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Assessment of Nuclear Energy to Support Negative Emission Technologies

The feasibility and performance of nuclear energy coupled with Negative Emission Technology (NET) processes were investigated in this report. Three overarching questions from nuclear NET systems guided this research: which NET would be able to use heat and/or electricity from nuclear power plants (NPPs); what is the performance and cost of a nuclear NET system; and what would be the market outlook for this system? Among the various NETs that are actively being developed, several were found to potentially benefit from coupling with an NPP via (1) large amounts of decarbonized and constant-output electricity; (2) free waste heat or cheap low-temperature heat; or (3) high-temperature heat. NPPs were found to be compatible with Direct Air Capture (DAC) systems, and a detailed techno-economic analysis of coupled NPP&DAC systems was performed. Preliminary analysis also indicated that biomass and water-based NETs are potentially compatible with NPPs, but further work is needed to quantify the performance of these nuclear NET systems. Design and performance analyses were completed for both liquid solvent DAC (L-DAC) and solid sorbent DAC (S-DAC) technologies. A 1.0-GWth NPP coupled with L-DAC and S-DAC was found to be able to capture 12–15 Mt CO 2 /yr and 1.0–1.5 Mt CO 2 /yr, respectively. While the L-DAC process enables much greater CO 2 capture than the S-DAC process when both are sized with a 1 GWth NPP, the NPP&L-DAC system considered also requires >2 GWth natural gas oxy-combustion to reach adequate temperature in the calciner. CO 2 generated from natural gas combustion is also captured as part of the calcination process, in addition to the CO 2 captured from air, resulting in overall CO 2 sequestration of close to 30% more than what is captured from air. The cost of carbon capture calculated with the levelized cost of DAC (LCOD) had a range of $\$170–260$/tCO 2 for NPP&L-DAC systems and a range of $\$650–680$/tCO 2 for NPP&S-DAC systems. For both DAC systems, the NPP provides economic benefit when compared to previous National Energy Technology Laboratory (NETL) studies of non-nuclear DAC systems, leading to reduction of LCOD by 5–7% for L-DAC, and 8–13% for S-DAC. For the NPP&DAC systems, a preliminary market analysis reviewed potential CO 2 market prices and eligibility for incentives. The estimated potential revenues for CO 2 capture (coming from federal incentive, CO 2 commodity markets, or offset market) is in the range of $\$170–979$ tCO 2 , and the results show that because of lower LCOD, the NPP&L-DAC process would be more attractive to a market than the NPP&S-DAC process. The large investment needed for NPP&DAC processes would require long-term certainty of sufficient market size, CO 2 prices, and incentives. Enabling NPPs to ramp DAC operation up or down based on electricity market price is not expected to significantly increase revenues of the NPP&DAC system. This is because the revenues from CO 2 sequestration are required to be very high to justify the deployment and continuous operation of the very expensive DAC technologies. In this analysis, several new research questions were uncovered, and follow-up analyses are recommended for further investigation, including a detailed feasibility study of NPP coupled with other NET systems such as biomass pyrolysis and gasification with carbon capture and storage, and seawater carbon capture.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Recyclable Design for Retaining High Solar Absorptivity of the Media in CSP

Efficient thermal energy storage is pivotal to lowering the levelized cost of electricity (LCOE) for Concentrating Solar Power (CSP) plants. In solid-particle systems, however, prolonged high-temperature service degrades particle solar absorptivity, eroding overall efficiency. This project demonstrates a hydrogen-assisted recovery process that reliably restores absorptivity to >90 %, offering a practical route to sustain long-term CSP performance. Bench-scale investigations mapped the reduction kinetics of optically faded particles across hydrogen concentrations, temperatures, and residence times. Coupling mass-spectrometric monitoring with machine-learning optimization minimized energy demand while maximizing absorptivity gain. The resulting process window—moderate hydrogen partial pressures, 15–30 min dwell times, and temperatures well below initial calcination levels—cuts energy consumption well below that of incumbent re-blackening methods. A prototype recovery reactor processed multiple 2 kg batches with repeatable outcomes, confirming scalability and operational robustness. Integrated techno-economic analysis indicates material and operating cost reductions exceeding 15 % relative to conventional particle replacement or chemical re-coating, translating directly into lower LCOE for next-generation CSP facilities. By uniting fundamental reaction-kinetics insight with pragmatic engineering, this work advances the solid-particle pathway, delivering a cost-effective, field-deployable solution to one of CSP’s key durability challenges and strengthening the commercial outlook for high-temperature renewable power.

14 SOLAR ENERGY↗

Role of Wadsley Defects and Cation Disorder to Enhance MoNb 12 O 33 Diffusion

Wadsley-Roth (WR) niobates have emerged as high-rate anode materials that can combine rapid ionic diffusion with good electronic conductivity. WR compounds have been defect-enhanced by limited annealing, however, such materials often contain multiple types of defects. In particular, both Wadsley defects (variable block size) and transition metal disorder have the potential to modify transport rates, however the corresponding effects are not well understood mechanistically. Here, MoNb 12 O 33 (MNO) was calcined at two different temperatures to compare a defect-rich condition (MNO-800) with a proximal order-rich condition (MNO-900) as assessed through XRD, XANES, EXAFS, and STEM characterizations. Galvanostatically cycled lithium half cells of MNO-800 exhibited additional capacity (307 mAhg −1 at 0.1C, 4.66% higher) and improved high-rate capacity of 200 mAhg −1 at 10C. ICI-based overpotential analysis identified solid state diffusion as the dominant rate limiting process where MNO-800 correspondingly exhibited ∼3X faster capacity-weighted diffusivity. A machine-learning interatomic potential was trained to density functional theory and then applied with molecular dynamics (MLIP-MD) to examine the possible roles of Wadsley defects and transition metal disorder. For both defect-types, Li was found to populate and activate fast diffusion paths from window sites at lower extents of lithiation as compared to the order-rich model.

defect↗

Syntheses and Crystal Structures of Rare-Earth Oxyapatites Ca 2 RE 8 (SiO 4 ) 6 O 2 (RE = Pr, Tb, Ho, Tm)

Four different rare-earth oxyapatites of Ca 2 RE 8 (SiO 4 ) 6 O 2 (RE = Pr, Tb, Ho, Tm) were synthesized using a solution-based method followed by drying, calcination, and high-temperature sintering in air. X-ray powder diffraction and Raman spectroscopy were performed on the synthesized oxyapatites. Here, the RE oxyapatites crystallize in the hexagonal space group P6 3 /m with similar unit cell parameters, increasing linearly with larger RE cations. The unit cell volumes increase linearly whereas the densities decrease nonlinearly with larger RE cations. Raman spectra showed intense bands of the symmetric bending and stretching modes of SiO 4 at ~ 400 and 860 cm -1 regions, respectively. The bands generally shifted to higher frequencies with smaller RE cations in the structures.

36 MATERIALS SCIENCE↗

Kinetic assessment of pulp mill-derived lime mud calcination in high CO 2 atmosphere

The chemical pulping of biomass involves the recycling of calcium through the calcination of lime mud, which is mostly comprised of calcium carbonate (CaCO 3 ). Lime mud decomposes under elevated temperatures to generate calcium oxide (CaO) and carbon dioxide (CO 2 ), the kinetics of which are strongly influenced by the CO 2 partial pressure and temperature. Oxy-fuel combustion and electrified lime kilns for lime mud calcination are intriguing methods to decarbonize this highly polluting operation within the biomass pulping industry. However, the high CO 2 concentration in oxy-fuel and electrified calcination processes alters the kinetics and overall reactivity of lime mud. For the first time, a model-fitting method is used to determine the kinetic parameters for lime mud calcination under a wide range of temperatures (550 °C–1250 °C) and under different concentrations of CO2 (0 %, 15 %, 50 %, and 90 %). A kinetic model is developed that accurately predicts the reaction rates as a function of temperature and CO 2 concentration. The apparent activation of energy for lime mud calcination is elevated under a high CO 2 environment. Relative to inert gas (N 2 , Ar), the temperature window for calcination is much smaller under high CO 2 environments. The presence of Na in lime mud does not seem to affect calcination under a high CO 2 environment. Finally, particle size variation does not have a significant effect on calcination under a high CO 2 environment.

09 BIOMASS FUELS↗

Passivation of pigment particles for thermal control coatings

Five powders were received for plasma calcining during this report period. The particle size using a fluid energy mill, and obtained pigments that could be plasma calcined. Optimum results are obtained in the plasma calcining of zinc orthotitanate when finely dispersed particles are subjected to a calculated plasma temperature of 1670 C. Increasing the plasma calcining time by using multiple passes through the plasma stabilized the pigment to vacuum UV irradiation was evidenced by the resulting ESR spectra but slightly decreased the whiteness of the pigment. The observed darkening is apparently associated with the formation of Ti(+3) color centers.

Farley, E. P.↗

Synthetic Calcium Carbonate Production by Carbon Dioxide (CO 2 ) Mineralization of Industrial Waste Brines

The global scale of CO 2 emission has crossed 36 B tons, and the United State represents 14% of the total emissions. In light of the high cost associated with current CO 2 capture processes ($60-to-150 per ton of CO 2 ), carbon capture and utilization (CCU), wherein CO 2 is converted to beneficial products, provides a pragmatic path to overcome the economic barrier for CO 2 emissions control. In particular, CO 2 mineralization offers an attractive route as it produces high-value mineral carbonates that sequester CO 2 in a stable form. For instance, fine precipitated calcium carbonate, a valuable product with unit price in the range of $230-280/t and a global market projected to reach 99 M tons in 2020, can be produced by capturing CO 2 within aqueous Ca 2+ solution. However, two critical challenges need to be overcome—(i) the need for costly processes such as electrolysis or addition of alkali hydroxides to maintain alkalinity during mineralization, and (ii) the geographic availability of Ca-rich solutions (or brines) which often renders efficient integration with power plants impractical. To simultaneously address these challenges, this project developed two novel routes to enable carbonate production based on efficient CO 2 mineralization. In one variation, the project developed a new alkaline carbonation process to capture CO 2 and produce calcite precipitates from coal ashes. Herein, coal ash is carbonated first in a sodium carbonate solution. The carbonation reaction produces sodium hydroxide and raises the solution pH. This high-pH hydroxide solution is then used for CO 2 capture, which converts the sodium hydroxide solution back to sodium carbonate to repeat the carbonation cycle. The carbonated ash residue is refined with a CO 2 pressure swing step to produce high-purity precipitated calcium carbonate. In another variation, Ca-rich produced water brine serves as the Ca-source to mineralize CO 2 . An H + /Na + ion-exchange cycle was designed to provision alkalinity during mineralization and regenerate the ion-exchange reagent in brines with high salinity. Ca-depleted brines can then be treated within a centralized water treatment facility. Both variations beneficially utilize reject streams—such as coal ashes and brines from oil and gas extraction or CO 2 storage operations—that are available at substantial quantities in the vicinity of coal power plants within the U.S. In addition to technology development, this project included techno-economic and life-cycle analysis to identify technically and economically appropriate solutions for power plants in different geographic locations. Taken together, the project provides a unique route to integrate CO 2 emissions control and waste handling/treatment for coal power plants, while producing a high-value product to offset the economic burden associated with waste management. The developed processes utilize post-desulfurization flue gas from coal-fired power plants as is. The CO 2 conversion reactions are performed in alkaline brines at ambient pressure from the flue gas, thereby minimizing the energy burden. By beneficiation of industrial waste streams with low energy input, the processes offers significant technical advantages in energy and CO 2 footprint over the current paradigm of precipitated calcium carbonate production, which involves calcination of limestone at processing temperatures in excess of 800 °C. Overall, this project developed viable CO 2 mineralization processes while strategically maximizing the economic benefit.

01 COAL, LIGNITE, AND PEAT↗

Surface properties of the Orgueil meteorite - Implications for the early history of solar system volatiles

The Kr and H2O adsorption properties of Orgueil were studied. Dehydration by stepwise calcination produced a tenfold change in its B.E.T. surface area, which increased to 120 and then fell to 40 square meters per gram. Water exchangeability was measured by water regain from lab air between calcination cycles. Dehydration at room temperature showed that Orgueil contained 6 per cent by weight of water adsorbed on free surfaces. These results are consistent with an identification of Orgueil as montmorillonite, although chemical data conflict with this. High D/H ratios in CI carbonaceous chondrites may result from D enrichment in OH- groups during equilibration of dispersed phyllosilicate dust with preplanetary nebula gas at temperatures much less than 0 C.

Fanale, F. P.↗

Solid-State High-Temperature Power Cells

All-solid-state electrochemical power cells have been fabricated and tested in a continuing effort to develop batteries for instruments for use in environments as hot as 500 C. Batteries of this type are needed for exploration of Venus, and could be used on Earth for such applications as measuring physical and chemical conditions in geothermal and oil wells, processing furnaces, and combustion engines. In the state-of-the-art predecessors of the present solid-state power cells, fully packaged molten eutectic salts are used as electrolytes. The molten-salt-based cells can be susceptible to significant amounts of self-discharge and corrosion when used for extended times at elevated temperatures. In contrast, all-solid-state cells such as the present ones are expected to be capable of operating for many days at temperatures up to 500 C, without significant self-discharge. The solid-state cell described here includes a cathode made of FeS2, an electrolyte consisting of a crystalline solid solution of equimolar amounts of Li3PO4 and Li4SiO4, and an anode made of an alloy of Li and Si (see figure). The starting material for making the solid electrolyte is a stoichiometric mixture of Li3PO4, SiO2, and Li3CO2. This mixture is ball-milled, then calcined for two hours at a temperature of 1,100 C, then placed in a die atop the cathode material. Next, the layers in the die are squeezed together at a pressure between 60 and 120 MPa for one hour at a temperature of 600 C to form a unitary structure comprising the solid electrolyte and cathode bonded together. Finally, the lithium-alloy anode is pressure-bonded to the solid electrolyte layer, using an intermediate layer of pure lithium. In one test of a cell of this type, a discharge rate of about 1 mA per gram of cathode material was sustained for 72 hours at a temperature of about 460 C. This is about three times the discharge rate required to support some of the longer duration Venus-exploration mission scenarios.

Whitacre, Jay↗

Ceramic encapsulated metal phase change material for high temperature thermal energy storage

Thermal energy storage (TES) is a broad-based technology for reducing CO₂ emissions and advancing concentrating solar, fossil, and nuclear power through improvements in efficiency and economics. Phase change materials (PCMs) are of interest as TES media because of their ability to store large amounts of heat in relatively small volumes. The volume expansion during a phase change, typically between a solid and liquid, can cause breakage of protective coatings. This paper reports on the fabrication of a ceramic encapsulated metal (CEM) high temperature TES technology using a rotary calcining furnace and a fluidized bed chemical vapor deposition coating technique. Aluminum beads were chosen as the PCM because Al has a high melting point (660 °C), low cost, high heat of fusion, and an ability to form a thin, strong alumina layer capable of supporting the Al melt for subsequent processing. Quite remarkably, this study shows that 1 mm diameter Al can be fluidized up to at least 1500 °C in an appropriate atmosphere while maintaining a spheroid geometry. This allowed for producing a first of a kind CEM whereby Al particles were encapsulated in pyro-carbon (PyC) and high purity, dense chemical vapor deposited SiC. The CEM with a PyC only coating was exposed to thermal cycling to test the performance with a differential scanning calorimeter; the melting point and latent heat were measured to be 648.4 ± 2.8 °C and 293.3 ± 6.2 J/g respectively. It was demonstrated that the CEM design is possible to produce, laying the foundation for manufacturing of high temperature, tunable, TES media.

25 ENERGY STORAGE↗

Iron-based sulfur and nitrogen dual doped porous carbon as durable electrocatalysts for oxygen reduction reaction

The widespread use of fuel cell technology is hampered by the use of expensive and scarce platinum metal in electrodes which is required to facilitate the sluggish oxygen reduction reaction (ORR). In this work, a viable synthetic approach was developed to prepare iron-based sulfur and nitrogen dual doped porous carbon (Fe@SNDC) for use in ORR. Benzimidazole, a commercially available monomer, was used as a precursor for N doped carbon and calcined with potassium thiocyanate at different temperatures to tune the pore size, nitrogen content and different types of nitrogen functionality such as pyridinic, pyrrolic and graphitic. The Fe@SNDC–950 with high surface area, optimum N content of about 5 at% and high amount of pyridinic and graphitic N displayed an onset potential and half-wave potential of 0.98 and 0.83 V vs RHE, respectively, in 0.1 M KOH solution. The catalyst also exhibits similar oxygen reduction reaction performance compared to Pt/C (20 wt%) in acidic media. Furthermore, when compared to commercially available Pt/C (20 wt%), Fe@SNDC–950 showed enhanced durability over 6 h and poison tolerance in case of methanol crossover with the concentration up to 3.0 M in oxygen saturated alkaline electrolyte. Finally, our study demonstrates that the presence of N and S along with Fe-N moieties synergistically served as ORR active sites while the high surface area with accessible pores allowed for efficient mass transfer and interaction of oxygen molecules to the active sites contributing to the ORR activity of the catalyst.

08 HYDROGEN↗

Low-Temperature Plasma Treatment for Enhanced Recovery of Highly Valued Critical REEs from Coal (Final Report)

The principle objective of this project was to develop a novel process flowsheet using low-temperature plasma treatment (LTP) integrated with conventional hydrometallurgical processes to recover rare earth elements (REEs), especially highly valued REEs (i.e. scandium and critical REEs), from coal and coal byproducts. LTP treatment was used to pretreat the solid feed material prior to leaching in an effort to improve the leaching characteristics of the REEs and potentially reduce acid consumption. Initially, a detailed experimental program was performed on a laboratory LTP furnace to identify a set of process parameter values to be used for assessing the enhanced leaching performance achieved on four specific gravity fractions of West Kentucky No. 13 and Fire Clay coarse coal refuse materials. High-temperature oxidation (HTO)) was also evaluated as a means for improving REE leachability on the same fractions of both coal sources. The lixiviants used to assess leachability improvements included: i) untreated water, ii) 0.1 M ammonium sulfate solution and iii) 1.2 M sulfuric acid solution at a temperature of 75°C. The laboratory data was used to develop multiple process flow sheets using HTO only to produce a rare earth oxide mix concentrate or utilizing both LTP and HTO treatment processes to generate a high purity heavy REO mix concentrate and a light REO mix concentrate. A techno-economic analysis was performed on each circuit. Low-temperature plasma oxidation was found to enhance REE leaching characteristics for all specific gravity (SG) fractions of the West Kentucky No. 13 coarse refuse material. The leaching recovery improvement was preferentially achieved for the heavy REEs with higher values obtained when treating the lower density fraction material. For example, the leaching recovery for the heavy REEs in the untreated 1.6 SG Float fraction material was 8% in a 0.1 M ammonium sulfate solution. After LTP treatment for 32 hours, heavy REE recovery increased to 33%. The corresponding recovery value for the light REEs was 10%. These findings indicate a strong affinity of the heavy REEs with the organic material, which is the component being reduced in content during the LTP treatment. Scanning electron micrographs showed the development of a honeycomb structure with increased LTP treatment with higher surface area as confirmed from BET measurements. Higher surface area promotes improved leaching efficiency due to enhance chemical interactions. When using 1.2 M sulfuric acid, the LTP treatment was found to provide a heavy REE recovery increase from 23% to 53% for the 1.6 SG Float fraction which corresponded to an ash content increase from around 20% to 35%. However, LTP treatment provided no improvement in leaching characteristic for the 2.2 SG sink material in the acid solution, which was likely due to the low organic content. The LTP treatment of the Fire Clay SG fractions provided no improvement in REE leaching characteristic, which may be due to the association with REE minerals such as monazite and REE-associated mineral matter such as clays. High temperature oxidation using temperatures in the range of 600-750OC was found to significantly enhance the leaching characteristics of both the light and heavy REEs for all density fractions in both coarse coal refuse materials. Generally, the increase in light REE recovery for the West Kentucky material was from 15% for the untreated material to 90% for the HTO treated material at 600°C. Recovery values dropped significantly when using temperatures below 600°C and above 750°C. The impact of the excessive temperatures was most likely a result of sintering. For the heavy REEs, HTO significantly improved recovery in the lighter SG fractions, which may be due to an affinity with the organic content. Only limited heavy REE recovery improvement was obtained for the denser SG fractions. Another benefit of HTO is the conversion of calcium-based minerals to a very soluble calcium oxide, which is removable using a mild acid solution, and the conversion of Fe minerals to relatively insoluble minerals such as hematite and magnetite. The pregnant leaching solution produced from the leaching of all SG fractions obtained from both coal sources was treated using two stages of solvent extraction procedurally modeling a rougher-cleaner circuit followed by oxalic acid precipitation. Rare earth oxide products having a purity greater than 97% was produced from nearly all of the SG fractions. A novel process flowsheet was developed based on the selective leaching of heavy REEs that was made possible through LTP treatment of West Kentucky No. 13 coarse refuse followed by salt leaching. In the flowsheet, coal refuse material is ground to a top size of 1mm and then treated by LTP. The treated material is mixed into a 0.1 M ammonium sulfate solution and then filtered to produce a heavy REE enriched pregnant leach solution. The heavy REEs are concentrated by two stages of selective precipitation to produce a heavy REE mix oxalate and then roasted to obtain a heavy REO mix concentrate. The solid residues remaining after salt leaching is dried and then subjected to HTO treatment followed by concentration using selective precipitation and roasting to produce a light REO mix concentrate. An alternative circuit was developed using HTO treatment only to treat 100% of the coarse refuse material followed by selective precipitation and roasting to generate a high purity REO mix product. A techno-economic analysis performed for the treatment of West Kentucky No. 13 and Fire Clay coarse refuse based on a hypothetical 500-tph plant revealed that the net present value for all scenarios was significantly negative. Primary reasons include: i) a substantial decrease in the basket value of the final product relative to the feed and ii) high chemical costs relative to the amount of product generated. The basket value reduction was primarily due to little to no scandium recovery due to poor leaching characteristics when using low acid concentrations as necessitated by the low feed grades. Operating costs were primarily influenced by the chemical costs relative to the kilograms of concentrate produced and feed grade. For the Fire Clay coarse refuse material, the total operating cost was estimated to be $354 per kg of REO produced which was higher than the basket value of the REO product ($276/kg). Approximately 37% of the total cost was the sulfuric acid used during the leaching process. A comparative analysis performed to assess the economic viability of using low-temperature plasma furnaces found that market value enhancement for the generation of both heavy REO and light REO concentrates will be needed in addition to significant technology advancements to reduce the cost of plasma furnaces.

01 COAL, LIGNITE, AND PEAT↗

CuCr 2 O 4 particle growth and evolution across sol–gel routes and calcination profiles

CuCr 2 O 4 spinel is a candidate coating material for central receivers in concentrating solar power to protect structural alloys against high temperature oxidation and related degradation. Coating performance and microstructure of dip-coated and sintered coatings is dictated by the initial particle size of the CuCr 2 O 4 and sintering temperature, but can be compromised by particle agglomeration. Here in this study, sub-micron particles were synthesised through the Pechini and modified Pechini sol–gel methods. Phase composition was confirmed via X-ray diffraction. Particle growth during calcination of the nanoparticles at different temperatures (650°C, 750°C, 850°C) and times (between 1 and 24 h) was measured via laser diffraction and scanning electron microscopy. The modified Pechini method displayed evidence of smaller particle sizes and greater agglomeration. The kinetics of particle growth observed are consistent with a diffusion limited inhibited grain growth model.

36 MATERIALS SCIENCE↗

Development of high Tc (greater than 100 K) Bi, Tl and Y-based materials as superconducting circuit elements

Experimental work on this project over the last four years has resulted in establishing processing and characterization techniques for producing both the Bi-based and Tl-based superconductors in their high temperature (2223) forms. In the bulk, dry pressed form, maximum critical temperatures (Tc) of 108.2 K and 117.8 K, respectively, were measured. Results have further shown that the Bi and Tl-based superconducting materials in bulk form are noticeably different from the Y-based 123 material in that superconductivity is considerably harder to achieve, maintain, and reproduce. This is due primarily to the difficulty in obtaining the higher Tc phase in pure form since it commonly co-exists with other undesirable, lower Tc phases. In particular, it has been found that long processing times for calcining and firing (20 - 200 hrs.) and close control of temperatures which are very near the melting point are required in order to obtain higher proportions of the desirable, high Tc (2223) phase. Thus far, the BSCCO bulk materials has been prepared in uniaxially pressed, hot pressed, and tapecast form. The uniaxially pressed material has been synthesized by the mixed oxide, coprecipitation, and melt quenching processes. The tapecast and hot pressed materials have been prepared via the mixed oxide process. In addition, thick films of BSCCO (2223 phase) have been prepared by screen printing on to yttria and magnesia stabilized zirconia with only moderate success; i.e., superconductivity was achieved in these thick films, but the highest Tc obtained in these films was 89.0 K. The Tc's of the bulk hot pressed, tapecast, and screen printed thick film materials were found to be 108.2, 102.4, and 89.0 K, respectively.

Haertling, Gene↗

A pilot-process for calcium hydroxide production from iron slag by low-temperature precipitation

The production of Ca(OH) 2 via thermal decomposition of limestone is an energy intensive process resulting in significant CO 2 emissions. However, if produced in a manner that obviates the need for the thermal decomposition of limestone, Ca(OH) 2 could be a “CO 2 -negative” material. Herein, we design and demonstrate the operation of a continuous, low-temperature (< 100 °C), aqueous-phase pilot-process to produce Ca(OH) 2 using calcium extracted from alkaline industrial wastes. The three-step process encompasses unit operations including: (i) calcium leaching from basic oxygen furnace BOF slag, (ii) leachate concentration by reverse osmosis (RO), and (iii) Ca(OH) 2 precipitation by temperature swing. Here this process presents several advantages compared to the traditional route. First, it advances the recycling of waste from the steel industry. Second, it operates significantly below the temperature used in conventional lime production (900 °C) as it bypasses limestone calcination, responsible for ~65% of the CO 2 emissions from the current process. Thus, the new process has a lower CO 2 footprint and enables the use of industrial waste heat. The mass and energy balances were quantified to reveal that increasing the calcium concentration of the feed solution and the precipitation temperature, decrease the energy demands of the RO step, thereby reducing the process’s overall CO 2 footprint. The pilot system operated continuously and achieved a production rate of nearly 1 kg per day of Ca(OH) 2 with a purity greater than 95 wt%. The average particle size of the precipitates depended on the residence time in the precipitation reactor, demonstrating an ability to produce size-controlled particulates. Importantly, the process achieved full water recirculation/reutilization level indicative of a low-consumable water demand. The outcomes offer new insights and understanding relevant to developing and upscaling low-CO 2 processes for cement, lime, and portlandite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Preparation and Characterization of YBa 2 Cu 4 O 8 Superconductor

Solid-state reaction of appropriate amounts of Y 2 O 3 , BaCOs, and CuO for 2 h at 800°C in flowing oxygen with a total pressure of 2.7 x 10 2 Pa (2 mm Hg), followed by cooling and annealing at 750°C for 10 h in oxygen at ambient pressure, has produced orthorhombic YBa 2 Cu 4 O 8 (124) as the main phase with YBa 2 Cu 3 O x (123) as an impurity phase. After the as-calcined powder was annealed in oxygen at 800°C for 24 h under ambient pressure, the phase purity improved considerably. Calcined 124 powder was pressed into pellets and rapidly annealed at temperatures from 870°C to 935°C. At these temperatures, the 124 decomposed into 123. The superconducting transition temperature, T c , of the annealed samples depended upon the annealing temperature and atmosphere. The decomposed samples have been characterized by low field RF SQUID magnetometer and high resolution transmission electron microscopy.

36 MATERIALS SCIENCE↗

Space stable thermal control coatings

Both pigment and paint studies were conducted to determine the effect of calcination conditions on optical properties of Zn2TiO4. Paint studies were concerned with the effects of spraying technique, of pigment to binder ratio, and of thickness on the properties of finished coatings. The results are reviewed in detail. Pigments prepared by calcination at 600 deg. to 800 deg. were evaluated. Low temperature syntheses were conducted to determine; (1) extent of ZnO + TiO2 reaction; and (2) the potential of higher peak reflectance with finer particle size powder obtained at lower temperatures.

Harada, Y.↗