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High-strength silicon carbides by hot isostatic pressing
Silicon carbide has strong potential for heat engine hardware and other high-temperature applications because of its low density, good strength, high oxidation resistance, and good high-temperature creep resistance. Hot isostatic pressing (HIP) was used for producing alpha and beta silicon carbide (SiC) bodies with near-theoretical density, ultrafine grain size, and high strength at processing temperatures of 1900 to 2000 C. The HIPed materials exhibited ultrafine grain size. Furthermore, no phase transformation from beta to alpha was observed in HIPed beta-SiC. Both materials exhibited very high average flexural strength. It was also shown that alpha-SiC bodies without any sintering aids, when HIPed to high final density, can exhibit very high strength. Fracture toughness K (sub C) values were determined to be 3.6 to 4.0 MPa m (sup 1/2) for HIPed alpha-SiC and 3.7 to 4.1 MPa m (sup 1/2) for HIPed beta-SiC. In the HIPed specimens strength-controlling flaws were typically surface related. In spite of improvements in material properties such as strength and fracture toughness by elimination of the larger strength-limiting flaws and by grain size refinement, HIPing has no effect on the Weibull modulus.
High-strength silicon carbides by hot isostatic pressing
Silicon carbide has strong potential for heat engine hardware and other high-temperature applications because of its low density, good strength, high oxidation resistance, and good high-temperature creep resistance. Hot isostatic pressing (HIP) was used for producing alpha and beta silicon carbide (SiC) bodies with near-theoretical density, ultrafine grain size, and high strength at processing temperatures of 1900 to 2000 C. The HIPed materials exhibited ultrafine grain size. Furthermore, no phase transformation from beta to alpha was observed in HIPed beta-SiC. Both materials exhibited very high average flexural strength. It was also shown that alpha-SiC bodies without any sintering aids, when HIPed to high final density, can exhibit very high strength. Fracture toughness K (sub C) values were determined to be 3.6 to 4.0 MPa m (sup 1/2) for HIPed alpha-SiC and 3.7 to 4.1 MPa m (sup 1/2) for HIPed beta-SiC. In the HIPed specimens strength-controlling flaws were typically surface related. In spite of improvements in material properties such as strength and fracture toughness by elimination of the larger strength-limiting flaws and by grain size refinement, HIPing has no effect on the Weibull modulus.
Effusion Cell Measurements of the Vapor Pressure of Cobalt at Temperatures up to 2000K; Comparisons with Iron and Nickel
It has become increasingly clear over the past decade that high temperature processes played important roles in the Primitive Solar Nebula. Unfortunately, basic data, such as the vapor pressures of Fe, Ni, Co or SiO have not been measured over the appropriate temperature range (near T approx. 2000K), but must be extrapolated from lower temperature measurements often made more than 50 years ago. The extrapolation of the available data to higher temperatures can be quite complex (e.g., see [1] for SiO vapor pressures) and can depend on other factors such as the oxygen fugacity or the presence of hydrogen gas not accounted for in the original measurements. Moreover, modern technology has made possible more accurate measurements of such quantities over a wider temperature range. We have acquired a commercial Thermo-Cahn Thermogravimetric system capable of vacuum operation to 1700C and measurement of a 10g change in sample mass using up to a 100g sample, with microgram accuracy. With this new system we have initiated a series of basic vapor pressure measurements on simple metals such as Fe[2] and Ni[3] with the intention to extend such measurements to more complex systems once we gain sufficient experience.
Vacuum Sintering of Highland Simulant CSM-LHT-1G
Sintering of lunar regolith is a process of interest to consolidate the ubiquitous granular material in durable structures on the lunar surface such as platforms, landing/launch pads, roads, and foundations for long-term robotic and human activities. Many publications do not report quantitative assessment of the effects of processing conditions on the strength properties of the sintered products. The work presented is an investigation into such effects on a carefully selected simulant, CSM-LHT-1G prepared for high temperature processing to eliminate undesired components that would not be present from lunar materials. Careful experiments under vacuum were conducted to identify the relevant factors that dominate the properties and the quality of the sintered product. CSM-LHT-1G simulant is a variant of the CSM-LHT-1 lunar highland simulant produced by Colorado School of Mines. The original mineralogical composition of CSM-LHT-1 (70 wt.% Greenspar, 30 wt.% Merriam Crater basalt) was modified to obtain a 30 wt.% glass content with the addition of NU-LHT-5M glass balanced with pyroxene (augite) to yield CSM-LHT-1G.
Finned Carbon-Carbon Heat Pipe with Potassium Working Fluid
This elemental space radiator heat pipe is designed to operate in the 700 to 875 K temperature range. It consists of a C-C (carbon-carbon) shell made from poly-acrylonitride fibers that are woven in an angle interlock pattern and densified with pitch at high process temperature with integrally woven fins. The fins are 2.5 cm long and 1 mm thick, and provide an extended radiating surface at the colder condenser section of the heat pipe. The weave pattern features a continuous fiber bath from the inner tube surface to the outside edges of the fins to maximize the thermal conductance, and to thus minimize the temperature drop at the condenser end. The heat pipe and radiator element together are less than one-third the mass of conventional heat pipes of the same heat rejection surface area. To prevent the molten potassium working fluid from eroding the C C heat pipe wall, the shell is lined with a thin-walled, metallic tube liner (Nb-1 wt.% Zr), which is an integral part of a hermetic metal subassembly which is furnace-brazed to the inner surface of the C-C tube. The hermetic metal liner subassembly includes end caps and fill tubes fabricated from the same Nb-1Zr alloy. A combination of laser and electron beam methods is used to weld the end caps and fill tubes. A tungsten/inert gas weld seals the fill tubes after cleaning and charging the heat pipes with potassium. The external section of this liner, which was formed by a "Uniscan" rolling process, transitions to a larger wall thickness. This section, which protrudes beyond the C-C shell, constitutes the "evaporator" part of the heat pipe, while the section inside the shell constitutes the condenser of the heat pipe (see figure).
Indigenous lunar construction materials
The utilization of local resources for the construction and operation of a lunar base can significantly reduce the cost of transporting materials and supplies from Earth. The feasibility of processing lunar regolith to form construction materials and structural components is investigated. A preliminary review of potential processing methods such as sintering, hot-pressing, liquification, and cast basalt techniques, was completed. The processing method proposed is a variation on the cast basalt technique. It involves liquification of the regolith at 1200-1300 C, casting the liquid into a form, and controlled cooling. While the process temperature is higher than that for sintering or hot-pressing (1000-1100 C), this method is expected to yield a true engineering material with low variability in properties, high strength, and the potential to form large structural components. A scenario for this processing method was integrated with a design for a representative lunar base structure and potential construction techniques. The lunar shelter design is for a modular, segmented, pressurized, hemispherical dome which could serve as habitation and laboratory space. Based on this design, estimates of requirements for power, processing equipment, and construction equipment were made. This proposed combination of material processing method, structural design, and support requirements will help to establish the feasibility of lunar base construction using indigenous materials. Future work will refine the steps of the processing method. Specific areas where more information is needed are: furnace characteristics in vacuum; heat transfer during liquification; viscosity, pouring and forming behavior of molten regolith; design of high temperature forms; heat transfer during cooling; recrystallization of basalt; and refinement of estimates of elastic moduli, compressive and tensile strength, thermal expansion coefficient, thermal conductivity, and heat capacity. The preliminary design of the lunar shelter showed us that joining is a critical technology needed for building a structure from large segments. The problem of joining is important to the design of any structure that is not completely prefabricated. It is especially important when the structure is subjected to tensile loading by an internal pressure. For a lunar shelter constructed from large segments the joints between these large segments must be strong, and they must permit automated construction. With a cast basalt building material which is brittle, there is the additional problem of connecting the joint with the material and avoiding stress concentration that would cause failure. Thus, a well-defined project which we intend to pursue during this coming year is the design of joints for cast basalt structural elements.
Opportunities for Solar Industrial Process Heat in the United States
Energy used in the production and processing of materials and products represents a significant fraction of the overall energy footprint of the industrial sector. Solar technologies may provide suitable alternative to existing combustion technologies, but their relevance for industries in the United States has been largely unexplored at the necessary levels of spatial, temporal, and operational detail. To provide the first assessment of the technical opportunities for solar technologies to meet the demand for process heat in the United States, we first develop estimates of energy use by process temperature at the county and hourly resolutions for all manufacturing industries. We then estimate the opportunities for seven solar technology packages—comprised of solar thermal and photovoltaic-connected electrotechnologies—to meet process heat demand given solar resources and available land area by county.
Solar cell comprising an oxide-nanoparticle buffer layer and method of fabrication
A buffer layer for protecting an organic layer during high-energy deposition of an electrically conductive layer is disclosed. Buffer layers in accordance with the present invention are particularly well suited for use in perovskite-based single-junction solar cells and double-junction solar cell structures that include at least one perovskite-based absorbing layer. In some embodiments, the buffer layer comprises a layer of oxide-based nanoparticles that is formed using solution-state processing, in which a solution comprising the nanoparticles and a volatile solvent is spin coated onto a structure that includes the organic layer. The solvent is subsequently removed in a low-temperature process that does not degrade the organic layer.
Evaluation of Tungsten—Steel Solid-State Bonding: Options and the Role of CALPHAD to Screen Diffusion Bonding Interlayers
Critical aspects of innovative design in engineering disciplines like infrastructure, transportation, and medical applications require the joining of dissimilar materials. This study investigates the literature on solid-state bonding techniques, with a particular focus on diffusion bonding, as an effective method for establishing engineering bonds. Welding and brazing, while widely used, may pose challenges when joining materials with large differences in melting temperature and can lead to mechanical property degradation. In contrast, diffusion bonding offers a lower temperature process that relies on solid-state interactions to develop bond strength. The joining of tungsten and steel, especially for fusion reactors, presents a unique challenge due to the significant disparity in melting temperatures and the propensity to form brittle intermetallics. Here, diffusion characteristics of tungsten–steel interfaces are examined and the influence of bonding parameters on mechanical properties are investigated. Additionally, CALPHAD modeling is employed to explore joining parameters, thermal stability, and diffusion kinetics. The insights from this research can be extended to join numerous dissimilar materials for specific applications such as aerospace, automobile industry, power plants, etc., enabling advanced and robust design with high efficiency.
Ambient Rare Earth Metal Electrodeposition in Nitrogen-Coordinated Silylamide Electrolyte
The transition to a sustainable, low-carbon economy demands energy-efficient and environmentally benign methods for rare earth metal (REM) production. Furthermore, while high-temperature molten salt electrolysis remains energy-intensive, corrosive, and environmentally unfriendly, emerging room-temperature processes based on conventional ionic liquids are also hindered by high viscosity and chemical instability. In this study, a nitrogen-coordinated, water-, oxygen-, and fluorine-free silylamide-based electrolyte is presented as a promising system for room-temperature REM electrodeposition. Derived from commercially available lithium silylamide precursors, the system enables facile synthesis, broad electrochemical stability, and tunable metal–ligand interactions. Electrochemical analysis reveals high voltammetric stripping reversibility, stable cathodic and anodic potentials, and selective neodymium (Nd) deposition at appreciable current densities (>1 mA/cm 2 ), with minimal parasitic reactions. Bulk experiments produced high-purity Nd with reproducible performance across multiple batches. Scaled deposition yielded over 1 g of Nd with near-theoretical mass efficiency (0.40 mg/C) and >90% purity. Using sacrificial dysprosium (Dy) and Nd metal anodes, the system maintained constant Nd loading during extended deposition and enabled cathodic codeposition of stripped anode material, demonstrating the electrolyte’s dual functionality for REM electrorefining. Collectively, this silylamide platform offers a compelling combination of electrochemical robustness, chemical resilience, and process scalability for sustainable ambient REM recovery.
Implementation of a Model Predictive Control Strategy to Regulate Temperature Inside Plug-Flow Solar Reactor With Countercurrent Flow
Abstract Solar-driven thermochemical energy storage systems are proven to be promising energy carriers (solar fuels) to utilize solar energy by using reactive solid-state pellets. However, the production of solar fuel requires a quasi-steady-state process temperature, which represents the main challenge due to the transient nature of solar power. In this work, an adaptive model predictive controller (MPC) is presented to regulate the temperature inside a tubular solar reactor to produce solid-state solar fuel for long-term thermal storage systems. The solar reactor system consists of a vertical tube heated circumferentially over a segment of its length by concentrated solar power, and the reactive pellets (MgMn2O4) are fed from the top end and flow downwards through the heated tube. A countercurrent flowing gas supplied from the lower end interacts with flowing pellets to reduce it thermochemically at a temperature range of 1000—1500 °C. A low-order physical model was developed to simulate the dynamics of the solar reactor including the reaction kinetics, and the proposed model was validated numerically by using a 7-kW electric furnace. The numerical model then was utilized to design the MPC controller, where the control system consists of an MPC code linked to an adaptive system identification code that updates system parameters online to ensure system robustness against external disturbances (sudden change in the flow inside the reactor), model mismatches, and uncertainty. The MPC controller parameters are tuned to enhance the system performance with minimum steady-state error and overshoot. The controller is tested to track different temperature ranges between 500 °C and 1400 °C with different particles/gas mass flowrates and ramping temperature profiles. Results show that the MPC controller successfully regulated the reactor temperature within ± 1 °C of its setpoint and maintained robust performance with minimum input effort when subjected to sudden changes in the amount of flowing media and the presence of chemical reaction.
Comparison of AMZIRC and GRCop-84
The mechanical properties of two copper alloys with high thermal conductivity, GRCop-84 and AMZIRC, were compared. These are competing alloys in high temperature, high heat flux applications such as rocket nozzles. The GRCop-84 data presented was taken from previous work. The results of new tensile, creep, and compression tests on AMZIRC are presented. Tests were done on as-received hard drawn material, and on material that had been subjected to a heat treatment designed to simulate a brazing operation at 935 C. As-received AMZIRC was found to have excellent properties at temperatures below 550 C, with room temperature yield and ultimate tensile strengths of about 500 MPa, and ductile failures. By comparison, GRCop-84 s room temperature tensile yield and ultimate strengths are about 200 and 380 MPa respectively. However, the simulated brazing heat treatment substantially decreased the mechanical properties of AMZIRC; and the strength of as-received AMZIRC dropped precipitously as test temperatures exceeded 500 C. The properties of GRCop-84 were not significantly affected by the 935 C heat treatment. As a result, there appear to be advantages to GRCop- 84 over AMZIRC if use or processing temperatures of greater than 500 C are expected. Tensile creep tests were done at 500 and 650 C. At these temperatures, the creep properties of GRCop-84 were superior to AMZIRC s. At equivalent rupture life and stress, GRCop-84 was found to have a 150 C temperature advantage over AMZIRC; for equivalent rupture life and temperature GRCop-84 was two times stronger.
Thermal Evolution of Internal Strain in Doped PbTe
Recent improvements in the efficiency of heat-to-electricity energy conversion in lead chalcogenide thermoelectrics involve reducing the thermal conductivity by incorporating large amounts of internal strain. The extent to which typical lead chalcogenide processing techniques (such as doping, ball milling, and densification) increase internal strain and dislocation density must be quantified to improve materials design. In this study, neutron powder diffraction is leveraged to evaluate the internal strain introduced by ball milling in doped and undoped powders. Doping with Na and/or Eu increases internal strain beyond ball milling alone, with the greatest increase from combining the two dopants. Strain recovery occurs in each powder above 400 K but can be suppressed by co-doping, indicating a strong dopant–dislocation interaction in this system. Therefore, high-temperature processing of PbTe powders should be avoided if high internal strain is desired. Low-temperature densification and/or rapid pressing techniques may be key to maintaining internal strain in the final pressed pellet. The diffraction peak asymmetry and correlated elastic softening measured in pressed PbTe pellets in past studies were not observed in the precursor powders measured here, suggesting that measurements of the Debye temperature on final pressed pellets are required to examine the influence of defect-induced elastic softening on thermal conductivity. This work provides key guidance for defect engineering to maximize internal strain and thermoelectric performance in PbTe thermoelectrics.
Approaches to New Endcaps for Improved Oxidation Resistance
Norbornenyl-end capped PMR polyimide resins are widely used as polymer matrix composite materials for aircraft engine applications, since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a two-step approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, for PMR- 15. The end cap facilitates processing by controlling the molecular weight of the oligomer and allowing flow before it cross-links. However, after cross-linking, this very end cap accounts for much of the weight loss in the polymer on aging in air at elevated temperatures. Understanding this degradation provides clues for designing new end caps to slow down degradation, and prolong the lifetime of the material.
Reduced synthesis temperatures of SrNbO 2 N perovskite films for photoelectrochemical fuel production
Perovskite oxynitrides, such as SrNbO 2 N, have been shown to be promising materials for photoanodes in tandem photoelectrochemical cells, due to their suitable bandgap and charge transport. However, thin film synthesis and characterization of oxynitride perovskites are challenging due to high processing temperatures that are incompatible with available substrates. In this work, we report on reduced synthesis temperatures of SrNbO 2 N perovskite thin films on Si substrates across a range of chemical compositions. Polycrystalline thin films with perovskite crystal structure are obtained by sputtering at ambient temperature and annealing at 550-600 degrees C. The perovskite structure has a relatively broad range of cation composition between 50 and 60% Sr with varying O/N ratio according to Rutherford backscattering spectrometry. The maximum photocurrent density was obtained at 55 cation % of Sr, which is slightly Sr-rich compared to the nominal SrNbO 2 N stoichiometry. This work shows the importance of considering cation and anion composition in studying oxynitride perovskites for solar fuel applications.
Energy Requirements for Integration of Nuclear Reactors with Iron and Steel Plants
This report identifies energy needs of heavy energy users within the domestic iron and steel industry and suggests solutions for integrating nuclear energy. The iron and steel industry, composed of several types of plants which perform different processes with varied energy demands and vectors, is a heavy consumer of electric power and fossil fuels including coke and natural gas. Almost all major process temperatures exceed the temperatures of direct heat available from advanced reactors, and so electricity and hydrogen were considered instead. Reference units were adopted and estimated energy demands computed for the blast furnace (BF), direct reduced iron (DRI) unit, electric arc furnace (EAF), and reheat furnaces. By utilizing production capacity data from industry reports, the ranges of power demands were estimated, including for hydrogen production by high temperature steam electrolysis (HTSE). For the EAF and DRI unit, more detailed integration studies with thermodynamic modeling were also conducted and determined a possible solution with a specific reactor design and number of modules. Furthermore, because many unit processes are co-located, entire plants were considered by adding the energy demands of the unit processes to form four hypothetical reference plants. The range of power needs for the reference plants is compatible with multi-unit banks of microreactors at the low end, and would create a need for multiple larger-capacity SMRs at the high end (1 GWe plus 0.14 GWt). Although the overall power need at the high end is well-matched with one present-day large reactor offering (1.1 GWe), redundancy considerations may require a minimum of two reactors, potentially eliminating the single large reactor from consideration. Auxiliary or house loads would increase the reference plant estimates. Finally, the report provides total estimated energy needs under integration of all U.S. units of each process (BF, DRI, EAF, and reheat furnaces), representing a national potential for nuclear energy in the industry. U.S. iron and steel plants may be candidates for integration with nuclear reactors via electricity and hydrogen, and many sites have energy requirements that correspond well to the capacities of several advanced nuclear power designs.
Fiber-Optic Temperature Sensor Using a Thin-Film Fabry-Perot Interferometer
A fiber-optic temperature sensor was developed that is rugged, compact, stable, and can be inexpensively fabricated. This thin-film interferometric temperature sensor was shown to be capable of providing a +/- 2 C accuracy over the range of -55 to 275 C, throughout a 5000 hr operating life. A temperature-sensitive thin-film Fabry-Perot interferometer can be deposited directly onto the end of a multimode optical fiber. This batch-fabricatable sensor can be manufactured at a much lower cost than can a presently available sensor, which requires the mechanical attachment of a Fabry-Perot interferometer to a fiber. The principal disadvantage of the thin-film sensor is its inherent instability, due to the low processing temperatures that must be used to prevent degradation of the optical fiber's buffer coating. The design of the stable thin-film temperature sensor considered the potential sources of both short and long term drifts. The temperature- sensitive Fabry-Perot interferometer was a silicon film with a thickness of approx. 2 microns. A laser-annealing process was developed which crystallized the silicon film without damaging the optical fiber. The silicon film was encapsulated with a thin layer of Si3N4 over coated with aluminum. Crystallization of the silicon and its encapsulation with a highly stable, impermeable thin-film structure were essential steps in producing a sensor with the required long-term stability.