Publications

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Supercritical Carbon Dioxide (S-CO2) is an efficient and flexible working fluid for power production. Research to interface S-CO2 systems with nuclear, thermal solar, and fossil energy sources is currently underway. To proceed, we must address concerns regarding compatibility of materials, at high temperature, and compatibility between significantly different heat transfer fluids. Dry, pure S-CO2 is thought to be relatively inert [1], while the addition of ppm levels of water and oxygen result in formation of a protective chromia layer and iron oxide [2]. Thin oxides are favorable as diffusion barriers, and for their minimal impact on heat transfer. While S-CO2 is typically understood to be the secondary fluid, many varieties of primary fluids exist for nuclear applications. Molten salts, for use in the Molten Salt Reactor concept, are given as an example to contrast the materials requirements of primary and secondary fluids. Thin chromia layers are soluble in molten salt systems (nitrate, chloride, and fluoride based salts) [3-8], making materials selection for heat exchangers a precarious balancing act between high temperature oxidation (S-CO2) and metal dissolution (salt side of heat exchanger). Because concerns have been raised regarding component lifetimes, S-CO2 work has begun to characterize starting materials and to establish a baseline by analysis of 1) as-received stainless steel piping, and 2) piping exposed to S-CO2 under typical operating conditions with Sandia National Laboratories Brayton systems. A second issue discovered by SNL involves substantial erosion in the turbine blade and inlet nozzle. It is believed that this is caused by small particulates that originate from different materials around the loop that are entrained by the S-CO2 to the nozzle, where they impact the inlet nozzle vanes, causing erosion. We believe that, in some way, this is linked to the purity of the S-CO2, the corrosion contaminants, and the metal particulates that are present in the loop and its components.

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Supercritical Carbon Dioxide (S-CO2) is an efficient and flexible working fluid for power production. Research to interface S-CO2 systems with nuclear, thermal solar, and fossil energy sources are currently underway. To proceed, we must address concerns regarding high temperature compatibility of materials and compatibility between significantly different heat transfer fluids. Dry, pure S-CO2 is thought to be relatively inert [1], while ppm levels of water and oxygen result in formation of a protective chromia layer and iron oxide [2] Thin oxides are favorable as diffusion barriers, and for their minimal impact on heat transfer. Chromia, however, is soluble in molten salt systems (nitrate, chloride, and fluoride based salts) [3-8]. Fluoride anion based systems required the development of the alloy INOR-8 (Hastelloy N, base nickel, 17%Mo) [9] to ensure that chromium diffusion is minimized, thereby maximizing the life of containment vessels. This paper reviews the thermodynamic and kinetic considerations for promising, industrially available materials for both salt and S-CO2 systems.

Two classes of materials, poly(methylene diphenyl diisocyanate) or PMDI foam, and cross-linked epoxy resins, were characterized using thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC), to help understand the effects of aging and %E2%80%9Cbake-out%E2%80%9D. The materials were evaluated for mass loss and the onset of decomposition. In some experiments, volatile materials released during heating were analyzed via mass spectroscopy. In all, over twenty materials were evaluated to compare the mass loss and onset temperature for decomposition. Model free kinetic (MFK) measurements, acquired using variable heating rate TGA experiments, were used to calculate the apparent activation energy of thermal decomposition. From these compiled data the effects of aging, bake-out, and sample history on the thermal stability of materials were compared. No significant differences between aged and unaged materials were detected. Bake-out did slightly affect the onset temperature of decomposition but only at the highest bake-out temperatures. Finally, some recommendations for future handling are made.

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High temperature flow sensors must be developed for use with molten salts systems at temperatures in excess of 600ÀC. A novel magneto-hydrodynamic sensing approach was investigated. A prototype sensor was developed and tested in an aqueous sodium chloride solution as a surrogate for molten salt. Despite that the electrical conductivity was a factor of three less than molten salts, it was found that the electrical conductivity of an electrolyte was too low to adequately resolve the signal amidst surrounding noise. This sensor concept is expected to work well with any liquid metal application, as the generated magnetic field scales proportionately with electrical conductivity.

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A secondary containment vessel, made of stainless 316, failed due to severe nitrate salt corrosion. Corrosion was in the form of pitting was observed during high temperature, chemical stability experiments. Optical microscopy, scanning electron microscopy and energy dispersive spectroscopy were all used to diagnose the cause of the failure. Failure was caused by potassium oxide that crept into the gap between the primary vessel (alumina) and the stainless steel vessel. Molten nitrate solar salt (89% KNO{sub 3}, 11% NaNO{sub 3} by weight) was used during chemical stability experiments, with an oxygen cover gas, at a salt temperature of 350-700 C. Nitrate salt was primarily contained in an alumina vessel; however salt crept into the gap between the alumina and 316 stainless steel. Corrosion occurred over a period of approximately 2000 hours, with the end result of full wall penetration through the stainless steel vessel; see Figures 1 and 2 for images of the corrosion damage to the vessel. Wall thickness was 0.0625 inches, which, based on previous data, should have been adequate to avoid corrosion-induced failure while in direct contact with salt temperature at 677 C (0.081-inch/year). Salt temperatures exceeding 650 C lasted for approximately 14 days. However, previous corrosion data was performed with air as the cover gas. High temperature combined with an oxygen cover gas obviously drove corrosion rates to a much higher value. Corrosion resulted in the form of uniform pitting. Based on SEM and EDS data, pits contained primarily potassium oxide and potassium chromate, reinforcing the link between oxides and severe corrosion. In addition to the pitting corrosion, a large blister formed on the side wall, which was mainly composed of potassium, chromium and oxygen. All data indicated that corrosion initiated internally and moved outward. There was no evidence of intergranular corrosion nor were there any indication of fast pathways along grain boundaries. Much of the pitting occurred near welds; however this was the hottest region in the chamber. Pitting was observed up to two inches above the weld, indicating independence from weld effects.