In Situ Neutron Diffraction Showing Lithium-Yttrium Chloride Local Structure By Synthesis Method
Robert L. SacciTeerth BrahmbhattBuwen ChengLiqun GuoJie ZhengMounesha N. GaragaSteve GreenbaumYan YaoJagjit Nanda
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Lithium halide-based solid electrolytes have high Li + conductivity and are mostly synthesized through mechanochemical methods.[1] However, Li 3 InCl 6 can be readily synthesized through low-temperature aqueous solution routes by mere dehydration, presumably due to stable InCl 6 3- complexation. [2-4] Replacing In for Y results in partial hydrolysis to form YOCl during dehydration because H 2 O coordinates more strongly to Y 3+ cations. We provide insight into the reaction mechanisms involved in synthesizing halide solid electrolytes, highlighting the importance of synthetic and processing conditions to optimize their performance in all-solid-state batteries. We will describe the synthesis process of Li 3 YCl 6 using three different methods and the evolution thereof using in situ neutron diffraction. Our results show that aqueous-based synthesis requires the formation of an ammonium halide complex intermediate. We found that the synthesis method affects changes in local structure within the lattice, which then affect ionic transport and Li + diffusivity, as determined through diffusion NMR measurements. We ascribe these changes to the correlative transport of Li + . Synthesis affects particle morphology at the macroscale and relates to cycle life when used in a full cell. This project was supported by the Vehicle Technologies Office (VTO) under the Office of Energy Efficiency and Renewable Energy (EERE) as part of the Battery Materials Research (BMR) program. This research used resources at the Spallation Neutron Source, a DOE Office of Science User Facility operated by the Oak Ridge National Laboratory. [1] Park, K.-H.; Kaup, K.; Assoud, A.; Zhang, Q.; Wu, X.; Nazar, L. F. High-Voltage Superionic Halide Solid Electrolytes for All-Solid-State Li-Ion Batteries. ACS Energy Lett. 2020, 5, 2, 533–539. [2] Li, X.; Liang, J.; Luo, J.; Norouzi Banis, M.; Wang, C.; Li, W.; Deng, S.; Yu, C.; Zhao, F.; Hu, Y.; Sham, T.-K.; Zhang, L.; Zhao, S.; Lu, S.; Huang, H.; Li, R.; Adair, K. R.; Sun, X. Air-Stable Li 3 InCl 6 Electrolyte with High Voltage Compatibility for All-Solid-State Batteries. Energy Environ. Sci. 2019, 12, 2665-2671. [3] Li, W.; Liang, J.; Li, M.; Adair, K. R.; Li, X.; Hu, Y.; Xiao, Q.; Feng, R.; Li, R.; Zhang, L.; Lu, S.; Huang, H.; Zhao, S.; Sham, T.-K.; Sun, X. Unraveling the Origin of Moisture Stability of Halide Solid- State Electrolytes by In Situ and Operando Synchrotron X-Ray Analytical Techniques. Chem. Mater. 2020,32, 16, 7019–7027. [4] Sacci, R.L.; Bennett, T.H.; Drews, A.R.; Anandan, V.; Kirkham, M.J.; Daemen, L.L.; Nanda, K. Phase evolution during lithium indium halide superionic conductor dehydration. J. Mater. Chem. A , 2021,9, 990-996.Keywords:
Lithium chloride
(1) Solid sample electrodes were prepared from carbon, “sirupus simplex” and varying amounts of lithium chloride and the amount of lithium chloride was spectrographically determined with a sensitivity of 3×10−5% with respect to the line at λ=6707.9 Å, and with that of 1×10−4% with respect to the line at λ=6103.6 Å. (2) The method of comparison was found to be applicable for the determination of lithium chloride throughout the range of 0.001–0.050%. (3) Several samples containing lithium were analysed by the graphical method and were found to contain 1–12×10−3% of lithium chloride. (4) Several samples of clay produced in Seto and Inuyama were found to contain 3×10−5% of lithium by the graphical method.
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The reaction of metallic potassium with lithium chloride was studied for the effects of time, temperature, and concentration on the yield and purity of metallic lithium. For temperatures above 750/sup 0/C the yields were in the range of 51 to 68% with purities of 84 to 96 wt %. Essentially all of the impurity was unreacted potassium which should be easily removed. A comparison of chemical potentials obtained from the literature indicated that other reactants exist which should produce lithium in higher yields.
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Abstract Objectives —To assess the effect of increasing serum lithium concentrations on lithium dilution cardiac output (LiDCO) determination and to determine the ability to predict the serum lithium concentration from the cumulative lithium chloride dosage. Animals —10 dogs (7 males, 3 females). Procedure —Cardiac output (CO) was determined in anesthetized dogs by measuring LiDCO and thermodilution cardiac output (TDCO). The effect of the serum lithium concentration on LiDCO was assessed by observing the agreement between TDCO and LiDCO at various serum lithium concentrations. Also, cumulative lithium chloride dosage was compared with the corresponding serum lithium concentrations. Results —44 paired observations were used. The linear regression analysis for the effect of the serum lithium concentration on the agreement between TDCO and LiDCO revealed a slope of -1.530 (95% confidence interval [CI], -2.388 to -0.671) and a yintercept of 0.011 ( r 2 = 0.235). The linear regression analysis for the effect of the cumulative lithium chloride dosage on the serum lithium concentration revealed a slope of 2.291 (95% CI, 2.153 to 2.429) and a y-intercept of 0.008 (r 2 = 0.969). Conclusions and Clinical Relevance —The LiDCO measurement increased slightly as the serum lithium concentration increased. This error was not clinically relevant and was minimal at a serum lithium concentration of 0.1 mmol/L and modest at a concentration of 0.4 mmol/L. The serum lithium concentration can be reliably predicted from the cumulative lithium dosage if lithium chloride is administered often within a short period. ( Am J Vet Res 2002;63:1048–1052)
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Studies on the effects of lithium on drinking, food intake, locomotor activity and aggression in rats are reviewed. Particular attention is paid to the dosage, concentration, route and schedule of lithium treatments. The effects of lithium on behavior are found to depend on the experimental methods. The main effects of lithium treatments on rat behavior are found to be prevention of the reoccurrence of certain behaviors, enhancement of intake of water and sodium chloride solutions, suppression of some types of spontaneous and drug-induced activity, production of hyperactivity when given together with MAO inhibitors, reduction of some types of aggressive behavior, enhancement of morphine analygesia and reduction of morphine intake. The relationship between the outcome of studies on behavior in rats given lithium and the use of lithium salts to treat human disorders is briefly discussed.
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1 Addition of lithium carbonate (55 mmol/kg dry wt.) to the diet of rats for 4 days resulted in ratios between lithium in the brain and serum and between the cerebrospinal fluid (CSF) and serum of approx. 1 and 0.4, respectively. The relationships between the concentrations were linear. 2 After single intraperitoneal injections of lithium chloride (5 mmol/kg body wt.) the concentration of lithium in the CSF was greater than that of the brain for 2 h. 3 Repeated subcutaneous injections of lithium chloride (0.9 mmol/kg body wt.) resulted in steady state ratios corresponding to those observed when lithium was given in the diet. The rate of elimination from the CSF was intermediate between that of the serum and cerebral tissue until a new equilibrium was reached after approx. 24 h. At that time the ratios between lithium in the brain and serum, and in the CSF and serum were increased to approx. 5 and 0.8, respectively. 4 These results are consistent with passive transfer kinetics of lithium in the CSF and elimination of lithium from the cerebral tissue via the CSF. 5 The results may explain some of the phenomena observed in patients during intoxication with lithium.
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Lithium has been successfully employed to treat bipolar disorder for decades, and recently, was shown to attenuate the symptoms of other pathologies such as Alzheimer's disease, Down's syndrome, ischemic processes, and glutamate-mediated excitotoxicity. However, lithium's narrow therapeutic range limits its broader use. Therefore, the development of methods to better predict its dose becomes essential to an ideal therapy.the performance of adult Wistar rats was evaluated at the open field and elevated plus maze after a six weeks treatment with chow supplemented with 0.255%, or 0.383% of lithium chloride, or normal feed. Thereafter, blood samples were collected to measure the serum lithium concentration.Animals fed with 0.255% lithium chloride supplemented chow presented a higher rearing frequency at the open field, and higher frequency of arms entrance at the elevated plus maze than animals fed with a 50% higher lithium dose presented. Nevertheless, both groups presented similar lithium plasmatic concentration.different behaviors induced by both lithium doses suggest that these animals had different lithium distribution in their brains that was not detected by lithium serum measurement.serum lithium concentration measurements do not seem to provide sufficient precision to support its use as predictive of behaviors.
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