Synthesis of nanostructured battery materials

Abstract

The systems and methods of this disclosure describe synthesis techniques for nanoscale battery materials. In one or more examples, this disclosure provides one or more frameworks for precisely controlling the size and morphology of battery materials during synthesis using microemulsions. In one or more examples, this disclosure also provides one or more frameworks for precisely controlling the size and morphology of battery materials during synthesis even when microemulsions are not formed.

Description

Technical Field

[0001] (Cross - reference to related applications) This patent application claims the benefit of priority of U.S. Patent Application No. 63 / 514,721, filed on July 20, 2023, and the entire disclosure of that application is incorporated herein by reference.

[0002] (Technical Field) This application generally relates to compositions of battery materials and methods for manufacturing the same.

Background Art

[0003] The energy density of lithium - ion batteries is typically limited by the specific capacity of their cathodes. The high - nickel stoichiometric composition of LiNi x Mn y Co z O2, where x ranges from about 0.4 to 0.95, shows a sufficiently high cycle life for use in applications such as electric vehicles, but its specific capacity is still limited to a maximum of about 200 milliampere - hours (mAh) / gram (fully charged state). In contrast, graphite, which is a state - of - the - art anode active material, shows a much higher specific capacity of 350 - 372 mAh / g in the fully charged state. As a result, increasing the specific capacity of the cathode is the means to relatively most significantly improve the cell - level energy density of lithium - ion batteries.

Brief Description of the Drawings

[0004] [Figure 1] A diagram showing a process for generating battery material particles using an aqueous solution containing one or more co - solvents, according to one or more embodiments. [Figure 2] A diagram showing a framework for generating battery material particles using microemulsions, according to one or more embodiments.

Best Mode for Carrying Out the Invention

[0005] LiRing x Mn y Co z While cathode materials such as O2 can be charged to specific capacities exceeding 200 mAh / g by increasing the upper limit of the charging voltage, this significantly reduces the cycle life. High-voltage degradation is primarily due to the mechanical stress and strain on the cathode caused by repeated lithium insertion and deinsertion across a wide range of lithium mole fractions, leading to cathode particle fatigue and eventual crack formation. Cathode materials are polycrystalline "secondary" particles composed of numerous primary crystal grains, and are susceptible to fracture along grain boundaries between primary crystal grains during cycling. When this occurs, new cathode surfaces are exposed to the electrolyte, increasing the areas where high-impedance decomposition products accumulate and where transition metals leach from the cathode crystal lattice, effectively destroying the active material. Furthermore, cracked fragments of cathode material can be electrically isolated from the rest of the electrode matrix and become inert material.

[0006] Reducing the grain boundary area per unit mass of the cathode active material may suppress such surface-related degradation phenomena. One way to significantly reduce the proportion of grain boundaries in the cathode active material is to increase the size of the primary crystal grains, mainly by firing at high temperatures (i.e., above approximately 950°C). High-temperature firing promotes grain growth and reduces the electrochemically available surface area when secondary particles are fractured.

[0007] However, increasing the calcination temperature when synthesizing cathode active materials using state-of-the-art coprecipitation processes has the adverse effect of causing excessive aggregation of secondary particles. Therefore, the final synthesized secondary particles need to be ground and sieved to achieve the desired particle size distribution, which is an undesirable additional manufacturing step. Furthermore, the ground secondary particles may require a secondary annealing step at a temperature slightly lower than the calcination temperature to repair defects caused during grinding, which is also an undesirable additional step.

[0008] The conventional co-precipitation process for synthesizing cathode active material precursors can be easily optimized to obtain a desired particle size in the range of about 1 μm to 50 μm, with a median value of about 10 μm. The precursors are usually mixed metal hydroxides or carbonates, and during synthesis, the primary crystallites rapidly aggregate to form secondary particles of 1 to 50 μm. If the temperature during the subsequent calcination process required to convert the active material precursor to the final oxide analog is kept below about 900 °C, little aggregation between secondary particles is observed, and the desired particle size distribution is maintained. However, when the calcination temperature exceeds 950 °C, the same mechanism that promotes grain growth of the primary crystallites also promotes sintering between secondary particles, causing particle aggregation.

[0009] If the secondary particle size can be more precisely controlled at the precursor stage of synthesis, it would be very helpful for obtaining the desired final particle size distribution even during high-temperature calcination. For example, if the precursor secondary particles can be synthesized reproducibly with a size of less than 1 μm and a narrow particle size distribution, when finally calcined at 900 °C to 1000 °C, the final secondary particle dimensions will be in the desired range of 1 μm to 50 μm, eliminating the need for additional processes such as grinding, milling, sieving, and annealing. Therefore, there is a need for new synthesis technologies for uniformly manufacturing primary particles for battery active materials with a particle size of less than 1 μm.

[0010] The state-of-the-art lithium-ion cathode material LiNi x Mn y Co z In addition to O2, there are many battery materials whose performance is greatly improved by reducing the particle size to the nanoscale. For example, the cathode material LiFePO4 has a relatively low specific output due to the relatively low solid diffusivity of lithium within its crystal lattice, but it has been observed that when the particle size is reduced to less than 1 μm, the rate performance is significantly improved. Other cathode materials with low electronic conductivity, such as the conversion-type cathode FeF3, have also been shown to have improved rate performance by reducing the active material particle size to the nanoscale. Furthermore, lithium ketomalonate, a lithium-containing compound that is usually inert and highly resistive but has a high specific capacity (exceeding 400 mAh / g), also exhibits a potential of about 4 V (Li / Li +It can be electrochemically activated at a reasonable oxidation potential (reference). Finally, anode materials such as lithium titanates, although having low electronic and ionic conductivity, have been observed to show significantly improved rate properties when the particle size is reduced to the nanoscale.

[0011] A useful feature of the coprecipitation process in battery material manufacturing is that secondary particles typically do not grow to a size significantly larger than 50 μm. Secondary particle sizes of 1 μm to 50 μm are typical for LiNi x Mn y Co z This method provides good lithium insertion dynamics for materials with sufficient rate characteristics, such as O2. Furthermore, the coprecipitation process readily generates spherical particles, resulting in good tap density and minimized active material surface area, thus suppressing surface-related degradation phenomena.

[0012] However, while the coprecipitation process can reliably produce particle sizes from 1 μm to 50 μm, it is difficult to obtain particle sizes smaller than 1 μm with a narrow size distribution and electrochemical and morphological properties equivalent to those of larger particle sizes. This is because the reaction conditions required to obtain the desired stoichiometry and morphology of the coprecipitation cathode material precursor are strongly linked to the resulting particle size. For example, precursor Ni x Mn y Co z In the case of (OH)2, synthesis at a high pH (i.e., above approximately 11.5) results in smaller particle size, but the morphology is irregular and the size distribution is broad. In contrast, synthesis at a more moderate pH (10.5-11) yields smooth, spherical particles with a narrow size distribution, but the average particle size is much larger. Therefore, in existing coprecipitation processes, there is currently no method to separate the control of cathode precursor particle size from the control of size distribution and morphology.

[0013] Limiting reagent access to the precursor nucleus surface during synthesis through some form of particle confinement or surface protection is one way to limit the size of the cathode precursor. This approach is commonly used, for example, in the solution-phase synthesis of colloidal dispersions of nanoparticles, where the nanoparticle surface is stabilized by the addition of a "ligand." Ligands are typically short-chain molecules, with one end group strongly coordinating to the nanoparticle surface after nucleation and the other end strongly coordinating to a solvent molecule to maintain particle dispersion. The ligand forms a capping shell around the nanoparticle, preventing additional reagents from reacting with the particle surface and thus limiting further growth. Utilizing ligand-based particle confinement is particularly useful for creating relatively monodisperse nanoparticle dispersions with an average size of a few nanometers.

[0014] Microemulsions offer another option for synthesizing larger nanoparticles and micron-sized particles while keeping them confinated. A microemulsion is a dispersion of two immiscible solvents stabilized by the presence of a surfactant. Microemulsions are typically characterized as water-in-oil (o / w) or oil-in-water (w / o) dispersions, but this concept can be generalized to various combinations of solvents with sufficiently different polarities and miscibility. While microemulsions often appear macroscopically homogeneous, in reality, one phase is dispersed in the other phase as tiny micelles, and because the micelles are small in size and uniformly distributed, the mixture as a whole is optically transparent with no scattering. Microemulsions are useful for the controlled synthesis of nanoparticles with uniform particle size distribution and morphology because the micelles function as "nanoractors," where size-restricted synthesis takes place.

[0015] Microemulsions are highly suitable for synthesizing battery materials because particle sizes can be uniformly controlled in the range of single-digit nanometers to several microns. The morphology and particle size of the battery material can be precisely controlled by varying the composition and relative amounts of the two immiscible phases, the type and amount of the main surfactant and co-surfactant, and process parameters such as temperature and ambient pressure.

[0016] Embodiments of this specification aim to generate battery material particles having one or more dimensions of 1 μm or less without using grinding processes or other particle size reduction processes. For example, a microemulsion can be generated and used to generate battery material particles. The microemulsion may include a first phase consisting of a first solution and a second phase consisting of a second solution. In various examples, the second phase may include droplets dispersed in the first phase. The composition of the second solution may include precursors of the battery material particles. In one or more examples, one or more reactions with respect to compounds in the second solution may proceed within the droplet to generate battery material particles. The droplet may have dimensions that limit the size of the battery material particles generated within it. For example, the droplet may have dimensions that limit one or more dimensions of the battery material particles to less than 1 μm.

[0017] In one or more further examples, an additional co-solvent other than water may be introduced into the reaction solution as a way to influence the particle size when precipitating the battery material and its precursors from the solution. In these embodiments, battery material particles having one or more dimensions of 1 μm or less can be produced without a grinding process or other particle size reduction process.

[0018] As an example, in the synthesis of Ni(OH)2, a battery material precursor, a 50:50 water-methanol mixture can be used instead of 100% water. In this example, the pH of the solution and the precipitation of hydroxide can be controlled by adding ammonia. As another example, lithium-containing compounds such as lithium ketomalonate can be synthesized using a water:methanol solvent mixture. In this case, LiOH is first added to the 50:50 water-methanol mixture. After the hydroxide dissolves, ketomalonic acid is added to the reaction solution. The product, lithium ketomalonate, is extremely soluble in the reaction solution and therefore precipitates.

[0019] Using multiple solvents in a reaction solution has diverse effects on the size of precipitated particles. For example, the solubility of the final product (such as metal hydroxides or salts) differs significantly in organic solvents compared to water, often being lower. This promotes nucleation, resulting in a tendency for smaller particle sizes. Adding solvents other than water also affects the overall dielectric constant, influencing ionic solvation and ion-pair interactions. This, too, increases local supersaturation, promoting nucleation and further reducing particle size.

[0020] Figure 1 shows the process of generating battery material particles using an aqueous solution containing one or more cosolvents. This figure illustrates process 100 according to one or more embodiments. Process 100 can be carried out according to multiple techniques for producing battery material particles. For example, process 100 may include microemulsion process operations that can be carried out to produce battery material particles. Furthermore, process 100 may include non-microemulsion process operations for producing battery material particles. In addition, some operations of process 100 may be generally the same between microemulsion and non-microemulsion processes, but the specific implementation of these operations may differ.

[0021] Process 100 can be carried out in one or more reaction vessels, the capacity of which each reaction vessel may be at least 0.1 liters (L), at least 0.5 L, at least 1 L, at least 2 L, at least 5 L, at least 10 L, at least 25 L, at least 50 L, at least 75 L, at least 100 L, or at least 250 L. In one or more exemplary examples, process 100 can be carried out in one or more reaction vessels, each with a capacity ranging from about 0.1 L to about 500 L, about 1 L to about 400 L, about 2 L to about 300 L, about 5 L to about 200 L, about 10 L to about 100 L, about 0.1 L to about 1 L, about 1 L to about 10 L, about 10 L to about 50 L, about 50 L to about 100 L, about 100 L to about 150 L, about 150 L to about 200 L, about 200 L to about 250 L, about 250 L to about 500 L, or about 500 L to about 1000 L. In one or more examples, one or more reaction vessels used to carry out process 100 may include one or more mixing devices. One or more mixing devices may include one or more stirring mixers. For example, one or more mixing devices may include one or more rotating paddles. In one or more further examples, one or more mixing devices may include one or more jet mixers. In yet another example, one or more mixing devices may include one or more supersonic mixers. One or more reaction vessels used to carry out process 100 may further include or be connected to one or more temperature control devices. One or more temperature control devices may operate to heat or cool the liquid in one or more reaction vessels. One or more temperature control devices may include at least one of one or more electric heating elements, one or more chemical heating elements, one or more flame heating elements, one or more heat exchangers, one or more refrigeration elements, one or more fans, or one or more ventilation devices.

[0022] Process 100 may include preparing an initial solution in 102. The initial solution may include an aqueous solution and one or more cosolvents. In non-microemulsion embodiments, the preparation of the initial solution may include operation 104. In 104, process 100 may include combining water and one or more cosolvents, which are soluble in water and may be soluble in each other. In various examples, one or more cosolvents may be soluble in water and in each other at a temperature of about 15°C to about 30°C and a standard pressure of about 101 kilopascals (kPa). In further examples, one or more cosolvents may be soluble in water and in each other at a temperature above about 30°C and a pressure above about 101 kPa.

[0023] In one or more examples, one or more cosolvents may contain one or more alcohols. For example, one or more cosolvents may contain one or more alcohols whose carbon chains consist of 10 or fewer, 9 or fewer, 8 or fewer, 7 or fewer, 6 or fewer, 5 or fewer, 4 or fewer, 3 or fewer, 2 or fewer, or 1 or fewer carbon atoms. Furthermore, one or more cosolvents may contain one or more alcohols having rings in which each ring consists of 6 or fewer, 5 or fewer, or 4 or fewer carbon atoms. In one or more exemplary examples, one or more cosolvents may contain one or more alcohols having aliphatic chains. In yet another exemplary example, one or more cosolvents may contain one or more alcohols having carbon chains with at least one alkenyl group. In yet another exemplary example, one or more cosolvents may contain one or more single-bonded cyclic alcohols or one or more phenolic alcohols. In at least some exemplary examples, one or more cosolvents may contain one or more alcohols having unsubstituted carbon atoms. In yet another example, one or more cosolvents may contain one or more alcohols having one or more substituted carbon atoms. If one or more cosolvents contain one or more alcohols having one or more substituted carbon atoms, the carbon atoms may be substituted with at least one methyl group, amino group, carboxylate group, or nitro group. In various exemplary examples, one or more cosolvents may include methanol. In one or more further examples, one or more cosolvents may include ethanol.

[0024] In one or more additional examples, water can be combined with one or more cosolvents, and the initial solution may contain at least 40 vol% water, at least 45 vol% water, at least 50 vol% water, at least 55 vol% water, at least 60 vol% water, at least 65 vol% water, or at least 70 vol% water. In one or more exemplary examples, the initial solution may contain about 40 to about 75 vol% water, about 50 to about 70 vol% water, about 45 to about 55 vol% water, about 50 to about 60 vol% water, about 55 to about 65 vol% water, about 60 to about 70 vol% water, or about 65 to about 75 vol% water.

[0025] Furthermore, the initial solution may contain at least 25 vol% of one or more co-solvents, at least 30 vol% of one or more co-solvents, at least 35 vol% of one or more co-solvents, at least 40 vol% of one or more co-solvents, at least 45 vol% of one or more co-solvents, at least 50 vol% of one or more co-solvents, or at least 55 vol% of one or more co-solvents. In one or more additional exemplary examples, the initial solution may contain about 25 vol% to about 60 vol% of one or more co-solvents, about 30 vol% to about 50 vol% of one or more co-solvents, about 40 vol% to about 50 vol% of one or more co-solvents, about 45 vol% to about 55 vol% of one or more co-solvents, or about 50 vol% to about 60 vol% of one or more co-solvents.

[0026] In one or more additional examples, the volume ratio of the amount of one or more co-solvents present in the initial solution to the amount of water present in the initial solution may be about 0.7:1.3 to about 1.3:0.7, about 0.8:1.2 to about 1.2:0.8, about 0.85:1.15 to about 1.15:0.85, about 1.1:0.9 to about 0.9:1.1, and about 0.95:1.05 to about 1.05:0.95. In yet another example, the volume ratio of the amount of one or more co-solvents present in the aqueous solution to the amount of water present in the aqueous solution may be about 1:1. In various exemplary examples, the initial solution may contain about 50% by volume of water and about 50% by volume of one or more alcohols. The one or more alcohols may include methanol or ethanol.

[0027] Water and one or more co-solvents can be combined at temperatures ranging from about 10°C to about 60°C, about 15°C to about 50°C, about 20°C to about 40°C, about 15°C to about 25°C, about 20°C to about 30°C, about 25°C to about 35°C, or about 30°C to about 40°C. The initial solution can also be prepared at pressures ranging from about 80 kPa to about 130 kPa, about 90 kPa to about 120 kPa, or about 100 kPa to about 110 kPa. In one or more examples, water and one or more co-solvents can be mixed for about 15 seconds to about 30 minutes, about 1 minute to about 20 minutes, about 2 minutes to about 10 minutes, about 30 seconds to about 5 minutes, about 1 minute to about 3 minutes, about 2 minutes to about 4 minutes, or about 3 minutes to about 5 minutes.

[0028] In cases where a microemulsion is produced by process 100, the preparation of the initial solution may include, in 106, combining water with at least two immiscible reagents. In one or more examples, the at least two immiscible reagents may include one or more first reagents. One or more first reagents may include at least one of methanol, ethanol, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, acetone, one or more grimes, and one or more ethers. In one or more exemplary examples, one or more first reagents may include butanol.

[0029] At least two immiscible reagents may also include one or more second reagents. One or more second reagents may include one or more surfactants. One or more surfactants may include one or more nonionic surfactants. One or more nonionic surfactants may include one or more Igepar, Triton, Brigi, Merge, NP80, NP95, Targitol, Decyl Glucoside, Lauryl Glucoside, Sucrose Laurate, Tween 85, Pluronic, or one or more combinations thereof. In one or more additional examples, one or more surfactants may include one or more anionic surfactants. One or more anionic surfactants may include one or more sodium bis(2-ethylhexyl)sulfosuccinate (AOT), sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), sodium dodecylbenzenesulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulfated castor oil, or one or more combinations thereof. In one or more further examples, one or more surfactants may include one or more cationic surfactants. One or more cationic surfactants may include one or more cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or a combination thereof. In yet another example, one or more surfactants may include one or more amphoteric surfactants. One or more amphoteric surfactants may include one or more cocamidopropyl betaine, dimethyllaurylamine N-oxide, myristylamine oxide, SB12, SB16, lecithin, or a combination thereof. In various examples, one or more surfactants may include fluorinated molecules. In one or more exemplary examples, one or more surfactants may include perfluoropolyethers. In yet another example, one or more surfactants may include glycols. For example, one or more surfactants may include polyethylene glycol. In one or more exemplary examples, one or more second reagents may include one or more quaternary ammonium salts. In various exemplary cases, one or more second reagents may include cetrimonium bromide.

[0030] A combination of water and one or more first reagents and one or more second reagents can produce an initial solution containing a microemulsion. In one or more examples, the amount of at least one first reagent in the initial solution may be about 10% to about 50% by weight, or about 20% to about 40% by weight. The amount of the second solvent may be about 5% to about 30% by weight, or about 10% to about 20% by weight. The remainder may consist of at least one additional first reagent or one or more second reagents. In one or more further examples, in embodiments in which the initial solution contains at least one surfactant and one or more solvents, the one or more solvents may include water, but the initial solution may contain about 10% to about 80% by weight, about 20% to about 60% by weight, or about 40% to about 80% by weight of the one or more solvents. The initial solution may also contain about 5% to about 40% by weight, about 10% to about 30% by weight, or about 5% to about 25% by weight of one or more surfactants. In various examples, the remainder of the initial solution may contain one or more additional reagents. In one or more further exemplary examples, the initial solution may contain about 50% by weight or less of water and about 20% by weight or less of one or more alcohols, with the remainder consisting of one or more reagents such as one or more surfactants.

[0031] Water and immiscible reagents can be combined at temperatures ranging from approximately 10°C to 60°C, 15°C to 50°C, 20°C to 40°C, 15°C to 25°C, 20°C to 30°C, 25°C to 35°C, or 30°C to 40°C. The initial solution can also be prepared at pressures ranging from approximately 80 kPa to 130 kPa, 90 kPa to 120 kPa, or 100 kPa to 110 kPa. In one or more examples, water and immiscible reagents can be mixed for approximately 15 seconds to 30 minutes, 1 minute to 20 minutes, 2 minutes to 10 minutes, 30 seconds to 5 minutes, 1 minute to 3 minutes, 2 minutes to 4 minutes, or 3 minutes to 5 minutes. In one or more examples, the amount of individual reagents in the initial solution may be determined based on the reagents used to produce the initial solution. For example, the amount of individual reagents in the initial solution may be determined based on the solubility limits of one or more of those reagents in the initial solution. In at least some exemplary cases, if the initial solution contains water, the amount of one or more reagents in the initial solution may be determined based on the solubility limits of one or more of those reagents in water.

[0032] In 108, process 100 may include adding one or more reagents to an initial solution to produce an aqueous solution containing one or more cosolvents. The one or more reagents added to the initial solution may include one or more acidic compounds. The one or more acidic compounds may include unsubstituted acids having 6 or fewer carbon atoms. In one or more further examples, the one or more acidic compounds may include substituted carboxylic acids having aliphatic chains having 6 or fewer carbon atoms. In one or more further examples, the one or more acidic compounds may include unsubstituted carbon chains having at least one alkenyl group. In yet another example, the one or more acidic compounds may include unsubstituted carbon chains having at least one alkenyl group. If the one or more acidic compounds include at least one acid having a substituted aliphatic carbon chain and / or at least one acid having a substituted carbon chain having at least one alkenyl group, these chains may be substituted at one or more positions with at least one of a methyl, ethyl, propyl, hydroxyl, or carboxyl group. In one or more exemplary examples, the one or more reagents added to the initial solution may include one or more carboxylic acids. In one or more exemplary examples, the one or more reagents added to the initial solution may include one or more dicarboxylic acids. In one or more exemplary examples, one or more reagents added to the initial solution may include succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, citric acid, formic acid, or one or more combinations thereof.

[0033] In one or more examples, one or more reagents may be added to the initial solution at temperatures of approximately 10°C to 60°C, approximately 15°C to 50°C, approximately 20°C to 40°C, approximately 15°C to 25°C, approximately 20°C to 30°C, approximately 25°C to 35°C, or approximately 30°C to 40°C, in 108. Furthermore, one or more reagents may be added to the initial solution at pressures of approximately 80 kPa to 130 kPa, approximately 90 kPa to 120 kPa, or approximately 100 kPa to 110 kPa. Furthermore, one or more reagents may be mixed for periods of time ranging from approximately 15 seconds to 30 minutes, 1 minute to 20 minutes, 2 minutes to 10 minutes, 30 seconds to 5 minutes, 1 minute to 4 minutes, 2 minutes to 6 minutes, 3 minutes to 8 minutes, or 4 minutes to 10 minutes.

[0034] Process 100 may include, in 110, producing a lithium-containing aqueous solution. In one or more examples, in 110, one or more lithium-containing compounds may be added to the aqueous solution produced in 108 to produce a lithium-containing aqueous solution. In various examples, one or more lithium-containing compounds may include one or more lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or a combination thereof.

[0035] In at least some examples, one or more lithium-containing compounds can be added to an aqueous solution at 110 at temperatures ranging from about 10°C to about 60°C, about 15°C to about 50°C, about 20°C to about 40°C, about 15°C to about 25°C, about 20°C to about 30°C, about 25°C to about 35°C, or about 30°C to about 40°C. Furthermore, one or more lithium-containing compounds can be added to an aqueous solution at 110 at pressures ranging from about 80 kPa to about 130 kPa, about 90 kPa to about 120 kPa, or about 100 kPa to about 110 kPa. Furthermore, one or more lithium-containing compounds and aqueous solutions may be mixed in 110 for a period of time of about 3 to about 45 minutes, about 5 to about 30 minutes, about 10 to about 20 minutes, about 5 to about 10 minutes, about 10 to about 15 minutes, about 15 to about 20 minutes, about 20 to about 25 minutes, or about 25 to about 30 minutes.

[0036] Furthermore, in 112, process 100 may include precipitating a lithium-containing aqueous solution to produce a precipitate containing lithium-containing particles. The precipitation process may form a supernatant containing a precipitate with lithium-containing particles and a residue. In one or more exemplary examples, the lithium-containing particles may include lithium-containing salts. Precipitation of the lithium-containing aqueous solution may include carrying out at least one of one or more mechanical processes or one or more chemical processes. In one or more exemplary examples, in the case of a non-microemulsion process, precipitation of the lithium-containing aqueous solution may occur when the lithium-containing reagent of 110 is added to the aqueous solution and the lithium-containing reagent dissolves in the aqueous solution. Once the lithium-containing reagent dissolves in the aqueous solution, a reaction may proceed to produce a lithium-containing compound. In at least some examples, as the reaction to produce the lithium-containing compound proceeds, the lithium-containing compound may crystallize to produce lithium-containing particles. In one or more examples, one or more alcohols present in the aqueous solution may promote the crystallization of the lithium-containing compound to form lithium-containing particles. The lithium-containing reagent may dissolve in the aqueous solution by sufficient mixing at a relatively low temperature, for example, below 30°C. Furthermore, lithium-containing reagents can dissolve in aqueous solutions even with minimal mixing at relatively high temperatures, such as 30°C or higher.

[0037] When a microemulsion process is being carried out, precipitation of the lithium-containing solution may occur in response to the addition of one or more additional reagents to the lithium-containing aqueous solution. In one or more examples, the aqueous solution produced in 108 may contain at least two phases. In at least some examples, at least two phases may include an aqueous phase and a second phase containing droplets dispersed in the first phase. In various examples, the second phase may contain droplets surrounded by a barrier. In one or more exemplary examples, the barrier may consist of surfactant molecules. By adding a lithium-containing reagent to the aqueous solution in 110, a lithium-containing compound may be formed within the droplets of the second phase. By breaking the barrier of the second phase, the lithium-containing compound formed within the second phase can precipitate from the droplet. The barrier of the second phase can be broken by one or more physical processes or at least one of one or more chemical processes. In various cases, the droplet barrier can be broken using one or more mixing devices. Furthermore, the droplet barrier can also be broken by heating the lithium-containing aqueous solution. In addition, the droplet barrier can also be broken by disrupting the equilibrium of the microemulsion by adding one or more additional reagents to the lithium-containing aqueous solution. For example, lithium-containing compounds can be released from droplets by adding a sufficient amount of acetone to a lithium-containing aqueous solution. In at least some examples, at least some of the additional reagents added to disrupt the equilibrium of the microemulsion can be reused. For example, some of the additional reagents recovered from the barrier breaking process can be reused in other suitable processes of process 100. In various examples, lithium-containing particles can be formed within the droplet, while in other examples, lithium-containing particles can be formed when lithium-containing compounds formed within the droplet are released.

[0038] Furthermore, in 114, process 100 may include performing one or more separation processes. One or more separation processes may separate lithium-containing particles from the residual liquid. One or more separation processes may include centrifugation. In one or more further examples, one or more separation processes may include one or more filtration processes. In at least some examples, one or more separation processes may include one or more vacuum filtration processes.

[0039] In 116, process 100 may include carrying out a drying process for lithium-containing particles. The drying process may be carried out at a temperature of at least 50°C, at least 75°C, at least 100°C, at least 125°C, at least 150°C, at least 175°C, at least 200°C, at least 225°C, at least 250°C, at least 275°C, or at least 300°C. In one or more exemplary examples, the drying process may be carried out in a temperature range of about 50°C to about 500°C, about 75°C to about 300°C, about 100°C to about 250°C, about 50°C to about 250°C, about 100°C to about 300°C, about 300°C to about 500°C, about 100°C to about 200°C, about 150°C to about 250°C, about 200°C to about 300°C, or about 250°C to about 350°C. Furthermore, the drying process may be carried out for a period of at least 15 minutes, at least 30 minutes, at least 1 hour, at least 2 hours, at least 3 hours, at least 4 hours, or at least 5 hours. In one or more exemplary cases, the drying process may be carried out for a period of about 15 minutes to about 12 hours, about 30 minutes to about 6 hours, about 30 minutes to about 2 hours, about 1 hour to about 3 hours, about 2 hours to about 4 hours, about 3 hours to about 5 hours, or about 4 hours to about 6 hours.

[0040] In embodiments in which lithium-containing particles are produced using a microemulsion, process 100 may include performing one or more washes between one or more separation processes performed in 114 and a drying process performed in 116. In one or more examples, one or more washes may be performed using one or more reagents that constitute the initial solution. For example, one or more washes may be performed using one or more alcohols present in the initial solution. In one or more exemplary examples, one or more washes may be performed using butanol. In at least some examples, some of the reagents used in one or more washes may be recovered and reused in subsequent washes. For example, one or more alcohol washes in 118 may include a first butanol wash, a second butanol wash, and a third butanol wash. In these cases, butanol recovered in the first butanol wash may be used in the second butanol wash, and butanol recovered in the first or second butanol wash may be used in the third butanol wash.

[0041] Lithium-containing particles can have various shapes. For example, lithium-containing particles may be spherical, pellet-shaped, or rod-shaped. In one or more examples, the coefficient of variation of the aspect ratio of lithium-containing particles may be 1%, 5%, 10%, 15%, 20%, 25%, or 30% or less. The coefficient of variation may correspond to the ratio of the standard deviation of the size distribution of lithium-containing particles to the mean value of the size distribution of lithium-containing particles.

[0042] If the lithium-containing particles are spherical, the spheres may have aspect ratios of approximately 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more exemplary cases, the spheres may have aspect ratios of approximately 0.9 to approximately 1.25, approximately 0.95 to approximately 1.15, or approximately 1 to approximately 1.1. If the lithium-containing particles are pelletized, the pellets may have aspect ratios of approximately 0.9, approximately 0.95, approximately 1, approximately 1.05, approximately 1.1, approximately 1.15, approximately 1.2, approximately 1.25, approximately 1.3, approximately 1.35, or approximately 1.4. In one or more further exemplary cases, the pellets may have aspect ratios of approximately 0.9 to approximately 1.4, approximately 1 to approximately 1.3, approximately 1.1 to approximately 1.2, approximately 1 to approximately 1.2, or approximately 0.9 to approximately 1.2. In yet another example, if the lithium-containing particles are rod-shaped, the rods may have aspect ratios of at least 2.5, at least 2.6, at least 2.7, at least 2.8, at least 2.9, at least 3, at least 3.1, at least 3.2, at least 3.3, at least 3.4, at least 3.5, at least 3.6, at least 3.7, at least 3.8, at least 3.9, or at least 4.

[0043] In one or more examples, lithium-containing particles may have one or more dimensions of 5 micrometers (μm) or less, 2 μm or less, 1 μm or less, 0.8 μm or less, 0.6 μm or less, 0.4 μm or less, 0.2 μm or less, 0.1 μm or less, or 0.05 μm or less. In one or more exemplary examples, battery material particles may have dimensions of approximately 0.05 μm to approximately 5 μm, approximately 0.1 μm to approximately 1 μm, approximately 0.3 μm to approximately 3 μm, approximately 0.5 μm to approximately 2 μm, or approximately 0.05 μm to approximately 0.8 μm. In one or more exemplary examples, lithium-containing particles may be rod-shaped with a diameter of approximately 0.1 μm to approximately 0.8 μm and a length of approximately 1 μm to approximately 5 μm.

[0044] In various examples, the yield of process 100 may be at least 80%, at least 85%, at least 90%, at least 95%, or at least 99%. In one or more exemplary examples, the yield may be approximately 80% to approximately 99.9%, approximately 85% to approximately 99.5%, approximately 90% to approximately 99%, approximately 90% to approximately 99.9%, or approximately 95% to approximately 99.9%. The yield may be calculated based on the weight of lithium-containing particles produced relative to the amount of lithium-containing reagent used in process 100 in 110.

[0045] In at least some examples of non-microemulsion processes, a conductive additive may be added to the initial solution. The conductive additive may include carbon-containing materials. In one or more exemplary examples, the carbon-based additive may include carbon black or carbon nanotubes. In embodiments where the conductive additive is part of a non-microemulsion process, at least one of the reaction conditions in operations 102, 108, 110, or 112 may be increased. In one or more examples, when a conductive additive is used in a non-microemulsion process, the product produced in process 100 may include lithium-containing particles arranged on a matrix of conductive additives.

[0046] In various cases, lithium-containing compound particles can be used in the manufacture of lithium-ion batteries. For example, lithium-containing compound particles can be included in the anode of a lithium-ion battery. In one or more cases, lithium-containing compound particles can be included in the active material of the anode of a lithium-ion battery.

[0047] Although process 100 is described in relation to the production of lithium-containing particles, process 100 can also be carried out to produce particles with different compositions. For example, process 100 can be carried out to produce nickel hydroxide particles. Specifically, instead of producing a lithium-containing solution in operation 110, a nickel-containing compound can be added to an aqueous solution to produce a nickel-containing solution. In one or more examples, the nickel-containing compound may include a nickel(II) salt. Nickel hydroxide particles can then be precipitated from the nickel-containing solution. In at least some examples, potassium hydroxide can be used to form nickel hydroxide.

[0048] Figure 2 shows a framework 200 for producing battery material particles using a microemulsion according to one or more embodiments. In at least some embodiments, the framework 200 can perform one or more operations performed with respect to the microemulsion embodiment of process 100 described in relation to Figure 1. Furthermore, at least some operations performed in relation to the framework 200 can correspond to one or more operations performed with respect to the microemulsion embodiment of process 100 described in relation to Figure 1. Furthermore, in some cases, the battery material particles produced in relation to the framework 200 can correspond to lithium-containing compound particles produced by one or more microemulsion embodiments of process 100 described in relation to Figure 1.

[0049] The framework may include a reaction vessel 202. The reaction vessel 202 may have a capacity of at least 0.1 liters (L), 0.5 L, 1 L, 2 L, 5 L, 10 L, 25 L, 50 L, 75 L, 100 L, 250 L, or 500 L. In one or more examples, the reaction vessel 202 may include one or more mixing devices 204. One or more mixing devices 204 may include one or more agitation mixers. For example, one or more mixing devices 204 may include one or more rotating paddles. In one or more further examples, one or more mixing devices 204 may include one or more jet mixers. In one or more further examples, one or more mixing devices 204 may include one or more supersonic mixers.

[0050] The first solution 206 can be added to the reaction vessel 202. The first solution 206 may contain one or more first solvents. In one or more examples, one or more first solvents may include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more grimes, one or more ethers, or one or more combinations thereof. The second solution 208 may also be added to the reaction vessel 202. In various examples, the second solution 208 may contain one or more second solvents. In one or more examples, one or more solvents in the second solution 208 may be selected so that the second solution 208 and the first solution 206 are not miscible with each other.

[0051] At least one of the one or more solutions 206, 208 may contain one or more reagents. In various examples, one or more reagents may be dissolved in one or more solutions 206, 208. In embodiments in which at least one of the first solution 206 or the second solution 208 contains multiple solvents, the amount of the first solvent is about 10% to about 50% by weight or about 20% to about 40% by weight, the amount of the second solvent is about 5% to about 30% by weight or about 10% to about 20% by weight, and the remainder may contain one or more reagents in at least one of the first or second solutions. In one or more additional examples, in embodiments in which the first solution 206 and the second solution 208 are mixed with one or more surfactants 210 to form a mixture, the mixture may contain one or more solvents in amounts from about 10% to about 80% by weight, from about 20% to about 60% by weight, or from about 40% to about 80% by weight, one or more surfactants 210 in amounts from about 5% to about 40% by weight, from about 10% to about 30% by weight, or from about 5% to about 25% by weight, with the remainder being one or more reagents. In one or more additional examples, the mixture containing the first solution 206 and the second solution 208 may contain water in amounts of about 50% by weight or less, one or more alcohols in amounts of about 20% by weight or less, with the remainder being one or more reagents. In one or more examples, the amount of individual reagents contained in at least one of the first solution 206 or the second solution 208 may be determined based on the composition of the first solution 206 and / or the composition of the second solution 208. For example, the amount of individual reagents contained in at least one of the first solution 206 or the second solution 208 can be determined based on the solubility limits of one or more individual reagents in at least one of the first solution 206 or the second solution 208. In at least some examples, if at least one of the first solution 206 or the second solution 208 contains water, the amount of one or more reagents can be determined based on the solubility limits of one or more reagents in water.

[0052] The first phase 212 and the second phase 214 can be produced by mixing the first solution 206, the second solution 208, and optionally one or more surfactants 210. In one or more examples, the first phase 212 may include the first solution 206 and optionally one or more additional liquids, such as one or more surfactants 210. Furthermore, the second phase 214 may include droplets containing at least the second phase 214. In various examples, the second phase 214 may include droplets of the second solution 208 enclosed in a barrier. In one or more further examples, the barrier may consist of surfactant molecules.

[0053] In one or more cases, the first phase 212 and the second phase 214 may include a microemulsion. Specifically, the first solution 206, the second solution 208, and optionally one or more surfactants 210 can be mixed in a reaction vessel 202 under temperature and pressure conditions for forming a microemulsion to form a microemulsion containing the first phase 212 and the second phase 214. In one or more examples, the first solution 206, the second solution 208, and optionally one or more surfactants 210 can be mixed at temperatures ranging from about 10°C to about 100°C, about 20°C to about 90°C, about 30°C to about 80°C, about 20°C to about 50°C, or about 25°C to about 75°C to produce a microemulsion in the reaction vessel 202. Furthermore, the first solution 206, the second solution 208, and optionally one or more surfactants 210 can be mixed at a pressure of about 90 kilopascals (kPa) to about 120 kPa, or about 95 kPa to about 105 kPa, to produce a microemulsion in the reaction vessel 202. If supercritical CO2 is the solvent contained in at least one of the first solution 206 or the second solution 208, a microemulsion can be formed at a temperature and pressure in which CO2 behaves as a supercritical fluid. Specifically, if supercritical CO2 is the solvent contained in at least one of the first solution 206 or the second solution 208, a microemulsion can be formed at a temperature of about 30°C or higher and a pressure of about 7 megapascals (MPa) or higher.

[0054] In one or more examples, one or more reagents may contain one or more lithium-containing components. For example, one or more reagents may contain lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof. Furthermore, one or more reagents may contain one or more transition metal halides. Specifically, one or more reagents may contain at least one of FeCl3 or NiCl2. Furthermore, one or more reagents may contain one or more transition metal sulfates. In one or more examples, one or more reagents may contain at least one of FeSO4 or NiSO4. In one or more additional examples, one or more reagents may contain one or more basic compounds. In one or more additional examples, one or more reagents may contain sodium hydroxide, ammonium hydroxide, lithium hydroxide, or one or more combinations thereof. One or more reagents may also contain one or more organic acids. In one or more additional examples, one or more reagents may contain succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, or one or more combinations thereof.

[0055] One or more surfactants may include one or more nonionic surfactants. One or more nonionic surfactants may include Igepearl, Triton, Brigi, Merge, NP80, NP95, Tergitol, Decyl Glucoside, Lauryl Glucoside, Sucrose Laurate, Tween 85, Pluronic, or one or more combinations thereof. In one or more additional examples, one or more surfactants may include one or more anionic surfactants. One or more anionic surfactants may include sodium bis(2-ethylhexyl) sulfosuccinate (AOT), sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), sodium dodecylbenzenesulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulfated castor oil, or one or more combinations thereof. In one or more additional examples, one or more surfactants may include one or more cationic surfactants. One or more cationic surfactants may include cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or one or more combinations thereof. In other examples, one or more surfactants may include one or more amphoteric surfactants. One or more amphoteric surfactants may include cocamidopropyl betaine, dimethyllaurylamine N-oxide, myristamine oxide, SB12, SB16, lecithin, or one or more combinations thereof. In various examples, one or more surfactants may include fluorinated molecules. In one or more examples, one or more surfactants may include perfluoropolyethers. In one or more additional examples, one or more surfactants may include glycols. Specifically, one or more surfactants may include polyethylene glycol.

[0056] In at least some examples, one or more surfactants 210 may include one or more auxiliary surfactants. In one or more examples, one or more surfactants 210 may include a first surfactant and an auxiliary surfactant. In various examples, the first surfactant may include at least one of the following: a nonionic surfactant, an anionic surfactant, a cationic surfactant, an amphoteric surfactant, a surfactant containing a fluorinated molecule, or a glycol. Furthermore, one or more auxiliary surfactants may include one or more alcohols. For example, one or more auxiliary surfactants may include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, sorbitol, or one or more combinations thereof. In various examples, one or more auxiliary surfactants may include at least one of benzalkonium chloride (BZK) or stearin.

[0057] In various examples, a first solution 206 and a second solution 208, along with one or more surfactants 210 as needed, are mixed in a reaction vessel 202 under reaction conditions 216, and one or more reagents participate in one or more reactions to produce battery material particles 218. In one or more examples, reaction conditions 216 can include effective temperatures, pressures, and amounts of reagents for producing battery material particles 218. In one or more examples, the reagents contained in the first solution 206 and the second solution 208 are mixed under reaction conditions 216 to cause precipitation of battery material particles 218. In one or more examples, one or more reagents contained in the first phase 212 can move to the second phase 214 and react with one or more additional reagents contained in the second phase to produce battery material particles 218. In one or more further examples, reaction conditions 216 can include temperatures from 10°C to about 100°C and pressures from about 90kPa to about 120kPa.

[0058] The battery material particles 218 may contain one or more cathode active material precursors. For example, the battery material particles 218 may contain FePO4, NiPO4, CoPO4, Fe x Mn y PO4, CoX, NiX, MnX, Nix Mn y Co z X, Next x Co y A z X, Next w Co x Mn y A z X can contain w+x+y+z=1. In one or more examples, X can contain a divalent anionic radical. In one or more examples, the divalent anionic radical can contain CO3 or C2O4. In one or more additional examples, X can contain two monovalent anions. Specifically, the two monovalent anions can contain (OH)2 or OH2-vF. Furthermore, A can contain one or more cationic dopants. In one or more additional examples, the one or more cationic dopants can contain Al, Mg, Ti, Zr, Cr, Ru, Mo, V, or one or more combinations thereof.

[0059] The battery material particles 218 may also contain one or more lithium-containing materials. For example, the battery material particles 218 may include lithium succinate, lithium oxalate, lithium ketomalonate, lithium citrate, lithium oxide, lithium peroxide, lithium acetate, lithium formate, lithium hydroxide, lithium carbonate, lithium sulfate, lithium phosphate, lithium fluoride, lithium peroxide, lithium amine hydroxide, lithium oxalate, lithium succinate, lithium dimethylsuccinate, lithium fumarate, lithium 2-methylfumarate, dilithium maleate, dilithium 2-methylmaleate, 1,4-hydroquinone dilithium, catechol dilithium, lithium poly(hydroquinone), lithium (1S,2S)-cyclopentane-1,2-dicarboxylate, lithium (1S,2S)-cyclohexane-1,2-dicarboxylate, lithium malonate, hydrazine 1,2-bis(trimethylsilyl)dilinium, pyromellidiimide lithium, naphthalenediimide lithium, lithium cyanurate, or one or more of these.

[0060] Furthermore, the battery material particles 218 may contain one or more cathode active materials. The one or more cathode active materials may contain one or more transition metal fluorides. In various examples, the one or more transition metal fluorides may be FeF3, CuF2, CoF3, NiF2, MnF2, or LiFePO4, LiMn x Fe y PO4, LiNi x Mn y Co z O2, LiLiLi x Co y A z O2, LiLiLi w Co x Mn y A z O2, where w+x+y+z=1, can be included. In various examples, A can contain one or more cationic dopants. In one or more examples, one or more cationic dopants can contain at least one of Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.

[0061] Furthermore, the battery material particles 218 may contain one or more anode active materials. In one or more examples, one or more anode active materials may be Li4Ti5O 12 It may contain at least one of LiNb3O8 or a hydroxyamine hydrochloride.

[0062] In yet another example, the battery material particle 218 may contain one or more anode active material precursors. In one or more examples, one or more anode active material precursors may be TiO2 or NbO x It can include at least one of the following.

[0063] The battery material particles 218 can have a variety of properties. For example, the coefficient of variation in the aspect ratio of the battery material particles 218 may be 1% or less, 5% or less, 10% or less, 15% or less, 20% or less, 25% or less, or 30% or less. The coefficient of variation may correspond to the ratio of the standard deviation of the size distribution of the battery material particles to the mean value of the size distribution of the battery material particles.

[0064] Furthermore, the battery material particles 218 may include nanospheres. The nanospheres may have aspect ratios of about 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more exemplary examples, the nanospheres may have aspect ratios of about 0.9 to about 1.25, about 0.95 to about 1.15, or about 1 to 1.1. In one or more further examples, the battery material particles 218 may include nanopellets. The nanopellets may have aspect ratios of about 0.9, about 0.95, about 1, about 1.05, about 1.1, about 1.15, about 1.2, about 1.25, about 1.3, about 1.35, or about 1.4. In further exemplary examples, the nanopellets may have aspect ratios of about 0.9 to about 1.4, about 1 to about 1.3, about 1.1 to about 1.2, about 1 to about 1.2, or about 0.9 to about 1.2. Furthermore, the battery material particles 218 may include nanorods. The nanorods may have aspect ratios of at least 2.5, at least 2.6, at least 2.7, at least 2.8, at least 2.9, at least 3, at least 3.1, at least 3.2, at least 3.3, at least 3.4, at least 3.5, at least 3.6, at least 3.7, at least 3.8, at least 3.9, or at least 4.

[0065] In one or more examples, the battery material particles 218 may have one or more dimensions of 5 micrometers (μm) or less, 2 μm or less, 1 μm or less, 0.8 μm or less, 0.6 μm or less, 0.4 μm or less, 0.2 μm or less, 0.1 μm or less, or 0.05 μm or less. In one or more exemplary examples, the battery material particles may have dimensions of about 0.05 μm to about 5 μm, about 0.1 μm to about 1 μm, about 0.3 μm to about 3 μm, about 0.5 μm to about 2 μm, or about 0.05 μm to about 0.8 μm.

[0066] In at least some examples, the battery material particles 218 are 9 × 10 -2 Siemens / centimeter (S / cm) or less, 8 x 10 -2 S / cm, 7×10 -2 S / cm, 6×10 -2 S / cm, 5× -2 S / cm, 4×10-2 S / cm, 3×10 -2 S / cm, 2×10 -2 S / cm, 1×10 -2 S / cm, 0.8 × 10 -2 S / cm, 0.5×10 -2 S / cm, or 0.2 × 10 -2 It may have an electrical conductivity of S / cm.

[0067] In further examples, ligands may bind to the battery material particles 218. In one or more examples, ligands may minimize aggregation between the battery material particles 218. For example, ligands may stabilize the surface of the battery material particles 218. In even more examples, ligands may control the morphology of the battery material particles 218. For example, water-soluble ligands may be used to control the morphology of the battery material particles 218.

[0068] In one or more examples, the ligand may include a polymeric ligand. In one or more exemplary examples, the polymeric ligand may include at least one of polyacrylic acid (PAA) or polyvinylpyrrolidone (PVP). In further examples, the ligand may include a monomer unit containing one or more carboxylic acids. In further exemplary examples, one or more carboxylic acids may include hexanoic acid or oleic acid. In yet another example, the ligand may include a monomer unit containing one or more alkanethiols. In yet another exemplary example, one or more alkanethiols may include hexanethiol or octanthiol. In yet another example, the ligand may include a monomer unit containing one or more mercaptoalkanoic acids. For example, the ligand may include mercaptohexadecanoic acid. The ligand may also include a monomer unit containing one or more phosphines. For example, the ligand may include trioctylphosphine oxide or phosphinic acid. In various examples, the ligand may include a monomer unit containing one or more amines. In at least some examples, one or more amines may include amine-terminated polyethylene glycol.

[0069] After the battery material particles 218 are formed in the second phase 214, the battery material particles 218 can be separated from the second phase 214 in operation 120. In one or more examples, the battery material particles 218 can be removed from the second phase 214 by breaking the droplet barrier of the second phase 214 in the microemulsion. In at least some examples, the breakdown of the droplet barrier of the second phase 214 may be temporary. In various examples, the droplet barrier of the second phase 214 can be broken by heating the mixture of the first phase 212 and the second phase 214. In further additional examples, the battery material particles 218 can be removed from the droplets of the second phase 214 by adding an additional solvent to disrupt the equilibrium of the microemulsion and precipitate the battery material particles 218 from the droplets of the second phase 214.

[0070] After removing the battery material particles 218 from the second phase 214, one or more liquid / solid separation processes 222 may be performed to generate the battery material particles 218 and residual liquid phase 224. In one or more exemplary cases, the battery material particles 218 may be removed from the droplets of the second phase 214 using one or more centrifugation processes. In further exemplary cases, the battery material particles 218 may be removed from the droplets of the second phase 214 using a filtration process. In yet another exemplary case, the battery material particles 218 may be removed from the droplets of the second phase 214 by decantation after the battery material particles 218 have settled in the reaction vessel 202. In yet another exemplary case, the battery material particles 218 may settle in the reaction vessel 202, and the residual liquid phase 224 may be decanted without destroying the droplets of the second phase 214. In these cases, separation of the battery material particles in 220 may not be performed.

[0071] In various examples, the residual liquid phase 224 may be stored in an additional container 126. In at least some examples, the residual liquid phase 224 may be separated into components comprising at least one of the first solution 206, the second solution 208, and / or one or more surfactants 210, and added to the reaction vessel 202 to carry out one or more additional cycles of the process for forming additional battery material particles. In this way, the residual liquid phase 224 may be recycled in one or more subsequent cycles of the process for forming additional battery material particles.

[0072] The battery material particles 218 can be formed as a first layer 228 on the second layer 230 of the battery 232 using one or more battery formation processes 134. In one or more examples, the battery material particles 218 can be heated to a temperature of about 900°C to 1000°C before being formed as the first layer 228 to produce aggregated battery material particles. In one or more exemplary examples, the aggregated battery material particles have dimensions of about 1 μm to about 50 μm. In further examples, the battery material particles 218 can be used to form one or more cathode layers of the battery 232. In yet another example, the battery material particles 218 can be used to form one or more anode layers of the battery 232. In at least some examples, the battery material particles 218 can be deposited on the second layer 230 using one or more liquid phase deposition techniques. In further exemplary examples, the battery material particles 218 can be deposited on the second layer 230 using one or more vapor phase deposition techniques. In various examples, the second layer 230 may include a current collector layer. In one or more cases, the battery 232 may include a lithium-ion battery.

[0073] In further examples, the first solution 206 may contain a first microemulsion, and the second solution 208 may contain a second microemulsion. In this way, the first microemulsion and the second microemulsion may be mixed in a reaction vessel to produce a mixture of microemulsions. In various examples, the mixture of microemulsions may contain a first number of droplets corresponding to the first microemulsion and a second number of droplets corresponding to the second microemulsion. In one or more exemplary examples, the first number of droplets and the second number of droplets are combined, and a reaction may occur between one or more first reagents contained in the first number of droplets and one or more second reagents contained in the second number of droplets to produce battery material particles 218. [Examples]

[0074] In consideration of the embodiments of the subject matter described above, the present application discloses the following list of embodiments. Herein, a single feature of a single embodiment, or a combination of one or more features of multiple embodiments, and further combinations with one or more features of other embodiments as necessary, constitutes a further embodiment included in the disclosure.

[0075] Example 1 is a process comprising: supplying a first solution and a second solution into a reaction vessel, wherein the first solution contains one or more first solvents, the second solution contains one or more second solvents, the one or more first solvents are immiscible with the one or more second solvents, and at least one of the first solution or the second solution contains one or more reagents; combining the first solution and the second solution to produce a microemulsion comprising a first phase containing one or more first solvents and a second phase consisting of a plurality of droplets containing one or more second solvents; reacting with one or more reagents to produce battery material particles in the plurality of droplets, wherein at least one of the battery material particles has a dimension of 1 micrometer (μm) or less; and removing the battery material particles from the plurality of droplets.

[0076] Example 2 is the subject of Example 1, in which the battery material particles are removed from multiple droplets by heating the multiple droplets.

[0077] Example 3 is the subject of Example 1 or 2, wherein the battery material particles are removed by adding an additional solvent to disrupt the equilibrium of the microemulsion and causing the battery material particles to precipitate from multiple droplets.

[0078] Example 4 is the subject matter described in any one of Examples 1 to 3, and includes destroying the surfaces of multiple droplets to remove battery material particles from the multiple droplets.

[0079] Example 5 is a subject of Example 4, in which the surfaces of multiple droplets are temporarily destroyed and battery material particles are removed from the multiple droplets.

[0080] Example 6 is the subject matter described in any one of Examples 1 to 3, wherein the battery material particles are removed from multiple droplets without damaging the surface of the multiple droplets.

[0081] Example 7 is the subject matter described in any one of Examples 1 to 6, and comprises performing one or more separation processes to separate battery material particles from the residual liquid phase, wherein the residual liquid phase comprises one or more first solvents and one or more second solvents.

[0082] Example 8 is the subject of Example 7, wherein the residual liquid phase is generated during a first cycle of the battery material particle generation process, and the process includes reusing the residual liquid phase in a second cycle of the battery material particle generation process.

[0083] Example 9 is the subject of Example 7 or 8 and includes performing one or more centrifugal separation processes to separate battery material particles from the residual liquid phase.

[0084] Example 10 is the subject matter described in any one of Examples 7 to 9, and includes performing one or more filtration processes to separate the battery material particles and the residual liquid phase.

[0085] Example 11 is the subject of Example 7 and includes allowing battery material particles to settle in a reaction vessel and separating the battery material particles from the residual liquid phase by performing one or more decantation processes.

[0086] Example 12 is the subject matter described in any one of Examples 1 to 11, and includes heating battery material particles at a temperature of about 900°C to 1000°C to produce aggregated battery material particles.

[0087] Example 13 is the subject of Example 12, and the aggregated battery material particles have dimensions ranging from about 1 μm to about 50 μm.

[0088] Example 14 is the subject matter described in any one of Examples 1 to 13, wherein at least one of one of the first solvents or one or more second solvents includes water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more grimes, one or more ethers, or one or more combinations thereof.

[0089] Example 15 is a subject described in any one of Examples 1 to 14, wherein one or more reagents contain one or more lithium-containing components.

[0090] Example 16 is the subject of Example 15, wherein one or more lithium-containing components include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or a combination of one or more of these.

[0091] Example 17 is a subject matter described in any one of Examples 1 to 14, wherein one or more reagents contain one or more transition metal halides.

[0092] Example 18 is the subject of Example 17, wherein one or more transition metal halides include at least one of FeCl3 or NiCl2.

[0093] Example 19 is a subject described in any one of Examples 1 to 14, wherein one or more reagents contain one or more transition metal sulfates.

[0094] Example 20 is the subject of Example 19, wherein one or more transition metal sulfates include at least one of FeSO4 or NiSO4.

[0095] Example 21 is a subject described in any one of Examples 1 to 20, wherein one or more reagents include one or more basic compounds.

[0096] Example 22 is the subject of Example 21, wherein one or more basic compounds include at least one of sodium hydroxide, ammonium hydroxide, or lithium hydroxide.

[0097] Example 23 is a subject described in any one of Examples 1 to 20, wherein one or more reagents contain one or more acidic compounds.

[0098] Example 24 is the subject of Example 23, wherein one or more acidic compounds include succinic acid, malonic acid, oxalic acid, glutaric acid, or adipic acid.

[0099] Example 25 is the subject matter described in any one of Examples 1 to 24, wherein the battery material particles include one or more cathode active material precursors.

[0100] Example 26 is the subject of Example 25, and the cathode active material precursor is one or more types of FePO4, NiPO4, CoPO4, Fe x Mn y PO4, CoX, NiX, MnX, Ni x Mn y Co z X, Next x Co y A z X, Next w Co x Mn y A zX, where w+x+y+z=1, where X represents a divalent anionic radical or a combination of two monovalent anions, and A represents a cationic dopant, comprising at least one of these.

[0101] Example 27 is the subject of Example 26, and the divalent anionic radical includes CO3 or C2O4.

[0102] Example 28 is the subject of Example 26, and the combination of two monovalent anions includes (OH)2 or OH2-vFv.

[0103] Example 29 is the subject of Example 26, and the cationic dopant comprises Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.

[0104] Example 30 is the subject matter described in any one of Examples 1 to 24, wherein the battery material particles contain one or more lithium-containing materials.

[0105] Example 31 is the subject of Example 30, and contains one or more lithium-containing substances: lithium succinate, lithium oxalate, lithium ketomalonate, lithium citrate, lithium oxide, lithium peroxide, lithium acetate, lithium formate, lithium hydroxide, lithium carbonate, lithium sulfate, lithium phosphate, lithium fluoride, lithium peroxide, lithium hydroxylamine lithium, lithium oxalate, lithium succinate, lithium dimethylsuccinate, lithium fumarate, lithium 2-methylfumarate, dilithium maleate-containing substance, 2 - Containing at least one of the following: dilithium methylmaleate, dilithium 1,4-hydroquinone, dilithium catechol, lithium poly(hydroquinone), lithium (1S,2S)-cyclopentane-1,2-dicarboxylate, lithium (1S,2S)-cyclohexane-1,2-dicarboxylate, lithium malonate, hydrazine 1,2-bis(trimethylsilyl)dililium, lithium pyromellidiimide, lithium naphthalenediimide, or lithium cyanurate.

[0106] Example 32 is the subject matter described in any one of Examples 1 to 24, wherein the battery material particles include one or more cathode active materials.

[0107] Example 33 is the subject of Example 32, wherein one or more cathode active materials include one or more transition metal fluorides.

[0108] Example 34 is the subject of Example 33, and the one or more transition metal fluorides are FeF3, CuF2, CoF3, NiF2, MnF2, LiFePO4, LiMn x Fe y PO4, LiNi x Mn y Co z O2, LiLiLi x Co y A z O2, LiLiLi w Co x Mn y A z It contains at least one of the following: O2, where w+x+y+z=1, and A represents a cationic dopant.

[0109] Example 35 is the subject of Example 34, wherein the cationic dopant comprises Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.

[0110] Example 36 is the subject matter described in any one of Examples 1 to 24, wherein the battery material particles include one or more anode active materials.

[0111] Example 37 is the subject of Example 36, wherein one or more anode active materials are Li4Ti5O 12 It comprises at least one of LiNb3O8 or hydroxylamine hydrochloride.

[0112] Example 38 is the subject matter described in any one of Examples 1 to 24, wherein the battery material particles include one or more anode active material precursors.

[0113] Example 39 is the subject of Example 38, wherein one or more anode active material precursors are TiO2 or NbO2.x It includes at least one of the following.

[0114] Example 40 is the subject matter described in any one of Examples 1 to 39, wherein the coefficient of variation of the aspect ratio of the battery material particles is approximately 25% or less.

[0115] Example 41 is the subject matter described in any one of Examples 1 to 40, wherein the battery material particles form nanospheres.

[0116] Example 42 is the subject of Example 41, wherein the nanospheres have an aspect ratio of about 1 to about 1.1.

[0117] Example 43 is the subject matter described in any one of Examples 1 to 40, wherein the battery material particles form nanopellets.

[0118] Example 44 is the subject of Example 43, and the nanopellets have an aspect ratio of about 1.1 to about 3.

[0119] Example 45 is the subject matter described in any one of Examples 1 to 40, wherein the battery material particles form nanorods.

[0120] Example 46 is the subject of Example 45, wherein the nanorod has an aspect ratio of at least about 3.

[0121] Example 47 is the subject matter described in any one of Examples 1 to 46, wherein the battery material particles are approximately 1 × 10⁶ -2 It has an electrical conductivity of less than Siemens / centimeter.

[0122] Example 48 is the subject matter described in any one of Examples 1 to 47, wherein the ligand is bound to one or more surfaces of individual battery material particles.

[0123] Example 49 is the subject of Example 48, and the ligand comprises one or more polymer materials.

[0124] Example 50 is the subject of Example 49, wherein one or more polymer materials include at least one of polyacrylic acid or polyvinylpyrrolidone.

[0125] Example 51 is the subject of Example 49, wherein one or more polymer materials contain monomer units having one or more carboxylic acids.

[0126] Example 52 is the subject of Example 51, wherein one or more carboxylic acids include at least one of hexanoic acid or oleic acid.

[0127] Example 53 is the subject of Example 49, wherein one or more polymer materials include monomer units having one or more alkanethiols.

[0128] Example 54 is the subject of Example 53, wherein one or more alkanethiols include at least one of hexanethiol or octanthiol.

[0129] Example 55 is the subject of Example 49, wherein one or more polymer materials contain monomer units having one or more mercaptoalkanoic acids.

[0130] Example 56 is the subject of Example 55, wherein one or more mercaptoalkanoic acids include mercaptohexadecanoic acid.

[0131] Example 57 is the subject of Example 49, wherein one or more polymer materials contain one or more monomer units having phosphine.

[0132] Example 58 is the subject of Example 57, wherein one or more phosphines include trioctylphosphine oxide or phosphinic acid.

[0133] Example 59 is the subject of Example 49, wherein one or more polymer materials contain monomer units having one or more amines.

[0134] Example 60 is the subject of Example 59, wherein one or more polymer materials include amine-terminated polyethylene glycol.

[0135] Example 61 is a subject matter described in any one of Examples 1 to 60, and comprises combining the first solution and the second solution with one or more surfactants.

[0136] Example 62 is the subject of Example 61, wherein one or more surfactants include one or more nonionic surfactants.

[0137] Example 63 is the subject of Example 62, wherein one or more nonionic surfactants include at least one of Igepearl, Triton, Bridge, Merge, NP80, NP95, Targitol, Decyl Glucoside, Lauryl Glucoside, Sucrose Laurate, Tween 85, or Pluronic.

[0138] Example 64 is the subject of Example 61, wherein one or more surfactants include one or more anionic surfactants.

[0139] Example 65 is the subject of Example 64, wherein one or more anionic surfactants include at least one of AOT, SDS, SLS, SDBS, stearic acid, oleic acid, lauric acid, or sulfated castor oil.

[0140] Example 66 is the subject of Example 61, wherein one or more surfactants include one or more cationic surfactants.

[0141] Example 67 is the subject of Example 66, wherein one or more cationic surfactants include at least one of CTAB, TMA, BTA, TMOA, HDTMA, or BDTA.

[0142] Example 68 is the subject of Example 61, wherein one or more surfactants include one or more amphoteric surfactants.

[0143] Example 69 is the subject of Example 68, wherein one or more amphoteric surfactants include at least one of cocamidopropyl betaine, dimethyl laurylamine N-oxide, myristamine oxide, SB12, SB16, or lecithin.

[0144] Example 70 is the subject of Example 61, wherein one or more surfactants contain fluorinated molecules.

[0145] Example 71 is the subject of Example 70, and the fluorinated molecule includes a perfluoropolyether.

[0146] Example 72 is the subject of Example 61, wherein one or more surfactants include glycol.

[0147] Example 73 is the subject of Example 72, and the glycol includes polyethylene glycol.

[0148] Example 74 is the subject of Example 61, wherein one or more surfactants include one or more first surfactants and one or more auxiliary surfactants.

[0149] Example 75 is the subject of Example 74, wherein one or more first surfactants include at least one of a nonionic surfactant, anionic surfactant, cationic surfactant, amphoteric surfactant, surfactant containing a fluorinated molecule, or glycol.

[0150] Example 76 is the subject of Example 74 or 75, wherein one or more auxiliary surfactants contain one or more alcohols.

[0151] Example 77 is the subject of Example 76, wherein one or more alcohols include at least one of isoamyl alcohol, hexanol, dodecanol, glycerol butanol, glycerol, or sorbitol.

[0152] Example 78 is the subject of Example 75, wherein one or more auxiliary surfactants include at least one of BZK or stearin.

[0153] Example 79 is a method comprising the steps of generating an aqueous solution containing a cosolvent, adding a lithium-containing reagent to the aqueous solution to generate a lithium-containing aqueous solution, and precipitating the lithium-containing aqueous solution to generate a precipitate containing particles composed of a lithium-containing compound, wherein at least one particle has a dimension of less than 10 micrometers.

[0154] Example 80 is the subject of Example 79, and the cosolvent is an alcohol.

[0155] Example 81 is the subject of Example 80, wherein the alcohol is an unsubstituted alcohol having 4 or fewer carbon atoms, or an aliphatic chain having 4 or fewer carbon atoms, and is a substituted alcohol in which one or more methyl groups are substituted.

[0156] Example 82 is the subject of Example 80 or 81, where the alcohol is methanol or ethanol.

[0157] Example 83 is the subject matter described in any one of Examples 79 to 82, wherein the step of producing an aqueous solution includes adding an acid to an initial solution containing water and a cosolvent.

[0158] Example 84 is the subject of Example 83, wherein the acid is an unsubstituted acid having 6 or fewer carbon atoms, or a substituted carboxylic acid having (i) an aliphatic chain having 6 or fewer carbon atoms, or (ii) a carbon chain having at least one alkenyl group, and the aliphatic chain or the carbon chain having at least one alkenyl group is optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxyl group, or a carboxyl group.

[0159] Example 85 is the subject of Example 83 or 84, and the acid is a carboxylic acid.

[0160] Example 86 is the subject of Example 85, and the carboxylic acid is a dicarboxylic acid.

[0161] Example 87 is the subject of any one of Examples 83 to 86, wherein the acid is oxalic acid, malonic acid, citric acid, succinic acid, or formic acid.

[0162] Example 88 is the subject matter described in any one of Examples 83 to 87, and includes the step of mixing an acid with an initial solution at a temperature of about 15°C to about 60°C for about 3 minutes to about 8 minutes.

[0163] Example 89 is the subject matter described in any one of Examples 79 to 88, and includes the step of mixing a lithium-containing reagent with an aqueous solution at a temperature of about 15°C to about 60°C for about 12 minutes to about 20 minutes.

[0164] Example 90 is the subject matter described in any one of Examples 79 to 89, and includes the step of performing a centrifugation process to separate the precipitate from the supernatant.

[0165] Example 91 is the subject matter described in any one of Examples 79 to 89, and includes the step of performing a vacuum filtration process to separate the precipitate from the supernatant.

[0166] Example 92 is the subject matter described in any one of Examples 79 to 91, and includes the step of carrying out a drying process for the precipitate.

[0167] Example 93 is the subject of Example 92, and the drying process involves heating the precipitate at a temperature of about 75°C to about 300°C for about 1 to 3 hours.

[0168] Example 94 is the subject matter described in any one of Examples 79 to 85, wherein the amount of lithium-containing reagent present in the aqueous solution is approximately 1% to 10% by weight.

[0169] Example 95 is the subject matter described in any one of Examples 83 to 88, wherein the amount of acid present in the aqueous solution is approximately 5% to 15% by weight.

[0170] Example 96 is the subject matter described in any one of Examples 79 to 95, wherein the ratio of the amount of water to the amount of cosolvent present in the aqueous solution is approximately 0.8 g to approximately 1.2 g of water to approximately 0.8 g to approximately 1.2 g of cosolvent.

[0171] Example 97 is the subject matter described in any one of Examples 79 to 96, wherein the amount of water present in the aqueous solution is approximately 30% to approximately 50% by weight.

[0172] Example 98 is the subject matter described in any one of Examples 79 to 97, wherein the amount of cosolvent present in the aqueous solution is about 30% to about 50% by weight.

[0173] Example 99 is the subject matter described in any one of Examples 79 to 98, wherein the yield of the lithium-containing compound relative to the amount of lithium-containing reagent present in the aqueous solution is approximately 85% to approximately 99%.

[0174] Example 100 is the subject matter described in any one of Examples 79 to 99, and includes the step of adding a carbon-based additive to a solution comprising water and a cosolvent before producing an aqueous solution.

[0175] Example 101 is the subject of Example 100, and the carbon-based additive is carbon black or carbon nanotubes.

[0176] Example 102 is the subject of Example 100 or 101, wherein the precipitate product is a matrix of carbon-based additives having a lithium-containing compound arranged in a matrix of carbon-based additives.

[0177] Example 103 is the subject of Example 102, and the product comprises about 15% to about 25% by weight of a carbon-based additive and about 75% to about 85% of a lithium-containing compound.

[0178] Example 104 is the subject matter described in any one of Examples 79 to 103, wherein the particles composed of a lithium-containing compound have a width of about 0.1 μm to about 0.8 μm, a length of about 1 μm to about 3 μm, and a rod-like shape.

[0179] Example 105 is the subject matter described in any one of Examples 79 to 104, wherein the particles composed of a lithium-containing compound have an aspect ratio of about 2 to 8.

[0180] Example 106 is the subject of Example 81, with butanol as the cosolvent.

[0181] Example 107 is the subject of Example 79 or 106, and the aqueous solution is produced by mixing water, a cosolvent, and a quaternary ammonium salt.

[0182] Example 108 is the subject of Example 107, and the quaternary ammonium salt includes cetrimonium bromide, tetramethylammonium bromide, tetramethylammonium hydroxide, hexadecyltrimethylammonium chloride, or benzyldimethyltetradecylammonium chloride.

[0183] Example 109 is the subject of Example 79 or 107, and the step of producing an aqueous solution includes adding an acid to an initial solution containing water and a cosolvent.

[0184] Example 110 is the subject of Example 109, wherein the acid is an unsubstituted acid having 6 or fewer carbon atoms, or a substituted carboxylic acid having (i) an aliphatic chain having 6 or fewer carbon atoms, or (ii) a carbon chain having at least one alkenyl group, and the aliphatic chain or the carbon chain having at least one alkenyl group is optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxyl group, or a carboxyl group.

[0185] Example 111 is the subject of Example 109 or 110, where the acid is a carboxylic acid.

[0186] Example 112 is the subject of Example 111, and the carboxylic acid is a dicarboxylic acid.

[0187] Example 113 is the subject of Example 112, where the carboxylic acid is oxalic acid, malonic acid, citric acid, succinic acid, or formic acid.

[0188] Example 114 is the subject matter described in either Example 79 or one of Examples 105 to 113, and includes the step of adding acetone to a lithium-containing aqueous solution to precipitate particles composed of a lithium-containing compound.

[0189] Example 115 is the subject matter described in either Example 79 or one of Examples 105-114, and includes the step of washing the precipitate one or more times with an additional co-solvent.

[0190] Example 116 is a subject described in either Example 79 or one of Examples 105 to 115, wherein an emulsion is produced by adding a lithium-containing reagent to an aqueous solution.

[0191] Example 117 is the subject matter described in any one of Examples 105 to 116, wherein the particles composed of a lithium-containing compound have a width of about 0.1 μm to about 0.8 μm, a length of about 1 μm to about 3 μm, and a rod-like shape.

[0192] Example 118 is the subject matter described in any one of Examples 105 to 117, wherein the particles composed of a lithium-containing compound have an aspect ratio of about 2 to 8.

[0193] Example 119 is the subject matter described in any one of Examples 105 to 118, and includes the step of performing a centrifugation process to separate the precipitate from the supernatant.

[0194] Example 120 is the subject matter described in any one of Examples 105 to 118, and includes the step of performing a vacuum filtration process to separate the precipitate from the supernatant.

[0195] Example 121 is the subject matter described in any one of Examples 105 to 120, and includes the step of carrying out a drying process for the precipitate.

[0196] Example 122 is the subject of Example 121, and the drying process involves heating the precipitate at a temperature of about 75°C to about 300°C for about 1 to about 3 hours.

[0197] Example 123 is the subject matter described in any one of Examples 105 to 122, wherein the yield of particles composed of the lithium-containing compound relative to the amount of lithium-containing reagent present in the aqueous solution is approximately 85% to approximately 99%. [Examples] [Examples]

[0198] Battery material particles were produced using a process that formed an initial solution containing an amount of water and an amount of ethanol or methanol. The volume ratio of water to ethanol or methanol was approximately 50% water to 50% ethanol or methanol. Oxalic acid was added to the initial solution and mixed for approximately 5 minutes to produce an intermediate solution. Lithium hydroxide was added to the intermediate solution and mixed for approximately 15 minutes. A centrifugation process was performed, followed by a drying process. Each operation was carried out under standard temperature and pressure. Lithium oxalate particles with a rod-like shape were produced. The yield from this process was approximately 99.3%. In particular, the lithium oxalate particles consisted of lithium oxalate nanorods with a diameter of approximately 0.3 μm and a length of approximately 2 μm. [Examples]

[0199] Battery material particles were produced using a process to form an initial solution containing amounts of water, butanol, and CTAB. Oxalic acid was added to the initial solution and mixed for an appropriate time to produce an intermediate solution forming a microemulsion. Lithium hydroxide was added to the intermediate solution and mixed for an appropriate time. Acetone was added to the resulting solution, followed by a centrifugation process. Three butanol washes were performed, followed by a drying process. Each operation was carried out under standard temperature and pressure. Lithium oxalate particles with a rod-like shape were produced. Figure 4 shows scanning electron microscope images 402 and X-ray diffraction analysis 404 of the lithium oxalate particles produced in this example. In particular, the lithium oxalate particles consist of lithium oxalate nanorods with a diameter of approximately 0.3 μm and a length of approximately 2 μm. [Examples]

[0200] Battery material particles were produced using a process that formed an initial solution containing an amount of water and an amount of ethanol or methanol. The volume ratio of water to ethanol or methanol was approximately 50% water to 50% ethanol or methanol. A carbon black additive was added to the initial solution and mixed for about 10 minutes. Then, oxalic acid was added to the initial solution and mixed for about 10 minutes to produce an intermediate solution. Lithium hydroxide was added to the intermediate solution and mixed for about 30 minutes. A centrifugation process was performed, followed by a drying process. Each operation was carried out under standard temperature and pressure. Lithium oxalate particles with a rod-like shape were produced. The yield from this process was approximately 95.4%. In particular, the lithium-containing particles consisted of lithium oxalate nanorods with a diameter of approximately 0.3 μm and a length of approximately 2 μm, arranged in a carbon black matrix.

Claims

1. A step of preparing an aqueous solution containing a cosolvent, A step of adding a lithium-containing reagent to the aqueous solution to produce a lithium-containing aqueous solution, A method comprising the steps of: precipitating the lithium-containing aqueous solution to produce a precipitate containing particles composed of a lithium-containing compound, wherein the particles have at least one dimension of less than 10 micrometers.

2. The method according to claim 1, wherein the cosolvent is an alcohol.

3. The method according to claim 2, wherein the alcohol is an unsubstituted alcohol having 4 or fewer carbon atoms, or an aliphatic chain having 4 or fewer carbon atoms, which is substituted with a methyl group at one or more positions.

4. The method according to claim 2, wherein the alcohol is methanol or ethanol.

5. The method according to claim 1, wherein the step of producing the aqueous solution comprises adding an acid to an initial solution containing water and the cosolvent.

6. The method according to claim 5, wherein the acid is an unsubstituted acid having 6 or fewer carbon atoms, or (i) an aliphatic chain having 6 or fewer carbon atoms, or (ii) a substituted carboxylic acid having a carbon chain having at least one alkenyl group, and the aliphatic chain or the carbon chain having at least one alkenyl group is optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxyl group, or a carboxyl group.

7. The method according to claim 5, wherein the acid is a carboxylic acid.

8. The method according to claim 7, wherein the carboxylic acid is a dicarboxylic acid.

9. The method according to claim 5, wherein the acid is oxalic acid, malonic acid, citric acid, succinic acid, or formic acid.

10. The method according to claim 5, comprising the step of mixing the acid with the initial solution for about 3 minutes to about 8 minutes at a temperature of about 15°C to about 60°C.

11. The method according to claim 1, comprising the step of mixing the lithium-containing reagent with the aqueous solution for about 12 minutes to about 20 minutes at a temperature of about 15°C to about 60°C.

12. The method according to claim 1, further comprising the step of performing a centrifugal separation process to separate the precipitate from the supernatant.

13. The method according to claim 1, further comprising the step of performing a vacuum filtration process to separate the precipitate from the supernatant.

14. The method according to claim 1, comprising the step of carrying out a drying process of the precipitate.

15. The method according to claim 14, wherein the drying process comprises heating the precipitate at a temperature of about 75°C to about 300°C for about 1 hour to about 3 hours.

16. The method according to claim 1, wherein the amount of the lithium-containing reagent present in the aqueous solution is about 1% by weight to about 10% by weight.

17. The method according to claim 5, wherein the amount of the acid present in the aqueous solution is about 5% by weight to about 15% by weight.

18. The method according to claim 1, wherein the ratio of the amount of water to the amount of the co-solvent present in the aqueous solution is approximately 0.8 mL to approximately 1.2 mL of water to approximately 0.8 mL to approximately 1.2 mL of the co-solvent.

19. The method according to claim 1, wherein the amount of water present in the aqueous solution is about 30% by weight to about 50% by weight.

20. The method according to claim 1, wherein the amount of the cosolvent present in the aqueous solution is about 30% by weight to about 50% by weight.

21. The method according to claim 1, wherein the yield of the lithium-containing compound relative to the amount of the lithium-containing reagent present in the aqueous solution is about 85% to about 99%.

22. The method according to claim 1, comprising the step of adding a carbon-based additive to a solution comprising water and the cosolvent before producing the aqueous solution.

23. The method according to claim 22, wherein the carbon-based additive is carbon black or carbon nanotubes.

24. The method according to claim 22, wherein the product of the precipitate is a matrix of carbon-based additives having the lithium-containing compound disposed in the matrix of carbon-based additives.

25. The method according to claim 24, wherein the product comprises about 15% to about 25% by weight of the carbon-based additive and about 75% to about 85% of the lithium-containing compound.

26. The method according to claim 1, wherein the particles composed of the lithium-containing compound have a width of about 0.1 μm to about 0.8 μm, a length of about 1 μm to about 3 μm, and a rod-like shape.

27. The method according to claim 1, wherein the particles composed of the lithium-containing compound have an aspect ratio of about 2 to 8.

28. The method according to claim 3, wherein the cosolvent is butanol.

29. The method according to claim 1, wherein the aqueous solution is produced by mixing water, the cosolvent, and the quaternary ammonium salt.

30. The method according to claim 29, wherein the quaternary ammonium salt comprises cetrimonium bromide, tetramethylammonium bromide, tetramethylammonium hydroxide, hexadecyltrimethylammonium chloride, or benzyldimethyltetradecylammonium chloride.

31. The method according to claim 29, wherein the step of producing the aqueous solution comprises adding an acid to an initial solution containing water and the cosolvent.

32. The method according to claim 31, wherein the acid is an unsubstituted acid having 6 or fewer carbon atoms, or (i) an aliphatic chain having 6 or fewer carbon atoms, or (ii) a substituted carboxylic acid having a carbon chain having at least one alkenyl group, and the aliphatic chain or the carbon chain having at least one alkenyl group is optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxyl group, or a carboxyl group.

33. The method according to claim 31, wherein the acid is a carboxylic acid.

34. The method according to claim 33, wherein the carboxylic acid is a dicarboxylic acid.

35. The method according to claim 34, wherein the carboxylic acid is oxalic acid, malonic acid, citric acid, succinic acid, or formic acid.

36. The method according to claim 29, comprising the step of adding acetone to the lithium-containing aqueous solution to precipitate particles composed of the lithium-containing compound.

37. The method according to claim 29, further comprising the step of washing the precipitate once or more with an additional cosolvent.

38. The method according to claim 29, wherein the lithium-containing reagent is added to the aqueous solution to produce an emulsion.

39. The method according to claim 29, wherein the particles composed of the lithium-containing compound have a width of about 0.1 μm to about 0.8 μm, a length of about 1 μm to about 3 μm, and a rod-like shape.

40. The method according to claim 29, wherein the particles composed of the lithium-containing compound have an aspect ratio of about 2 to 8.

41. The method according to claim 29, further comprising the step of performing a centrifugal separation process to separate the precipitate from the supernatant.

42. The method according to claim 29, further comprising the step of performing a vacuum filtration process to separate the precipitate from the supernatant.

43. The method according to claim 29, comprising the step of carrying out a drying process of the precipitate.

44. The method according to claim 43, wherein the drying process includes the step of heating the precipitate at a temperature of about 75°C to about 300°C for about 1 hour to about 3 hours.

45. The method according to claim 29, wherein the yield of particles composed of the lithium-containing compound relative to the amount of the lithium-containing reagent present in the aqueous solution is about 85% to about 99%.

Images