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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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161 records · Page 9
All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Sintering of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) with/without SrTiO3 Dopant

The perovskite composition, BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta), displays excellent protonic conduction at high temperatures making it a desirable candidate for hydrogen separation membranes. This paper reports on the sintering behavior of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders doped with SrTiO3. Two methods were used to synthesize BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders: (1) solid state reaction and (2) wet chemical co-precipitation. Co-precipitated powder crystallized into the perovskite phase at 1000 C for 4 hrs. Complete reaction and crystallization of the perovskite phase by solid state was achieved by calcining at 1200 C for 24 hrs. Solid state synthesis produced a coarser powder with an average particle size of 1.3 microns and surface area of 0.74 sq m/g. Co-precipitation produced a finer powder with a average particle size of 65 nm and surface area of 14.9 sq m/g. Powders were doped with 1, 2, 5, and 10 mole % SrTiO3. Samples were sintered at 1450 C, 1550 C and 1650 C. SrTiO3 enhances sintering, optimal dopant level is different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior. Dopant levels of 5 and 10 mole % SrTiO3 significantly enhances the grain size.

Dynys, F.↗
DOE OSTI2023

Highly Active and Stable Single Atom Rh 1 /CeO 2 Catalyst for CO Oxidation during Redox Cycling

We report a single atom Rh 1 /CeO 2 catalyst prepared by the high temperature (800 °C) atom trapping (AT) method which is stable under both oxidative and reductive conditions. Infrared spectroscopic and electron microscopy characterization revealed the presence of exclusively ionic Rh species. These ionic Rh species are stable even under reducing conditions (CO at 300 °C) due to the strong interaction between Rh and CeO 2 achieved by the AT method, leading to high and reproducible CO oxidation activity regardless of whether the catalyst is reduced or oxidized. In contrast, ionic Rh species in catalysts synthesized by a conventional impregnation approach (e. g., calcined at 350 °C) can be readily reduced to form Rh nanoclusters/nanoparticles, which are easily oxidized under oxidative conditions, leading to loss of catalytic performance. The single atom Rh 1 /CeO 2 catalysts synthesized by the AT method do not exhibit changes during redox cycling hence are promising catalysts for emission control where redox cycling is encountered, and severe oxidation (fuel cut) leads to loss of performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Influence of residual chlorine on Ru/TiO 2 active sites during CO 2 methanation

Titania-supported ruthenium (Ru/TiO 2 ) is an established catalyst for the hydrogenation of carbon dioxide to methane (Sabatier reaction). Chlorine contamination, owed to the RuCl 3 precursor, is demonstrated to have a detrimental impact on methanation activity. After calcination and reduction the catalyst contains residual chlorine, shown by XPS. An aqueous ammonia wash removes Cl without leaching Ru. The washed catalysts exhibit improvements in CH 4 site-time yields. Low Ru loading catalysts encounter the greatest activity enhancements after washing (~4.5-fold). DFT calculations indicate that chlorine and CO 2 directly compete for adsorption on Ru step sites, with Cl impeding the adsorption of CO 2 at under-coordinated sites and at higher Cl coverages. H 2 -chemisorption/TPR show that Cl removal lowers the onset of low temperature H 2 dissociation on Ru. Finally, DRIFTS provide evidence that the removal of Cl facilitates low temperature dissociative binding of CO 2 , indicated by the formation of surface bound linear CO species.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1994

Hematite formed from pyroxene on Mars by meteoritic impact

In earlier work, we showed using Mossbauer data that the mineralogy of iron-bearing phases in impact melt rocks from Manicouagan Crater (Quebec, Canada) is to a first approximation hematite and pyroxene. The visible and near-IR reflectivity data for these impact melt rocks show a continuous trend in band position from approximately 850 to approximately 1000 nm, which corresponds to the positions for the hematite and pyroxene endmembers, respectively. The oxidation is thought to occur shortly after the impact when oxidizing vapors and/or solutions reacted with the impact melt which was below its solidus temperature but still relatively hot. The reflectance data have important implications for Mars because band positions which occur between approximately 850 and 1000 nm bands observed for Mars can be attributed to hematite-pyroxene assemblages and not necessarily to different ferric mineralogy. Because oxidation of impact melt rocks at Manicouagan is thought to occur subsolidus, precursors for the hematite include oxides such as magnetite and ilmenite and silicates such as pyroxene and olivine. To determine if the Manicouagan impact-melt rocks are related to each other by simple thermal subsolidus oxidation, we calcined in air a relatively unoxidized Manicouagan impact-melt rock (MAN-74-608A). Previous work has shown that np-Hm (nanophase hematite) particles can be derived by calcination of iron-bearing silicates.

Morris, Richard V.↗
DOE OSTI2021

Fischer-Tropsch Synthesis: The Characterization and Testing of Pt-Co/SiO 2 Catalysts Prepared with Alternative Cobalt Precursors

Different low-cost cobalt precursors (acetate, chloride) and thermal treatments (air calcination/H 2 reduction versus direct H 2 -activation) were investigated to alter the interaction between cobalt and silica. H 2 -activated catalysts prepared from cobalt chloride had large Co 0 particles (XRD, chemisorption) formed by weak interactions between cobalt chloride and silica (temperature programmed reduction (TPR), TPR with mass spectrometry (TPR-MS), TPR with extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge spectroscopy (XANES) techniques) and retained Cl-blocked active sites, resulting in poor activity. In contrast, unpromoted Co/SiO 2 catalysts derived from cobalt acetate had strong interactions between Co species and silica (TPR/TPR-MS, TPR-EXAFS/XANES); adding Pt increased the extent of the Co reduction. For these Pt-promoted catalysts, the reduction of uncalcined catalysts was faster, resulting in larger Co 0 clusters (19.5 nm) in comparison with the air-calcined/H 2 -activated catalyst (7.8 nm). Both catalysts had CO conversions 25% higher than that of the Pt-promoted catalyst prepared in the traditional manner (air calcination/H 2 reduction using cobalt nitrate) and three times higher than that of the traditional unpromoted Co/silica catalyst. The retention of residual cobalt carbide (observed in XANES) from cobalt acetate decomposition impacted performance, resulting in a higher C 1 –C 4 selectivity (32.2% for air-calcined and 38.7% for uncalcined) than that of traditional catalysts (17.5–18.6%). The residual carbide also lowered the α-value and olefin/paraffin ratio. Future work will focus on improving selectivity through oxidation–reduction cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Production of renewable alcohols from maple wood using supercritical methanol hydrodeoxygenation in a semi-continuous flowthrough reactor

Biomass conversion to alcohols using supercritical methanol depolymerization and hydrodeoxygenation (SCM-DHO) with CuMgAl mixed metal oxide is a promising process for biofuel production. Here, we demonstrate how maple wood can be converted at high weight loadings and product concentrations in a batch and a semi-continuous reactor to a mixture of C 2 –C 10 linear and cyclic alcohols. Maple wood was solubilized semi-continuously in supercritical methanol and then converted to a mixture of C 2 –C 9 alcohols and aromatics over a packed bed of CuMgAlO x catalyst. Up to 95 wt% of maple wood can be solubilized in the methanol by using four temperature holds at 190, 230, 300, and 330 °C. Lignin was solubilized at 190 and 230 °C to a mixture of monomers, dimers, and trimers while hemicellulose and cellulose solubilized at 300 and 330 °C to a mixture of oligomeric sugars and liquefaction products. The hemicellulose, cellulose, and lignin were converted to C 2 –C 10 alcohol fuel precursors over a packed bed of CuMgAlO x catalyst with 70–80% carbon yield of the entire maple wood. The methanol reforming activity of the catalyst decreased by 25% over four beds of biomass, which corresponds to 5 turnovers for the catalyst, but was regenerable after calcination and reduction. In batch reactions, maple wood was converted at 10 wt% in methanol with 93% carbon yield to liquid products. The product concentration can be increased to 20 wt% by partially replacing the methanol with liquid products. The yield of alcohols in the semi-continuous reactor was approximately 30% lower than in batch reactions likely due to degradation of lignin and cellulose during solubilization. These results show that solubilization of whole biomass can be separated from catalytic conversion of the intermediates while still achieving a high yield of products. However, close contact of the catalyst and the biomass during solubilization is critical to achieve the highest yields and concentration of products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Atomic Layer Deposition for Enhanced Reactivity and Stability of Biomass Conversion Catalysts

Heterogeneous catalysts are an essential tool in the transition towards a sustainable, bio-based economy for fuels and chemicals. However, the harsh conditions (e.g., high temperatures, acidity, oxidizing/reducing environments) of many key biomass conversion processes give rise to nanoparticle sintering, support collapse, and metal leaching in conventional PGM catalysts. Active site poisoning due to the relatively high sulfur content of most biomass feedstocks further compounds these durability problems. Next-generation catalysts must be developed to address these stability challenges. In this work, we used a scalable atomic layer deposition (ALD) process to modify conventional Pd-based hydrogenation catalysts to generate significant performance improvements. TiO2 ALD coatings were found to increase the activity of Pd/Al2O3 catalysts towards naphthalene hydrogenation; additionally, these coatings improved the catalyst's resistance to sulfur poisoning and thermal stability under oxidative calcination. Additional work in which Al2O3 ALD coatings were applied to Pd/TiO2 catalysts for muconic acid hydrogenation found similar stability benefits, including improved resistance to Pd leaching in the acidic environment. ALD technology holds great potential in the development of next-generation catalysts for biofuels and bioproducts and this work constitutes an important examination of applying ALD coatings to supported Pd hydrogenation catalysts.

ALD↗
NASA NTRS2009

Application of a mixed metal oxide catalyst to a metallic substrate

A method for applying a mixed metal oxide catalyst to a metallic substrate for the creation of a robust, high temperature catalyst system for use in decomposing propellants, particularly hydrogen peroxide propellants, for use in propulsion systems. The method begins by forming a prepared substrate material consisting of a metallic inner substrate and a bound layer of a noble metal intermediate. Alternatively, a bound ceramic coating, or frit, may be introduced between the metallic inner substrate and noble metal intermediate when the metallic substrate is oxidation resistant. A high-activity catalyst slurry is applied to the surface of the prepared substrate and dried to remove the organic solvent. The catalyst layer is then heat treated to bind the catalyst layer to the surface. The bound catalyst layer is then activated using an activation treatment and calcinations to form the high-activity catalyst system.

Sevener, Kathleen M.↗
DOE OSTI2020

Dehydra-decyclization of tetrahydrofurans to diene monomers over metal oxides

The dehydra-decyclization of tetrahydrofuran (THF) to butadiene was investigated over a series of metal oxide catalysts, where a common set of chemical pathways was identified. Alongside butadiene, propene is formed via a retro-Prins condensation as the main side product typically observed. Reaction occurred at similar temperatures on each of the oxides, but tetragonal zirconia (t-ZrO 2 ) and monoclinic zirconia (m-ZrO 2 ) were unique in showing high selectivity to butadiene (>90%). Near quantitative yields to butadiene could be achieved over t-ZrO 2 at 673 K and a WHSV of 0.93 g THF gcat –1 h –1 . Through contact time studies, butadiene is determined to be a primary product. Methyl-substituted THF gave only moderate increases in rates and the products showed minimal isomerization of the carbon backbone. The t-ZrO 2 catalyst was found to be relatively stable with time on stream, experiencing coking as a likely source of deactivation. Complete regeneration of the catalyst was demonstrated through calcination alone, allowing for multiple regenerations with no irreversible loss in activity or selectivity. Lastly, the catalytic activity of zirconia was found to be structure insensitive, with t-ZrO 2 and m-ZrO 2 exhibiting similar initial activities; however, m-ZrO 2 was observed to deactivate much more rapidly.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Silver Nanowire-Indium Zinc Oxide Composite Flexible Transparent Conducting Electrodes Made by Spin- coating and Photonic Curing

Realizing high-throughput, low-cost perovskite solar cell (PSC) manufacturing is highly sought-after in photovoltaic (PV) research in recent years. To fully achieve roll-to-roll (R2R) manufacturing of PSCs, it is important to consider the flexible transparent electrode (TE). PET/ITO is a commonly used substrate for making flexible PSCs. When optimizing transparent conducting materials, there is a tradeoff between sheet resistance (Rsh) and optical transparency. Because commercial PET/ITO substrates are made with slow (~1 m/min) vacuum deposition processes, they tend to be expensive. Therefore, it would be advantageous to develop a high-throughput, R2R compatible, solution-deposition approach for fabricating the TE on PET substrates. While various solution-deposition processes, such as blade coating or slot-die coating, can achieve the desired web speed of > 10 m/min, there is still a need to improve the post-deposition annealing step. One promising post-deposition processing technique is intense-pulsed-light processing, also known as photonic curing. Photonic curing delivers short (0.01 – 100 ms) pulses of broadband (200 – 1500 nm) light from a xenon flash lamp to the samples. Any materials in the sample stack that absorb light will convert the impinging light pulse into heat within the sample, which drives changes in the sample (calcination, phase change, crystallization, etc.). Photonic curing has three main advantages over thermal annealing: 1. Faster processing speed (milliseconds or seconds). 2. Compatibility with plastic substrates. 3. Smaller physical footprint and less wasted energy. Since the light pulses are on for a short time, the intensity can be high while the total energy delivered to the sample is low, minimizing damages to the plastic substrates. In this work, a hybrid TE material is fabricated on PET substrates using photonic curing. The hybrid TE material contains a layer of silver nanowires (AgNWs) and a layer of metal-oxide (InOx, ITO, IZO, etc.). The AgNWs increase the light absorbed by the film during the photonic curing process, which leads to higher processing temperatures, possibly improving the conversion of the metal-oxide layer. The AgNWs also enhance the electrical conductivity of the final TE layer after photonic curing. A AgNW and metal-oxide bilayer is formed by spin coating each solution onto the PET substrate sequentially followed by a single photonic curing process. We use average optical transmittance (Tavg) from 400 to 700 nm and average Rsh to evaluate the TE performance. The following photonic curing parameters are varied to optimize Tavg (maximize) and Rsh (minimize): Pulse voltage, pulse envelope, number of micro-pulses, duty cycle, number of pulses, and pulse repetition rate. Preliminarily, we also observe a significant impact on the TE properties by the volume of AgNW deposited during the spin coating deposition step. Using dispense volumes of 80 µL and 20 µL, we achieve samples with Tavg = 73%, Rsh = 19 Ω/sq, and roughness = 9 nm, and Tavg = 83%, Rsh = 58 Ω/sq, and roughness = 5.6 nm, respectively, after photonic curing.

14 SOLAR ENERGY↗
NASA NTRS1992

An acetate precursor process for BSCCO (2223) thin films and coprecipitated powders

Since the discovery of high temperature superconducting oxides much attention has been paid to finding better and useful ways to take advantage of the special properties exhibited by these materials. One such process is the development of thin films for engineering applications. Another such process is the coprecipitation route to producing superconducting powders. An acetate precursor process for use in thin film fabrication and a chemical coprecipitation route to Bismuth based superconducting materials has been developed. Data obtained from the thin film process were inconclusive to date and require more study. The chemical coprecipitation method of producing bulk material is a viable method, and is preferred over the previously used solid state route. This method of powder production appears to be an excellent route to producing thin section tape cast material and screen printed devices, as it requires less calcines than the oxide route to produce quality powders.

Haertling, Gene H.↗
NASA NTRS2010

Process for Making a Noble Metal on Tin Oxide Catalyst

To produce a noble metal-on-metal oxide catalyst on an inert, high-surface-area support material (that functions as a catalyst at approximately room temperature using chloride-free reagents), for use in a carbon dioxide laser, requires two steps: First, a commercially available, inert, high-surface-area support material (silica spheres) is coated with a thin layer of metal oxide, a monolayer equivalent. Very beneficial results have been obtained using nitric acid as an oxidizing agent because it leaves no residue. It is also helpful if the spheres are first deaerated by boiling in water to allow the entire surface to be coated. A metal, such as tin, is then dissolved in the oxidizing agent/support material mixture to yield, in the case of tin, metastannic acid. Although tin has proven especially beneficial for use in a closed-cycle CO2 laser, in general any metal with two valence states, such as most transition metals and antimony, may be used. The metastannic acid will be adsorbed onto the high-surface-area spheres, coating them. Any excess oxidizing agent is then evaporated, and the resulting metastannic acid-coated spheres are dried and calcined, whereby the metastannic acid becomes tin(IV) oxide. The second step is accomplished by preparing an aqueous mixture of the tin(IV) oxide-coated spheres, and a soluble, chloride-free salt of at least one catalyst metal. The catalyst metal may be selected from the group consisting of platinum, palladium, ruthenium, gold, and rhodium, or other platinum group metals. Extremely beneficial results have been obtained using chloride-free salts of platinum, palladium, or a combination thereof, such as tetraammineplatinum (II) hydroxide ([Pt(NH3)4] (OH)2), or tetraammine palladium nitrate ([Pd(NH3)4](NO3)2).

Davis, Patricia↗
NASA NTRS2005

A comparison of soil moisture sensors for space flight applications

Plants will be an important part of future long-term space missions. Automated plant growth systems require accurate and reliable methods of monitoring soil moisture levels. There are a number of different methods to accomplish this task. This study evaluated sensors using the capacitance method (ECH2O), the heat-pulse method (TMAS), and tensiometers, compared to soil water loss measured gravimetrically in a side-by-side test. The experiment monitored evaporative losses from substrate compartments filled with 1- to 2-mm baked calcinated clay media. The ECH2O data correlated well with the gravimetric measurements, but over a limited range of soil moisture. The averaged TMAS sensor data overstated soil moisture content levels. The tensiometer data appeared to track evaporative losses in the 0.5- to 2.5-kPa range of matric potential that corresponds to the water content needed to grow plants. This small range is characteristic of large particle media, and thus high-resolution tensiometers are required to distinguish changing moisture contents in this range.

NASA Center KSC↗
DOE OSTI2025

Investigating rapid alpha-decay induced aging of 238 PuO 2 by Raman Spectroscopy

Investigating alpha-decay induced aging in PuO 2 is useful in nuclear forensics; helping to determine the time since last calcination. This was previously investigate by monitoring the damage to 240 PuO 2 over the course of a few years. The rate of alpha-decay induced aging has long been assumed to scale only with the decay rate of other isotopes without direct verification. This article reports the first alpha-decay aging study of 238 PuO 2 by Raman spectroscopy. Contrary to the expected 10 days for 238 PuO 2 to reach steady state based on 240 PuO 2 studies, the alpha aging curve reached an approximate steady state ∼24–30 h after laser annealing. While the cause of the order of magnitude decrease is unknown, it is speculated that dynamic annealing could contribute to the differences in rate of induced aging. The Raman spectra of annealed and aged 238 PuO 2 matched the expected features in 239 PuO 2 and 240 PuO 2 spectra; showing no formation of new stable chemical species in the material such as secondary Pu oxide phases (e.g., Pu 4 O 9 ). In conclusion, results indicate that 238 Pu could be leveraged for rapid alpha-decay aging studies to characterize alpha-decay induced features and better understand matrix temperatures and the annealing of Frankel pair defects.

Actinide↗
DOE OSTI2024

Formation and Detriments of Residual Alkaline Compounds on High-Nickel Layered Oxide Cathodes

High-nickel layered oxides LiNi x M 1-x O 2 (x ≥ 0.9) have emerged as promising cathode materials for automotive batteries due to their high energy density and lower cost. However, the formation and accumulation of surface alkaline compounds during storage hinder their mass production and commercialization. Here, in this study, a validated chemical method is employed to deconvolute and quantify the evolution of each residual lithium compound in four representative cathodes during ambient-air storage, viz., LiNiO 2 (LNO), LiNi 0.95 Co 0.05 O 2 (NC), LiNi 0.95 Mn 0.05 O 2 (NM), and LiNi 0.95 Al 0.05 O 2 (NA). Furthermore, the activation energy of the reaction between water and the cathode is determined by measuring the leached LiOH concentration at various temperatures. While residual lithium and time-of-flight secondary-ion mass spectrometry measurements collectively reveal that the air stability overall follows the trend of NM > NA ≈ NC > LNO, the aged NM exhibits the highest charge-transfer resistance and the worst electrochemical performance among the cathodes. In situ, X-ray diffraction and scanning transmission electron microscopy unveil that the aged NM is plagued by a large area of resistive spinel-like M 3–x Li x O 4 phases, leading to aggravated particle reaction heterogeneity. Finally, a one-step recalcination method is demonstrated effective in fully restoring the degraded cathodes. This work provides insights into overcoming air sensitivity issues of high-Ni cathodes.

(S)TEM↗
NASA NTRSDate not supplied

Microwave Structure Construction Capability Year One Accomplishments

The Microwave Structure Construction Capability (MSCC) element, part of the Moon to Mars Planetary Autonomous Construction Project (MMPACT) was initiated in 2020. MSCC is responsible for creating horizontal and vertical infrastructure on the moon using microwave energy. Microwave energy was selected since it is the only method to volumetrically heat the regolith. All other sintering/melting methods rely on thermal conduction through the very low conductivity surface, resulting in an inefficient process. Advances were achieved in materials characterization and understanding, microwave sintering in vacuum, and microwave design and analyses. Two dielectric property testing systems have been developed at Radiance Technologies and JPL. These will examine dielectric properties at cryogenic temperatures and over a broad frequency range. Permittivity and permeability testing at -60 ̊C in vacuum from 0.05 to 3 GHz has been generated at JPL. Additional modifications will be made to go to -190 ̊C (LN2). Radiance Technologies created a test system to measure dielectric properties at greater than 10 GHz and initiated work on developing a vacuum capable, portable test system to measure dielectric properties of Apollo regolith and simulants from 100 MHz to 18 GHz. These tests are to identify optimal heating frequencies and protocols. During microwave sintering at about 1100 ̊C, volatiles were creating difficulty in achieving a reasonably dense specimen. Due to processing in vacuum and the nature of the lunar regolith, some volatiles and porosity are expected. However, the Earth produced simulants have non-lunar materials in them that create volatiles that aren’t representative of lunar regolith. Therefore, a five month effort was conducted to establish a heat treat method to remove these non-lunar materials. Tests were conducted using TGA mass spectrometry, heating in vacuum and conducting mass spectrometry, dielectric and DTA, Raman, BET, particle size analysis, morphological analysis, carbon and sulfur chemical content determination and microscopy. The process has been scaled-up to 6 kg batch size and undergoing evaluation. A 36 kg batch size is the target for JSC-1A and other limited availability simulants. These calcining protocols will be standard for NASA and beyond. MSCC has also created scalable processes for fabricating synthetic lunar materials. Processes to fabricate Anorthite (plagioclase CaAl2Si2O8), Diopside (pyroxene CaMgSi₂O₆), and Enstatite (pyroxene Mg2Si2O6) have been generated. These materials will enable generation of microwave sintering models to bound various composition ranges anticipated on the Moon, therefore mitigating the need for a precise simulant with respect to location on the Moon. Successful microwave sintering in air using a horn applicator was demonstrated. All previous microwave vacuum sintering in the literature was at small scale and in a contained enclosure thus taking advantage of reflections. This is the first to use a lunar like microwave applicator to sinter ceramic in a bed as it would be done on the Moon. Small scale and inert sintering were conducted to assist in developing protocols with quicker turnaround times than larger scale testing. Testing has anchored thermal analysis predicting heat flow in vacuum during microwave sintering. Thermal conductivity testing was also initiated. Microwave coupling to the regolith has been modeled by multiple organizations and with different software packages. At least six horn designs and applicator configurations for both magnetron and solid state sources are being examined. Optimal simulant container designs for microwaves have also been generated. The power and electronics design for the solid state microwave system has been initiated. Concept designs for a lander based microwave sintering have been evaluated.

microwave↗
DOE OSTI2024

Aspects of Spodumene Lithium Extraction Techniques

Lithium (Li), a leading cathode material in rechargeable Li-ion batteries, is vital to modern energy storage technology, establishing it as one of the most impactful and strategical elements. Given the surge in the electric car market, it is crucial to improve lithium recovery from its rich mineral deposits using the most effective extraction technique. In recent years, both industry and academia have shown significant interest in Li recovery from various Li-bearing minerals. Of these, only extraction from spodumene has established a reliable industrial production of Li salts. The current approaches for cracking of the naturally occurring, stable α-spodumene structure into a more open structure—β-spodumene—involve the so-called decrepitation process that takes place at extreme temperatures of ~1100 °C. This conversion is necessary, as β-spodumene is more susceptible to chemical attacks facilitating Li extraction. In the last several decades, many techniques have been demonstrated and patented to process hard-rock mineral spodumene. The objective of this review is to present a thorough analysis of significant findings and the enhancement of process flowsheets over time that can be useful for both research endeavors and industrial process improvements. The review focuses on the following techniques: acid methods, alkali methods, carbonate roasting/autoclaving methods, sulfuric acid roasting/autoclaving methods, chlorinating methods, and mechanochemical activation. Recently, microwaves (MWs), as an energy source, have been employed to transform α-spodumene into β-spodumene. Considering its energy-efficient and short-duration aspects, the review discusses the interaction mechanism of MWs with solids, MW-assisted decrepitation, and Li extraction efficiencies. Finally, the merits and/or disadvantages, challenges, and prospects of the processes are summarized.

25 ENERGY STORAGE↗