxygen increased the degree of attack of molten silicon upon the chemical vapor deposited coatings. Cost projections show that reasonably priced, coated, molten silicon resistant refractory material shapes are obtainable.

Addington, L. A.↗

Pyrometry Without Spurious Reflections

Temperature of heated spherical specimen of opaque material with specular surface measured by optical pyrometry, without need to correct for effect of reflected thermal radiation upon measured radiances, provided reflections eliminated. To prevent unwanted reflections, apparatus must be arranged so field of view of pyrometer does not contain any lines of sight to image of wall. Particularly useful for making accurate noncontact measurements of levitated specimens of molten metal and other materials in containerless processing.

Thomas, Andrew S. W.↗

Development of a Miniature Small Punch Creep Test for Post Surveillance Test Specimens

Summary: This poster outlines a new small punch creep test (SPCT) for examining the mechanical properties of post surveillance test specimens. A surveillance test article was previously designed to study the effects of Molten-Salt conditions on the structural materials in the reactor. To better understand the post-test mechanical properties of the specimen, a miniature SPCT is proposed. The principle, testing standards and challenges of the method is introduced in the poster. An initial design of the testing apparatus is shown, and an experiment plan is outlined.

36 MATERIALS SCIENCE↗

Re-evaluating the Thermal-Spectrum Molten-Salt Breeder Reactor Fuel Cycle in a Modern Context

The current need to rapidly and substantially expand clean power production combined with limited capability for domestic uranium enrichment results in a U.S. nuclear power production planning environment similar to that of the first nuclear era. The U.S. thermal-spectrum molten-salt breeder reactor (TS-MSBR) program emerged during the first nuclear era as means to support rapid nuclear power expansion while minimizing demand on fissile resources. The primary reasons that the TS-MSBR program was discontinued in the 1970s were the comparatively large amount of required effort to mature its technology sufficiently for commercial deployment and the access to separated fissile material provided by the design of its integrated fuel cycle. The slowdown in U.S. electrical load growth after 1980 and the abundance of inexpensive fossil fuels inhibited reconsideration of TS-MSBR development for decades. The purpose of this discussion is to re-examine the value and technical challenges of TS-MSBRs with integrated fuel salt chemical processing considering the renewed need for rapid expansion of clean energy production worldwide, the current state of technology, the challenge of actinide wastes, and the continuing need to maintain a high degree of proliferation resistance and to integrate safeguards into the design.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Measure the effect of molten halide salt exposure on creep rupture lifetime

Recent resurgence in the research and commercial interests in molten salt reactors (MSRs) as a viable advanced reactor concept to achieve the short- and long-term climate goals has resulted in ongoing efforts to demonstrate their commercial potential. These are relying on a combination of the extensive legacy knowledge from the molten salt reactor experiment (MSRE) and relatively recent data on materials compatibility of structural materials of interest such as 316H in molten salts environments. However, there is a critical lack of data on the mechanical behavior of alloys of interest for MSRS such as 316H, 617 and 709 in molten fluoride (FLiNaK or FLiBe) or chloride (NaCl-MgCl 2 ) salts. Limited legacy data from the molten salt reactor experiment (MSRE) program showed a significant reduction in creep rupture strength of a Ni-base alloy (Ni-15Cr-7Fe wt.%) in the molten fluoride NaF-ZrF4-UF4 (50-46-4 mol.%) salt. With ongoing efforts to commercialize different molten salt reactor concepts, the industry can considerably benefit from quantitative information on the impact of molten halide salts on the engineering properties such as creep and fatigue strength of materials of interest. Creep tests for 316H were conducted with fluoride (FLiNaK) and chloride (NaCl-MgCl 2 ) salts tat 650°C/150 MPa while alloys 709 and 617 were tested with FLiNaK at 700C/158 MPa and 750C.146 MPa respectively. Baseline tests were conducted in air to assess the impact of the molten salts on the creep behavior.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗