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At least 163 records · Page 9

Non-classical ion-indiffusion processes in quasi-one-dimensional ionic conductor KTiOPO4

Developments in coercive field engineering and waveguide writing via ion-exchange in the ferroelectric ionic-conductor KTiOPO4 (KTP) have led to breakthroughs within the field of nonlinear optics and quantum photonics. However, the microscopic diffusion dynamics of ion-exchange in KTP are poorly understood and show signs of non-classical diffusion dynamics. The precise control of ion-exchange gradients is critical for developing KTP into a mature, integrated nonlinear optical material but requires a level of control that, in turn, demands a deeper understanding of the ion-exchange process. We employ direct ToF-SIMS mapping to untangle the complex diffusion dynamics of the commonly used ion-exchange dopant ions: Rb, Ba, and K. We map periodic diffusion gradients of two exchanges, one dominated by Rb-ions and the other by Ba-ions. For the first time, we show the interdependent nature of the Ba- and Rb ion in the ion-exchange diffusion gradient. The low incorporation of the Ba ion is mapped and quantified, and dopant–crystal interactions are identified. This work highlights the complex diffusion dynamics of dopants in the KTP structure and lays the foundation for deterministic control of diffusion gradients for the next generation of integrated nonlinear and quantum photonic devices.

Barrett, Laura [ORNL]↗

Reduced Temperature Cesium Removal from AP-101 Using Crystalline Silicotitanate

The Tank Side Cesium Removal (TSCR) system, currently operational under Washington River Protection Solutions LLC (WRPS), sends initial low-activity Hanford waste tank supernate feed to the Hanford Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) Facility. In addition to entrained solids removal from the supernate, the primary goal of TSCR is to remove cesium-137 ( 137 Cs) by ion exchange, allowing contact handling of the liquid effluent product at the WTP. Crystalline silicotitanate (CST) ion exchange media, manufactured by Honeywell UOP, LLC (product IONSIV™ R9140-B), was selected as the ion exchange media at TSCR. Laboratory-scale ion exchange processing using TSCR prototypic unit operations continues to contribute toward WRPS establishing accurate process flowsheets for the individual feed campaigns planned for TSCR. This report describes the small-scale ion exchange testing with 14.0 L of diluted and filtered supernate from tank 241-AP-101 (AP-101DF) at 16 °C (62 °F) to demonstrate processing at temperature conditions that are more prototypic of what the TSCR system could experience during colder seasons of the year. Since CST Cs capacity increases with decreasing contact temperature, testing at the lower operating temperature will help to predict the maximum 137 Cs loading onto the CST in the TSCR system. One of the waste acceptance criteria (WAC) for the WTP Low-Activity Waste Facility is that the waste must contain less than 3.18×10 -5 Ci 137 Cs per mole of Na. For the AP-101DF tank waste to meet this criterion, only 0.144% of the influent 137 Cs concentration may be delivered to the WTP; this requires a Cs decontamination factor of 694. Testing with AP-101DF matched TSCR prototypic operations where a lead-lag configuration was used until the lag column reached the WAC limit, then a polish column was brought online for continued processing in a lead-lag-polish column configuration. Feed was processed at 1.9 bed volumes (BVs) per hour; the flowrate, in terms of contact time with the CST bed, matched the expected flowrate at TSCR. The Cs-decontaminated product was retained for vitrification testing (to be reported separately). The lead column reached 62% Cs breakthrough after processing ~1400 BVs of feed; the 50% Cs breakthrough occurred at 1250 BVs. Testing compared to previous AP-107 testing at 16 °C showed ~80 BV increases in volume processed to reach the WAC limit for both lead and lag columns. A similar slope in breakthrough curves for both tests indicates similar kinetic behavior, with variations in feed matrices (Na and Cs concentrations) likely responsible for the deviations in reaching the WAC limit. The Cs effluent from the lag column reached the WAC limit after processing 875 BVs. Anticipating this breakthrough point, the polish column was preemptively installed at 770 BVs. Cs breakthrough from the lag column began at 300 BVs, reaching 5.32×10 0 µCi/mL, or 5.6 % Cs breakthrough, after processing all 1400 BVs of feed. Table S.1 and Figure S.1 summarize the observed column performance and relevant Cs loading characteristics.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

CO2 Capture Strategies via Mineralization with Industrial Waste Brines

Large coal-fired power plants (>500 MW) account for 30% of global CO2 emissions, and long-term management of this CO2 to is urgently needed mitigate global temperature increases. Sequestration of CO2 within stable mineral carbonates (e.g., CaCO3) represents an attractive emission reduction strategy because it offers a leakage-free alternative to geological storage of CO2 in an environmentally friendly form. We have previously described a mineralization process in which divalent cations are sourced from various waste streams (e.g., produced water and brackish water) and alkalinity is induced via regenerable ion-exchange materials (Bustillos et. al. Frontiers in Energy Research. 2020, 8, 352). In our process, aqueous carbonate-bearing streams with pH > 8 are produced by contacting fresh water and carbon dioxide with various ion-exchange materials (e.g., Na form zeolites or ion exchange resins). These streams are mixed with produced water containing varying concentrations (~0.01 – 1.0 M) of Ca2+ leading to the precipitation of solid calcium carbonate (PCC). This process has the advantages of using regenerable solids in a simple and continuous process to increase the pH of water by ion exchange instead of relying on the consumption of costly and unsustainable sources of alkalinity (e.g., sodium hydroxide). While once-through column experiments showed the above benefits, the same were yet to established in a steady-state process with recycle streams. In this work, we set up a process simulation to quantify the energy requirements and CO2 emissions associated with the process and seek optimal produced water compositions and CO2 concentrations (5 – 20 vol%). The process simulation was set up in ASPEN Plus using eRNTL as the thermodynamic property method and sequential modular strategy. Ion exchange alkaline solution was simulated using sodium hydroxide and validated against the experimental data obtained from once-through kinetic experiments. Nanofiltration and reverse osmosis membrane steps were also implemented for the separation of divalent cations and production of fresh water and a regeneration stream following mineralization. Sensitivity analysis was carried out using a range of produced water compositions (0.01 – 1.0 M Ca2+, 0.001 – 0.15 M Mg2+, 0.5 – 3.5 M Na+ and 0.0004 – 0.002 M Fe2+) according to the United States Geological Survey (USGS) database. Calcium carbonate yields increased with increasing CO2 concentrations and were maximized using produced water compositions with larger Ca2+ concentrations. Maximum calcium carbonate yields produced at 5 vol%, 12 vol% and 20 vol% CO2 were 2.3 mmol/L, 5.5 mmol/L, and 9.3 mmol/L, respectively, with the formation of brucite (a magnesium hydroxide phase, Mg(OH)2) and goethite (an iron hydroxide phase, FeOOH) as the primary contaminant phases (99% calcite, 0.6% brucite, 0.4% goethite), which agree with phases detected by XRD experimentally. These results indicate high purity calcium carbonate can be precipitated using industrial waste streams. Consequentially, energy consumption and net CO2 emissions were minimized where precipitated calcium carbonate was maximized for all produced water compositions and CO2 concentrations. Minimum energy consumptions were 0.21 kWh/ton CO2 processed, with 98% of the energy input required coming from the membrane filtration steps. Produced water compositions with large Na+ concentrations (> 0.5 M) were effective at reducing energy consumptions due to faster regeneration time of ion exchange materials. Additionally, calculated net CO2 emissions were negative for the process and ranged from -0.02 kg/ton CO2 to -0.15 kg/ton CO2 processed, indicating a low emission process. We will also present techno-economic assessment showing the economic benefits of the current process as an alternative to the addition of stoichiometric bases to induce alkalinity for the precipitation of CaCO3.

Simonetti, Dante↗

Thermodynamic and Kinetic Barriers Limiting Solid-State Reactions Resolved through In Situ Synchrotron Studies of Lithium Halide Salts

Although halide salts such as LiCl and LiBr are routinely used as a source of Li ions during ion exchange reactions, a detailed understanding of the processes controlling the rates of these reactions is presently lacking. Recently, it has been discovered that the rate limiting barriers for ion exchange are commonly associated with these salts rather than the ceramic target of ion exchange, making it important to quantitatively understand of salt processes. Here it is demonstrated that in situ synchrotron studies of ion exchange reactions can be used to precisely quantify the thermodynamic activation energies associated with these solid state reactions in a manner that can be directly compared with predictions from density functional theory (DFT). While the temperature dependence of the LiCl reaction rate is found to be set by a barrier associated with ion hopping, it was discovered that for LiBr it is also affected by the defect formation energy – an energy found to be substantially lower than predicted by DFT. Furthermore, it is shown that when reaction rates for different relative amounts of reactants are varied, it is possible to identify the rate-limiting reagent and to elucidate an overall scaling relationship that controls the concentration-dependence of the reaction rate. Also, it is demonstrated that global fits across doped and undoped salts can be used to probe both intrinsic and extrinsic vacancy concentrations. This improved understanding of ion exchange mechanisms can be used to accelerate ion exchange reaction rates by orders of magnitude. In conclusion, the techniques demonstrated here can be broadly applied to probe the kinetics and thermodynamics of solid state reactions.

36 MATERIALS SCIENCE↗

Concentration and Recovery of Rare Earth Elements from Eastern US Coal Refuse

Recent studies funded by the US Department of energy have shown that coal and coal byproducts contain elevated contents of Rare Earth Elements (REEs), making them a potential resource for these critical materials. The approach employed in this research focused on the concentration and extraction of REEs from fine coal refuse derived from various preparation plants in the Appalachian coal basin of the United States. Initial efforts in this research focused on the identification and characterization of REEs in various fine coal refuse streams from nine distinct industrial preparation plants in Appalachia. The average REE content in these materials was determined to be approximately 200 ppm, but the REE content showed a strong correlation to the aluminum content, suggesting that the REEs are closely associated with the clay minerals present in the refuse. Given the relatively low REE concentrations, initial efforts sought to concentrate the REEs through decarbonization and dispersive liberation steps. In these tests, high-shear agitation in the presence of a polyelectrolyte, followed by sedimentation was able to isolate the REE-enriched fine clay particles from siliceous gangue minerals. Following the dispersive liberation step, all samples were found to have an REE content greater than 300 ppm, a benchmark used for many initial exploratory studies. In one case, the REE content was increased by more than 125%. Subsequent extraction tests initially utilized a direct ion-exchange leaching approach with ammonium sulfate as lixiviant. In all cases, the simple ion-exchange leaching process failed to recover significant quantities of rare earth elements, ultimately suggesting that the REEs in fine coal waste may be passivated or bound in a colloidal phase. To access this colloidal phase, several alternative approaches were evaluated, including leaching with alternative ion-exchange lixiviants, reductive leaching, gas-purged leaching, and others. The approach that showed the most promise was strong alkaline pretreatment, followed by ion-exchange leaching with ammonium sulfate at pH 4. A combination of strong alkali and high-temperatures treatment successfully liberated the REEs, converting them to a form amenable to ion-exchange leaching. The highest REE recovery achieved with this method was determined to be 39%. Lastly, bench-scale solvent extraction tests were used to further concentrate REEs in the leach solution and demonstrate that mixed rare earth concentrates can be successfully produced from fine coal refuse.

01 COAL, LIGNITE, AND PEAT↗

Impact of feed variability on cesium removal with multiple actual waste samples from the Hanford site

Here, the Tank Side Cesium Removal (TSCR) system, under development by Washington River Protection Solutions (WRPS), will send initial low-activity Hanford waste tank supernate feeds to the Hanford Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) Facility. In addition to entrained solids removal from the supernate, the primary goal of TSCR is to remove cesium-137 ( 137 Cs) by ion exchange, allowing contact handling of the liquid effluent product at WTP. Crystalline silicotitanate (CST) ion exchange media, manufactured by Honeywell UOP (product IONSIV™ R9140-B), was selected as the ion exchange media at TSCR. This lot of material was found to have superior performance in comparison to historic batches of CST. Ion exchange column and batch contact testing with supernate from Hanford tanks AP-105, AP-107 and AW-102 was performed to assess the impact of feed variability on system performance. These tests demonstrated that batch contact measurements provide a reasonable prediction of column capacities with some deviation in performance attributed to column dynamics. In addition, the variability in CST capacity for cesium in the various actual waste samples does not track with historical understanding of the competing cations, suggesting that tank waste samples contain other components that may significantly impact cesium loading.

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Uncovering the predictive pathways of lithium and sodium interchange in layered oxides

Ion exchange is a powerful method to access metastable materials with advanced functionalities for energy storage applications. However, high concentrations and unfavourably large excesses of lithium are always used for synthesizing lithium cathodes from parent sodium material, and the reaction pathways remain elusive. Here, using layered oxides as model materials, we demonstrate that vacancy level and its corresponding lithium preference are critical in determining the accessible and inaccessible ion exchange pathways. Taking advantage of the strong lithium preference at the right vacancy level, we establish predictive compositional and structural evolution at extremely dilute and low excess lithium based on the phase equilibrium between Li 0.94 CoO 2 and Na 0.48 CoO 2 . Such phase separation behaviour is general in both surface reaction-limited and diffusion-limited exchange conditions and is accomplished with the charge redistribution on transition metals. Guided by this understanding, we demonstrate the synthesis of Na y CoO 2 from the parent Li x CoO 2 and the synthesis of Li 0.94 CoO 2 from Na y CoO 2 at 1-1,000 Li/Na (molar ratio) with an electrochemical assisted ion exchange method by mitigating the kinetic barriers. Our study opens new opportunities for ion exchange in predictive synthesis and separation applications. Ion exchange is a powerful method to access metastable materials for energy storage, but identifying lithium and sodium interchange in layered oxides remains challenging. Using such model materials, vacancy level and corresponding lithium preference are shown to be crucial for ion exchange pathway accessibility.

25 ENERGY STORAGE↗

Acid Catalysis over Low-Silica Faujasite Zeolites

We report low-silica faujasite (FAU) zeolites (with Si/Al ratio of ca. 1.2–1.8) sustain framework integrity and porosity upon moderate ion exchange (0.01 M NH 4 NO 3 solution for 1 h at ambient temperature), which introduces two kinds of protons, distinctive in reactivity and coordination to the zeolite framework, within supercages (H SUP ). Moderate ion exchange limited within supercages transpires while maintaining full occupancy of Na + cations within associated sodalite cages; this in turn helps stabilize the framework of low-silica H-FAU zeolites. Protons located on site II (H 3630 ) and site III (H 3650 ) within supercages on low-silica FAU zeolites can be classified and enumerated by virtue of infrared spectroscopy, providing an opportunity to compare reactivities of these distinct protons for monomolecular protolytic reactions of propane. Protons on site II exhibit prominently higher reactivity for monomolecular propane dehydrogenation and cracking than protons on site III. Low-silica proton-form FAU zeolites (zeolite X) upon moderate ion exchange possess protons on site III that are unavailable on high-silica FAU zeolites (zeolite Y) and limit ion exchange within supercages, providing unprecedented high-temperature structural and chemical stability (>773 K) and enabling their application as solid-acid catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A comparative study of silver- and palladium-exchanged zeolites in propylene and nitrogen oxide adsorption and desorption for cold-start applications

Here, silver and palladium ion-exchanged BEA zeolites (Si/Al = 12.5) and silver ion-exchanged ZSM-5 zeolites (Si/Al = 15) were studied for their ability to adsorb and desorb propylene and NO under simulated diesel exhaust conditions. The adsorption experiment results demonstrated the excellent ability of bare BEA zeolites to adsorb propylene, but only a small amount of NO. The presence of H 2 O inhibited the adsorption of both C 3 H 6 and NO. Ion-exchanging BEA zeolites with Ag (1.2 and 5.1 wt.% Ag/BEA) attenuated the inhibiting effect of H 2 O on C 3 H 6 adsorption, while NO storage remained inhibited. Adsorption experiments indicated that C 3 H 6 and NO competed with each other for Pd sites with C 3 H 6 showing stronger adsorption compared to NO, whereas Ag sites preferentially adsorbed C 3 H 6 . DRIFTS data indicated the formation of nitrate, formate and acetate species on Ag and Pd, while C 3 H 6 and NO adsorption was also observed on the zeolite hydroxyl groups in the absence of H 2 O. However, the C 3 H 6 and NO adsorption on the zeolite hydroxyl groups was significantly inhibited in the presence of H 2 O. Additionally, nitrosyl, acrolein and carbonate species were formed over 1.0 wt.% Pd/BEA. The effluent analysis during the temperature-programmed desorption in the DRIFTS reactor revealed that adsorbed C 3 H 6 and NO reacted during the release to form oxidation reaction byproducts. The 1.0 wt.% Pd/BEA zeolite showed the greatest oxidation ability during desorption with the majority of stored C 3 H 6 converted to CO 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CST R9120-B 30x60 Media Pretreatment and Digestion Standard Development to Support Tank Closure Cesium Removal 1A (TCCR-1A) Operations

In support of continued operations of Savannah River Remediation’s (SRR) ion exchange process to remove radioactive cesium from Savannah River Site (SRS) dissolved saltcake, referred to as the Tank Closure Cesium Removal 1A process (TCCR-1A; containing the second set of at-tank ion exchange columns), SRNL was tasked with: 1) validating the field protocol planned for pretreating the crystalline silicotitanate (CST) ion exchange media to be used in the columns, 2) preparing CST media for use in in-tank batch contact testing, and 3) developing a digestion standard to verify complete CST dissolution prior to characterization following each in-tank batch contact test. A procedure (SRNL L29 Manual, ITS-0229) was developed previously in support of the TCCR Demonstration (which contained the first set of ion exchange columns) based on evaluations of a different CST production lot with a larger particle size range to document the protocol for pretreating CST utilizing conditions similar to what will be performed in the field.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In Situ Observation of Ion Migration in a Ferroelectric Ionic Conductor Rb-KTP during Thermal Annealing

Ion exchange in Rb-doped KTiOPO 4 has facilitated significant advancements in ferroelectric domain engineering, yet understanding the underlying mechanisms remains in its infancy. We perform time-of-flight secondary ion mass spectrometry analysis on multiple periodically ion-exchanged and periodically poled Rb-doped KTiOPO 4 samples under different temperatures and annealing durations. The results are compared between annealing in air, which involved ex situ annealing before periodic poling, and vacuum annealing conducted in situ after periodic poling. The Rb + diffusion profile after periodic ion exchange forms a tooth-shaped pattern. We show that in situ annealing causes a surface pinning effect on the nonpolar face, limiting Rb + migration along the polar axis at the surface. Once the pinned layer is removed through milling, the underlying Rb + diffusion is distinctively different from the surface. Additionally, the rate of Rb + diffusion during in situ annealing is linear, while the periodic domain structures remain stable after annealing. These results contribute to understanding the ionic diffusion process in a ferroelectric ionic conductor and using ion exchange to tailor the linear and nonlinear properties of KTiOPO 4 .

36 MATERIALS SCIENCE↗

Sodium, Silver and Lithium-Ion Conducting β''-Alumina + YSZ Composites, Ionic Conductivity and Stability

Na-β''-alumina (Na 2 O.~6Al 2 O 3 ) is known to be an excellent sodium ion conductor in battery and sensor applications. In this study we report fabrication of Na- β''-alumina + YSZ dual phase composite to mitigate moisture and CO 2 corrosion that otherwise can lead to degradation in pure Na-β''-alumina conductor. Subsequently, we heat-treated the samples in molten AgNO 3 and LiNO3 to respectively form Ag-β''-alumina + YSZ and Li-β''-alumina + YSZ to investigate their potential applications in silver- and lithium-ion solid state batteries. Ion exchange fronts were captured via SEM and EDS techniques. Their ionic conductivities were measured using electrochemical impedance spectroscopy. Both ion exchange rates and ionic conductivities of these composite ionic conductors were firstly reported here and measured as a function of ion exchange time and temperature.

36 MATERIALS SCIENCE↗

Water production for coffee brewing by electrodeionization

A resin-wafer electrodeionization (RW-EDI) apparatus for purifying water for coffee brewing comprises a cathode; an anode; and multiple porous solid resin wafer exchange units arranged in a stack between the cathode and the anode, and an air distributor adapted and arranged to aerate the water to be purified. Each unit comprises a monovalent cation exchange membrane (CEM), an anion exchange membrane (AEM), and an ion exchange resin wafer between the CEM and the AEM, which is in contact with, and in fluid flow connection with the CEM and AEM. Each resin wafer comprises a cation exchange resin and an anion exchange resin. The units are oriented with the CEM facing the cathode and the AEM facing the anode, with space between the units defining ion concentrate chambers. Bipolar ion exchange membranes separate the anode and cathode from their nearest resin wafer exchange units.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High Ion Conductive and Selective Membrane Achieved through Dual Ion Conducting Mechanisms

Conventional ion-selective membranes, that is ion-exchange and porous membranes, are unable to perform high conductivity and selectivity simultaneously due to the contradictions between their ion selecting and conducting mechanisms. Here, in this work, a bifunctional ion-selective layer is developed via the combination of nanoporous boron nitride (PBN) and ion exchange groups from Nafion to achieve high ion conductivity through dual ion conducting mechanisms as well as high ion selectivity. A template-free method is adopted to synthesize flake-like PBN, which is further enmeshed with Nafion resin to form the bifunctional layer coated onto a porous polyetherimide membrane. The double-layer membrane exhibits excellent ion selectivity (1.49 × 10 8 mS cm –3 min), which is 22 times greater than that of the pristine porous polyetherimide membrane, with outstanding ion conductivity (64 mS cm –1 ). In a vanadium flow battery, the double-layer membrane achieves a high Coulombic efficiency of 97% and outstanding energy efficiency of 91% at 40 mA cm –2 with a stable cycling performance for over 700 cycles at 100 mA cm –2 . PBN with ion exchange groups may therefore offer a potential solution to the limitation between ion selectivity and conductivity in ion-selective membranes.

36 MATERIALS SCIENCE↗

Synthesis of Zeolites LiX and LiAgX

In this work, we produced approximately 50 grams of zeolite LiX and 50 grams of zeolite LiAgX from commercially available zeolite X. The production of the two specialized zeolite phases was accomplished via a series of ion exchange steps followed by washing, drying, and calcining to produce the final materials. The ion exchange was confirmed by several methods including inductively-coupled plasma emission spectroscopy of exchange solution aliquots, gravimetric analysis, energy dispersive x-ray spectroscopy, and X-ray diffraction. We synthesized approximately 115 grams of zeolite LiX in a large-scale production step after completing a proof-of-concept experiment demonstrating the methodology. The production of zeolite LiX from zeolite X yielded an ion exchange (Li + →Na + ) of approximately 82%. The production of zeolite LiAgX from the previously synthesized zeolite LiX was targeted to exchange approximately 20% of the Li + ions with Ag + ions. We first performed a proof-of-concept experiment demonstrating the reaction pathway and selectivity of the Ag + ion, and then performed a large-scale synthesis of zeolite LiAgX using approximately 50 grams of the zeolite LiX. Our final exchange percentage of silver into the zeolite LiX matrix was approximately 20.8%.

36 MATERIALS SCIENCE↗

FY2021 Rotating Bed Reactor for Iodine Removal from ETF Feed to Support DFLAW Start-Up

In FY20, Washington River Protection Solutions, LLC (WRPS) began a program of work to evaluate potential technologies for removal of iodine from the ETF feed. Work at the Pacific Northwest National Laboratory (PNNL) focused on ion exchange media and conventional column based deployment while Atkins and VSL focused on ion exchange media in a Rotating Bed Reactor (RBR) system. In the RBR system, the ion exchange media is loaded into a packed bed, which is rotated in the liquid to be treated. The work described in this report builds on the results from FY20 work, in particular, with regard to improving iodate removal, extending the data set to support process modeling, further comparison of RBR versus column performance, and RBR scale-up testing.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗