624results about "Lithium halides" patented technology

The present disclosure relates to the extraction of lithium from underground reservoirs of naturally occurring brines. Described herein are systems and methods to extract lithium entrapped within reservoirs that were previously inaccessible.

This invention discloses a method for leaching lithium iron phosphate mixed powder with iron salts and recovering all components, belonging to the field of battery recycling. The invention uses an iron salt solution to leach the mixed powder, obtaining a lithium-containing leachate and leaching residue. Ferrous ions in the leachate are regenerated into ferric iron through acidification and oxidation, and recycled for leaching the next batch of mixed powder. After reaching a preset number of cycles, the leachate is used for re-leaching multiple batches of leaching residue to improve the lithium leaching rate. Ultimately, a enriched solution containing Li, Fe, Cu, and Al and graphite-containing iron phosphate residue are obtained. Copper is recovered from the enriched solution through iron powder replacement, and a high-purity lithium chloride solution is obtained through extraction and separation, while ferric chloride (recycled) and aluminum chloride crystals are also recovered. The leaching residue is treated with hydrochloric acid to obtain regenerated graphite, and the pH is adjusted with alkali to obtain high-purity iron phosphate. This method achieves full component recovery under mild conditions, reducing separation steps and chemical consumption through a "leaching-regeneration-leaching" cycle mechanism, thus achieving both environmental and economic benefits.

The present application discloses a method for recovering battery-grade iron phosphate and lithium salts from lithium iron phosphate waste materials and its application, comprising the following steps: S100, dissolving the lithium iron phosphate waste materials with a phosphoric acid solution, filtering to obtain a waste material dissolution solution; S200, adding an acid solution and an oxidant to the waste material dissolution solution to obtain a crystallization stock solution; S300, diluting the crystallization stock solution with water until its pH value is 1.0 to 1.5, and performing high-temperature crystallization to obtain hydrated iron phosphate and a lithium-containing filtrate; S400, roasting the hydrated iron phosphate to obtain battery-grade iron phosphate; S500, removing water from the lithium-containing filtrate to obtain solution a, circulating solution a to dissolve the lithium iron phosphate waste materials, and concentrating to obtain lithium salts. The present application uses a phosphoric acid solution as the leaching solvent, does not require the use of an alkali solution subsequently and can be leached cyclically, improving the economic benefits while enabling the efficient recovery of all elements of Li, Fe, and P, and also capable of obtaining a battery-grade iron phosphate product with an iron-to-phosphorus ratio meeting the requirements.

The invention provides lithium fluoride as well as a preparation method and application thereof. The mass content of carbonate in the lithium fluoride is less than or equal to 1000mg / kg; d10 of the lithium fluoride is smaller than or equal to 10 microns, D50 of the lithium fluoride is smaller than or equal to 20 microns, and the bulk density of the lithium fluoride is 0.9-1.2 g / cm < 3 >. The lithium fluoride provided by the invention has a specific size specification and relatively low carbonate impurity content, and the lithium fluoride is beneficial to preparation of electrolyte salt capable of improving the electrical performance of a battery.

The invention belongs to the technical field of lithium ion battery positive electrode materials, and provides a plasma-assisted in-situ constructed lithium ion conductor coated high-nickel ternary positive electrode material as well as a preparation method and application thereof. Oxygen plasma active groups are formed through high-pressure ionization of oxygen, and the generated active groups interact with gas generated by thermal decomposition of an added solid source; the residual alkali on the surface of the high-nickel ternary positive electrode can be consumed, and a thin, continuous and compact lithium ion conductor coating layer with good conductivity is formed on the surface of the high-nickel ternary positive electrode material in situ, so that the development of the high-nickel ternary positive electrode material of the lithium ion battery is promoted. The high-nickel ternary positive electrode material prepared by the invention shows high specific capacity, excellent cycling stability, rate capability and first charge-discharge efficiency. Meanwhile, the preparation method provided by the invention is simple, rapid, efficient, convenient and low in cost, the residual alkali on the surface of the high-nickel ternary positive electrode material can be effectively removed, and the structural stability of the high-nickel ternary positive electrode material is improved.

The invention discloses a method for extracting and recovering metal elements in lithium batteries using a chlorination method, which belongs to the technical field of lithium battery recovery. The method comprises the following steps: step 1, calcining the positive electrode sheet of the lithium battery to remove organic matter, and peeling off the aluminum foil to obtain electrode material powder; step 2, placing the electrode material powder on a carrier of a Joule heat device, and performing a thermal shock treatment under a chlorine atmosphere, and the treatment process is staged by stage heating and chlorination; step 3, desublimating the gas generated after chlorination in each stage; step 4, adding the solid after desublimation in each stage to deionized water, adding a sodium carbonate aqueous solution after mixing, collecting the precipitate, washing and drying to obtain a metal salt product. The present invention is based on the characteristics of Joule heat that can heat quickly and accurately control the temperature, combined with the difference in the temperature of the chlorination reaction of different metal oxides and the gasification temperature of the chlorination product, to achieve staged gasification and desublimation treatment, obtain different metal chlorides, and purify accurately and efficiently.

The invention belongs to the technical field of hybrid supercapacitors, and discloses a coal-based hard carbon negative electrode material with high slope lithium storage capacity and a preparation method and application of the coal-based hard carbon negative electrode material. Washing the pulverized coal subjected to impurity removal with ultrapure water until the pH value is neutral, and then drying; pre-oxidizing the pulverized coal in an air atmosphere at 280-320 DEG C for 110-130 minutes, switching a gas atmosphere into a protective atmosphere after the pre-oxidation is finished, continuously heating, carbonizing at 1180-1220 DEG C for 110-130 minutes, washing with an acid solution to be neutral after the carbonization is finished, and drying to obtain a carbon material subjected to heat treatment; impregnating the surface of the carbon material subjected to heat treatment with lithium fluoride; and carrying out heat treatment on the material A at 280-320 DEG C in a protective atmosphere for 280-320 minutes to obtain the coal-based hard carbon negative electrode material with high slope lithium storage capacity. The power and capacity performance of the hybrid super capacitor can be improved, the intrinsic safety of the device can be further improved, and the hybrid super capacitor has great practical significance.

The present disclosure provides novel compositions of matter and a robust one-pot process to produce solid-state electrolytes, metal sulfides, and / or metal phosphates. The metal sulfides include argyrodite-type sulfide electrolyte, and the metal phosphates include lithium phosphate.

The invention provides a lithium iron phosphate repair material and a repair and recovery method thereof, a positive plate and a lithium ion battery, and the repair and recovery method comprises the following steps: washing the positive plate disassembled from the lithium ion battery with an organic solvent to remove lithium salt in the positive plate; carrying out first calcination treatment on a to-be-treated object containing the positive pole piece after the lithium salt is removed so as to destroy a carbon coating layer and separate a positive active material layer from a positive current collector; and coarsely crushing the separated positive electrode active material layer, mixing the crushed positive electrode active material layer with a lithium supplementing material, and carrying out secondary calcination treatment on the mixed material to obtain the lithium iron phosphate repairing material. According to the repair and recovery method provided by the invention, large-scale environment-friendly repair and recovery of lithium iron phosphate in the waste lithium ion battery can be realized, and the lithium iron phosphate repair material with excellent cycle performance can be obtained.

The present invention discloses a method for preparing a solid electrolyte interface of an electrolyte material, which belongs to the technical field of new energy materials, and comprises the following steps: placing an electrolyte in a reaction chamber of a plasma device, and introducing a fluorine-containing gas for vacuum fluorination treatment to obtain an electrolyte having a fluoride layer on one side of the surface; and in-situ constructing a solid electrolyte interface layer between the electrolyte and the negative electrode through a reaction between the fluoride layer on one side of the electrolyte surface and the negative electrode, wherein the component of the solid electrolyte interface layer is LiF. The present invention solves the problem that the negative electrode side of the existing electrolyte is seriously lithium-repellent and not stable enough.

The invention provides lithium brine thallium removal equipment and a magnetic MOFs thallium removal agent preparation process thereof. The water pollution treatment device comprises a bottom plate, a tank body, a top cover, a mounting plate, a positioning frame, a driving mechanism and a discharging mechanism, the tank body is mounted on the upper surface of the bottom plate, the top cover is mounted on the upper surface of the tank body through bolts, the mounting plate is mounted on the upper surface of the top cover, and the positioning frame is mounted on the upper surface of the mounting plate. In the rotating process of the rotating drum, the rotating drum is automatically driven by the guide wheel to automatically ascend along with the thickness of the auxiliary plate, and when the guide wheel rotates to the vertical plane of the auxiliary plate, the guide wheel automatically falls to control the rotating drum to reset, so that the rotating drum can vertically move in the rotating process; in addition, small-amplitude vibration can be formed, so that the Fe3O4-coated UiO-66-NH2 nanoparticles are firstly treated into a liquid state and then are injected into the lithium leaching solution, and the concentration in the leaching solution can be ensured to be more uniform.

The invention belongs to the technical field of inorganic salt chemical industry. The invention provides a method for preparing anhydrous lithium chloride by using salt lake brine with low magnesium-lithium ratio, which comprises the following steps: pumping clear salt lake brine with low magnesium-lithium ratio into a plate-and-frame filter press for filtration, and sequentially performing microporous filtration and ultrafiltration on filtrate to obtain primary refined brine; filtering the primary refined brine through a nanofiltration membrane device to obtain secondary refined brine; allowing the secondary refined brine to pass through chelating resin to obtain magnesium-removed brine; mixing the magnesium-removed brine with an alkali solution, adjusting the pH value of the mixed solution, and pumping the mixed solution into a continuous extraction device for solvent extraction to obtain a lithium chloride solution; and evaporating and drying the lithium chloride solution in sequence to obtain an anhydrous lithium chloride product. The anhydrous lithium chloride product is prepared by adopting a nanofiltration membrane separation and solvent extraction combined process, the recovery rate of lithium ions is higher than 80%, the fresh water consumption of 1 ton of lithium chloride product is less than 50 cubic meters, the production cost is low, the chemical units are few, and the automation degree is high.

The utility model discloses a lithium chloride mother liquor refining system for extracting lithium from a salt lake, which comprises a sodium sulfate dissolving kettle, a primary crystallization reaction kettle, a primary plate-and-frame filter press, a secondary crystallization reaction kettle, a secondary plate-and-frame filter press, a microporous filter element filter, nano-filtration equipment, a resin adsorption filter, a filter residue stirring kettle and a precipitation residue filter press, the sodium sulfate dissolving kettle is communicated with the interior of the primary crystallization reaction kettle through a sodium sulfate solution pipeline, the filter residue stirring kettle is communicated with slag outlets of the primary plate-and-frame filter press and the secondary plate-and-frame filter press, and the filter residue stirring kettle is communicated with the interior of the sodium sulfate dissolving kettle through a precipitation slag filter press. Compared with the prior art, the lithium chloride mother liquor is used as a raw material, insoluble impurities, soluble ions and organic matters in the raw material are removed through deep crystallization and impurity removal, solid-liquid separation of precipitates is easy, and meanwhile, entrainment of lithium ions in the precipitates is reduced, so that lithium chloride refined liquor is obtained, and 99.9% battery-grade lithium carbonate can be directly prepared in a lithium precipitation process.

The invention relates to a preparation method of a membrane material, in particular to a preparation method of a nanofiltration membrane applied to magnesium-lithium separation. According to the preparation method of the polyamide nanofiltration membrane capable of avoiding the acyl chloride hydrolysis influence, provided by the invention, the acyl chloride hydrolysis is avoided by mainly utilizing interfacial polymerization of gas-phase amine and acyl chloride, and the application potential of the membrane can be well improved by adopting the hollow fiber as the support body.

Methods and systems for direct-write liquid phase epitaxy of ionic materials are provided for herein, and relate to the manufacture of metal halide optics among other applications. Deposition of the ionic material is induced by mixing at least two fluids of differing composition, wherein the solubility limit of the ionic material in the mixed solution is lower than predicted from a linear combination of the original fluids. This deposition process is spatially controlled using a printhead, enabling localized material deposition and the ability to create arbitrary geometries in turn. In some cases, at least one of the fluids is saturated with the ionic material and surrounds the substrate upon which deposition occurs.

The invention belongs to the technical field of sodium-ion battery positive electrode material preparation, and particularly discloses a double-modified sodium-ion battery layered oxide positive electrode material and a preparation method thereof, and the preparation method comprises the following steps: S1, synthesizing a P2-type sodium-ion battery nickel-manganese-based layered oxide by using a high-temperature solid-phase method; s2, uniformly mixing two or more of lithium fluoride, sodium fluoride, calcium fluoride or magnesium fluoride in proportion to prepare a multi-element fluoride coating material; and S3, uniformly mixing the P2-type sodium-ion battery nickel-manganese-based layered oxide and the multi-fluoride coating material according to a ratio, and then carrying out high-temperature quenching treatment to obtain the surface fluoride-coated and near-bulk-phase-doped dual-modified sodium-ion battery layered oxide positive electrode material. According to the dual-modified layered oxide positive electrode material for the sodium-ion battery and the preparation method, surface fluoride coating and near bulk phase doping are cooperatively utilized, so that the high-voltage cycle performance of the layered oxide positive electrode material for the sodium-ion battery is improved.

The present disclosure provides a method of recovering a spent battery cathode material comprising lithium and at least one of nickel, cobalt and / or manganese, the method comprising: heating the spent battery cathode material in a reducing atmosphere to form a heat-treated spent battery cathode material comprising LiF and one or more of LijO, LiOH and LijCOs; washing the heat treated waste battery cathode material in an aqueous solvent to extract lithium-containing species and fluorine-containing species wherein the aqueous solvent is free of alkaline earth metal hydroxides or other species intended to reduce or prevent soluble fluorine species from remaining dissolved in the aqueous solvent; separating an aqueous solvent comprising lithium and fluorine species from the heat treated waste battery material; after separating an aqueous solvent comprising lithium and fluorine species from the heat-treated waste battery material, treating the aqueous solvent to separate lithium species from fluorine species; recycling a lithium substance in the form of lithium hydroxide or lithium carbonate; forming an acidic aqueous recovery feed comprising one or more of nickel, cobalt and / or manganese by leaching the heat treated waste battery cathode material with a mineral acid after the step of separating the aqueous solvent from the heat treated waste battery material; and recovering one or more of nickel, cobalt and / or manganese from the acidic aqueous recovery feed by a further process step selected from one or more of solvent extraction, solid phase extraction, electrochemical extraction and precipitation processes.

The invention relates to a composite lithium supplementing material, a preparation method thereof and a secondary battery. The composite lithium supplementing material comprises secondary particles, the secondary particles comprise a plurality of primary particles and a functional additive, at least part of the functional additive is distributed among the primary particles, the primary particles are lithium-rich particles, and the functional additive comprises one or more of a conductive agent, a dispersing agent and a catalyst. The composite lithium supplementing material has relatively good conductivity, ion conductivity and dispersing performance or relatively low lithium removal decomposition voltage, so that the composite lithium supplementing material has relatively good coating performance and processing performance.

The invention provides a boron gradient-doped positive electrode precursor and a preparation method thereof, a positive electrode material and a battery. The positive electrode precursor comprises a boron-doped ternary material core and a boron-doped ternary material layer coated outside the boron-doped ternary material core, the mass fraction of the boron element in the boron-doped ternary material core is lower than that of the boron element in the boron-doped ternary material layer. In the boron gradient-doped positive electrode precursor provided by the invention, boron doping is performed in the boron-doped ternary material core and the boron-doped ternary material layer, so that a B-O bond with relatively high bond energy is formed, and lattice stress accumulation in the positive electrode precursor is reduced, thereby improving the structural stability and thermal stability of the positive electrode precursor and the positive electrode material; in addition, through gradient doping of boron, the electrochemical performance of the positive electrode material is ensured, the surface and interface structure of the positive electrode precursor is strengthened, the expansion of cracks is inhibited, and the structural stability of the positive electrode precursor is improved.

The present invention provides a method for producing lithium hydroxide, comprising the steps of reacting lithium carbonate and calcium hydroxide in a liquid to obtain a solution containing lithium hydroxide, and performing solid-liquid separation on the solution into a liquid component containing lithium hydroxide and a solid component containing lithium derived from the lithium carbonate, and recovering lithium hydroxide from the liquid component.

The invention discloses a salt lake brine evaporative crystallization method and device, and the crystallization method comprises the following steps: spreading and straightening a brine absorbing cloth, setting the included angle between the brine absorbing cloth and the horizontal plane to be 80-90 degrees, immersing the lower end of the brine absorbing cloth in brine, and carrying out evaporative crystallization; after evaporative crystallization, the lower end of the halogen absorbing cloth is removed from the brine, and salt on the halogen absorbing cloth is collected; the aperture of the halogen absorbing cloth is lt; the top end of the halogen absorbing cloth is positioned at the height gt above the brine; 7 m. Under the action of wind energy and solar energy, the brine evaporation speed of the brine absorption cloth per unit area is more than 20 times that of the salt pan solar pond per unit area, and the occupied area of the evaporation device and the salt pan can be effectively reduced.

The invention discloses a fused salt purification method and a fused salt purification device.The fused salt purification method comprises the following steps that S1, in an oxygen-free and water-free operation environment, fused salt is put into a reaction container, firstly, the fused salt is heated to a first preset temperature and kept for a first preset duration, and then the fused salt is heated to a second preset temperature and kept for a second preset duration; s2, mixed gas of HCl and H2 is introduced into the reaction container heated to the second preset temperature, HCl is cut off after a period of time, then H2 is used for bubbling for a period of time, inert gas is introduced for bubbling, residual HCl and H2 in the molten salt are removed, and purified molten salt is obtained. The molten salt purification device comprises a gas supply system, a reaction container and a storage container, the device can treat kilogram-level chlorine salt in batches, and the molten salt purification efficiency is high.

The invention provides a preparation method of battery-grade lithium salt, and relates to the technical field of new energy materials. Starting from battery-grade lithium sulfate, part of lithium sulfate is reduced under hydrogen to obtain battery-grade lithium sulfide; part of lithium sulfate reacts with sodium carbonate to obtain battery-grade lithium carbonate, the battery-grade lithium carbonate reacts with hydrochloric acid to obtain lithium chloride, lithium chloride is electrolyzed to obtain metal lithium, and the metal lithium reacts with sulfur, is reduced and is converted into battery-grade lithium sulfide; part of lithium sulfate reacts with sodium hydroxide to obtain battery-grade lithium hydroxide, and then the battery-grade lithium hydroxide reacts with hydrogenation tail gas to obtain battery-grade lithium sulfide. Further, the battery-grade lithium sulfide can be obtained from the lithium-containing ore through the steps of calcination, sulfuric acid leaching, purification and the like. Through conversion and adjustment among different lithium salts, the cost of the lithium sulfide can be adjusted according to different conditions, and low-cost and large-scale mass production of the lithium sulfide is realized.

The present disclosure provides various characteristics for treating tail brine extracted from a bromine plant, when said brine contains residual bromine and chlorine with low pH and high ORP values that will be used in a lithium extraction production facility. The method conditions the extracted tail brine by adding either sodium hydroxide or ammonium hydroxide to bring its pH levels to between 5.5 and 6.5. The conditioned tail brine then gets pre-treated with hydrazine in either less than 70 ppm if used in combination with sodium hydroxide; or 195 ppm if used with ammonium hydroxide until the ORP levels have reached to below 100 mV. The extracted tail brine is then processed through DLE processing device having four groups of adsorption columns filled with lithium adsorption resins that, after treating the extracted tail brine, discharges the raw eluate solution to an effluent tail brine tank using an effluent tail brine pump connected to the DLE processing device.

The present invention belongs to the technical field of lithium chloride purification, and specifically relates to a method and a device for purifying lithium chloride containing organic matter. The method for purifying lithium chloride containing organic matter comprises the following steps: calcining the organic lithium chloride raw material under an oxygen-containing atmosphere, dissolving the obtained sintered product in a dissolving solution, filtering to obtain a purified solution, then subjecting it to N-level precipitation filtration cold box treatment, recovering the obtained filtrate as a dissolving solution for recycling, and drying the obtained solid to obtain a lithium chloride product; the dissolving solution comprises an organic solvent I and an organic solvent II, the organic solvent I is selected from at least one of pyrrolidone solvents, amide solvents, lactam solvents, and piperidone solvents, and the organic solvent II is selected from urea solvents and / or alcohol solvents. The purification method provided by the present invention obtains a high-purity lithium chloride product through the mutual cooperation of various processing steps, and the yield is high, and the recovered solvent has a low impurity content and can be recycled for a long time.

The disclosed subject matter relates to solid state lithium ion conductors and batteries (such as pseudo solid state and all solid state batteries), and methods of making and use thereof. For example, disclosed herein are solid state lithium ion conductors comprising: Li3+2x+yzM [III+z]X6-x-yNxOy, wherein M is an alkali metal, an alkaline earth metal, a transition metal, a post transition metal, or a combination thereof; X is a halide; x is from 0 to 6; y is from 0 to 6; z is from -2 to 2; and [III+z] represents the valence of the M-ion(s); with the proviso that: M is not Li; 0 < x + y ≤ 6; and 0 < (3+2z+y-z) ≤ 6. Also disclosed herein are methods of making and use of any of the solid state lithium ion conductors disclosed herein, for example in devices such as a solid state battery.

The invention discloses a method for circularly leaching lithium iron phosphate mixed powder from ferric salt and recovering all components, and belongs to the field of battery recovery. The method comprises the following steps: leaching mixed powder by adopting an iron salt solution to obtain a lithium-containing leaching solution and leaching residues; ferrous ions in the leachate are regenerated into ferric iron through acidification and oxidation, the ferric iron is cyclically used for leaching the next batch of mixed powder, after the preset cycle number is reached, the leachate is used for re-leaching treatment of multiple batches of leaching residues, and the lithium leaching rate is increased. And finally obtaining enriched liquid containing Li, Fe, Cu and Al and iron phosphate slag containing graphite. And replacing the enriched liquid with iron powder to recover copper, extracting and separating to obtain a high-purity lithium chloride solution, and simultaneously recovering ferric chloride (recycling) and aluminum chloride crystals. And treating the leaching residues with hydrochloric acid to obtain regenerated graphite, and adjusting the pH value with alkali to obtain high-purity iron phosphate. According to the method, all-component recovery is achieved under the mild condition, separation steps are reduced through a leaching-regeneration-leaching circulation mechanism, chemical consumption is reduced, and the method has both environmental and economic benefits.

Producing high purity lithium solution from a source brine containing at least 1 mg Li / kg brine, preferably 10 mg / kg, more preferably 25 mg Li / kg brine; treating the source brine, if necessary in pretreatment steps; processing the treated brine in a lithium adsorption step; after the adsorption step, desorbing the adsorbed lithium in a desorption step; after the desorption step, treating the desorption effluent in an enrichment step. Specified optional steps and new features can be used to increase lithium concentrations and purity.

The invention relates to a method for high-value recovery of a positive electrode material of a waste lithium iron phosphate battery, which mainly comprises the following steps: adding a lithium iron phosphate positive electrode material, ammonium chloride and hydrogen peroxide into a ball milling tank for grinding, controlling the mass ratio of the ammonium chloride to the lithium iron phosphate positive electrode material to be 5: 2-7: 2, and controlling the volume mass ratio of the hydrogen peroxide to the lithium iron phosphate positive electrode material to be (18-22): 1mL / g; after grinding, washing out the mixture from the ball-milling tank by using deionized water, and then carrying out water leaching treatment to fully leach out metal lithium; excessive ammonium fluoride is added into the filtrate, and reaction liquid and a product lithium fluoride are obtained after reaction; and carrying out adsorption treatment on the reaction liquid by using defluorination resin, regenerating the defluorination resin through elution, combining and concentrating the collected effluent and eluent to obtain an ammonium chloride solution, and recycling the ammonium chloride solution to a chlorination reaction stage. According to the invention, through H2O2 reinforced mechanical chlorination coupling fluorination reaction, nearly total recovery of the waste lithium iron phosphate battery positive electrode material and high value of the product are realized, and the process is simpler and more environment-friendly.

The present disclosure introduces advanced techniques for critical mineral processing using solid electrolyte membranes. In particular, a novel electrolytic and environmental direct lithium extraction (MOBILE) process, may be used comprising an extractor unit featuring alternating lithium and sodium storage modules, a lithium collection tank, and a precipitation stage. The MOBILE process offers several key advantages over traditional methods, including enabling selective lithium extraction from low-concentration feed solutions while reducing chemical consumption and minimizing environmental impact. Furthermore, the MOBILE process demonstrates faster extraction times and superior adaptability to diverse feed solution compositions. Its modular and scalable design allows for flexible adaptation to various feed solutions and production capacities, making it a versatile solution for lithium extraction across different scenarios. The MOBILE process represents a significant advancement in critical mineral processing, offering a more efficient, environmentally friendly, and adaptable method for lithium extraction and related mineral processing applications.