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WO2025019829A2 - Synthesis of nanostructured battery materials - Google Patents

Synthesis of nanostructured battery materials Download PDF

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Publication number
WO2025019829A2
WO2025019829A2 PCT/US2024/038869 US2024038869W WO2025019829A2 WO 2025019829 A2 WO2025019829 A2 WO 2025019829A2 US 2024038869 W US2024038869 W US 2024038869W WO 2025019829 A2 WO2025019829 A2 WO 2025019829A2
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WO
WIPO (PCT)
Prior art keywords
lithium
acid
aqueous solution
examples
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
PCT/US2024/038869
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French (fr)
Other versions
WO2025019829A3 (en
Inventor
Sourav Roger Basu
Bonil Koo
Michael D SLATER
Donald A. Zehnder
Matthew A. KOLACZKOWSKI
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Coreshell Technologies Inc
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Coreshell Technologies Inc
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Publication of WO2025019829A2 publication Critical patent/WO2025019829A2/en
Publication of WO2025019829A3 publication Critical patent/WO2025019829A3/en
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027Negative electrodes

Definitions

  • This application generally relates to compositions of battery materials and the methods of fabrication thereof.
  • the energy density of a lithium-ion battery is typically limited by the specific capacity of its cathode.
  • High-Nickel stoichiometries of the state-of-the-art lithium-ion cathode material LiNi x Mn y Co z O2, where x ranges from -0.4-0.95, have demonstrated sufficiently high cycle lifetime to warrant use in applications such as electric vehicles, but their specific capacity is still limited to a maximum of approximately 200 milliampere hours (mAh)/gram (g) at full state-of-charge.
  • the state-of-the-art anode active material, graphite yields a much higher specific capacity of 350-372 mAh/g at full state-of-charge.
  • increasing the specific capacity of the cathode generally provides the greatest relative improvement to the cell-level energy density of a lithium-ion battery.
  • Figure 1 illustrates a process to produce battery material particles using one or more co-solvents in an aqueous solution to produce battery material particles, in accordance with one or more example implementations.
  • Figure 2 illustrates a framework to produce battery material particles using a microemulsion, in accordance with one or more example implementations.
  • Cathode materials such as LiNi x Mn y Co z O2 can be charged to specific capacities greater than 200 mAh/g by increasing their voltage limit during charging but doing so drastically reduces their cycle lifetime. Failure at high voltage is primarily due to the mechanical stress and strain experienced by the cathode during repeated insertion and removal of lithium across a wide range of lithium mole fraction, which fatigues and eventually cracks cathode particles.
  • the cathode materials which are polycrystalline “secondary” particles composed of numerous primary crystallites, tend to fracture along the grain boundaries between primary crystallites during cycling.
  • cathode surfaces are exposed to electrolyte, allowing for more locations where high impedance decomposition products can accumulate, and from where transition metals can be leached out of the cathode crystal lattice, effectively destroying active material. Furthermore, cracked fragments of cathode material can become electrically disconnected from the remainder of the electrode matrix, thereby becoming inactive material. [0007] If the cumulative area of grain boundaries per mass of cathode active material can be reduced, such surface related degradation phenomena could be mitigated.
  • One way to greatly reduce the proportion of grain boundaries in cathode active material is to increase the primary crystallite size, mainly through calcination at higher temperatures (i.e., > ⁇ 950°C). Higher calcination temperature promotes larger grain growth, which then reduces the electrochemically available surface area in the event of secondary particle fracture.
  • the cathode material LiFePCU whose specific power is limited by the relatively poor solid-state diffusivity of lithium through its crystal lattice, is observed to have substantially improved rate capability when its particle dimensions are reduced to ⁇ 1 pm.
  • the compound lithium ketomalonate which is a typically inactive and highly resistive lithium-containing possessing a high specific capacity of > 400 mAh/g, can be rendered electrochemically active, with a reasonable oxidation potential of ⁇ 4 V vs. Li/Li + , when its constituent particles are nanosized.
  • anode materials such as lithium titanate, which also suffers from poor electronic and ionic conductivity, are also observed to have greatly improved rate capability when their particle sizes are reduced to the nanoscale.
  • a useful feature of the co-precipitation process for battery material fabrication is that secondary particles typically do not grow to sizes substantially larger than 50 pm.
  • the 1 pm - 50 pm secondary particle size provides good lithium intercalation kinetics for reasonably rate- capable materials such as LiNi x Mn y Co z O2.
  • the co-precipitation process tends to produce spherical particles, which also provides satisfactory tap density while minimizing active material surface area, thereby mitigating surface-related degradation phenomena.
  • One way to limit cathode precursor size during synthesis is to limit reagent access to the surface of precursor nuclei through some form of particle confinement or surface protection. This approach is commonly exploited in the solution-phase synthesis of colloidal suspensions of nanoparticles, for instance, where nanoparticle surfaces can be stabilized through the addition of “ligands”.
  • Ligands are typically short chain molecules possessing one end moiety which strongly coordinates to the nanoparticle surface after nucleation, and another end which strongly coordinates to solvent molecules and helps maintain particle suspension.
  • the ligands form a capping shell around the nanoparticle, which prevents additional reagent from reacting with the particle surface, thereby limiting any further growth. Utilizing ligandbased particle confinement is particularly useful for creating fairly monodisperse nanoparticle dispersions with average size on the order of a few nanometers.
  • microemulsions are dispersions of two immiscible solvents that are stabilized through the presence of surfactants.
  • Microemulsions are typically characterized as oil-in-water (o/w) or water-in-oil (w/o) dispersions, though the concept can be generalized to various combinations of solvents that simply differ sufficiently in their polarity/miscibility.
  • Microemulsions often appear to be macroscopically homogeneous, but in reality, they possess a fine dispersion of microscopic micelles comprising one phase within the other, where the small size of the micelles and their uniform distribution renders the overall mixture non-scattering and optically transparent. Microemulsions can be useful for the controlled synthesis of nanoparticles with uniform distribution and morphology, because the micelles within the emulsion provide “nanoreactors” within which size-confined synthesis can take place.
  • Microemulsions can be well suited for the synthesis of battery materials because they provide a means to uniformly control particle dimensions within the desired range of singledigit nanometers to several microns.
  • the morphology and particle size of the battery materials can be precisely controlled by varying the compositions and relative amounts of the two immiscible phases, the primary surfactant and the co-surfactant, as well as by varying process parameters such as temperature and ambient pressure.
  • Implementations herein are directed to producing battery material particles with one or more dimensions no greater than 1 micrometer without using a grinding process or other process to reduce the size of the particles formed by the processes and methods described herein. For example, microemulsions can be produced that can be used to produce battery material particles.
  • the microemulsions can include a first phase comprised of a first solution and a second phase comprised of a second solution.
  • the second phase can include droplets that are dispersed throughout the first phase.
  • the composition of the second solution can include precursors of battery material particles.
  • one or more reactions can take place with respect to the compounds included in the second solution to produce battery material particles within the droplets.
  • the droplets can have dimensions that limit the size of battery material particles produced within the droplets. For example, the droplets can have dimensions that limit one or more dimensions of the battery material particles to less than 1 pm.
  • a way to influence the particle size during precipitation of battery materials and battery material precursors from solution is to introduce additional co-solvents besides water into the reaction solution.
  • battery material particles can also be produced having at least one dimension no greater than 1 pm without performing a grinding process or another process to reduce the size of the particles that have been formed using the methods and processes herein.
  • a 50:50 mixture by volume of water and methanol is used in place of 100% water for the synthesis of a battery material precursor such as Ni(0H)2.
  • the pH of the solution and precipitation of hydroxide can be controlled through the addition of ammonia.
  • a lithium-containing compound such as lithium ketomalonate can be synthesized using a water: methanol solvent mixture.
  • LiOH can first be added to a 50:50 mixture (by volume) of water and methanol. Once the hydroxide is dissolved, ketomalonic acid can be added to the reaction solution. As the product, lithium ketomalonate, is highly insoluble in the reaction solution, it will precipitate.
  • FIG. 1 illustrates a process 100 to produce battery material particles using one or more co-solvents in an aqueous solution to produce battery material particles, in accordance with one or more example implementations.
  • the process 100 can be performed to produce battery material particles according to a number of techniques.
  • the process 100 can include operations of a microemulsion process that can be implemented to produce battery material particles.
  • the process 100 can include operations of a non-microemulsion process to produce battery material particles.
  • some operations of the process 100 can generally be the same between the microemulsion process and the non-microemulsion process, the specific implementation of these operations can be different.
  • the process 100 can be performed in one or more reaction vessels with individual reaction vessels having a volume of 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.
  • L at least 0.1 liters
  • the process 100 can be performed in one or more reaction vessels with individual reaction vessels having a volume from about 0.1 L to about 500 L, from about 1 L to about 400 L, from about 2 L to about 300 L, from about 5 L to about 200 L, from about 10 L to about 100 L, from about 0.1 L to about 1 L, from about 1 L to about 10 L, from about 10 L to about 50 L, from about 50 L to about 100 L, from about 100 L to about 150 L, from about 150 L to about 200 L, from about 200 L to about 250 L, from about 250 L to about 500 L, or from about 500 L to about 1000 L.
  • the one or more reaction vessels used to carry out the process 100 can include one or more mixing devices.
  • the one or more mixing devices can include one or more agitation mixing devices.
  • the one or more mixing devices can include one or more rotating paddles.
  • the one or more mixing devices can include one or more jet mixing devices.
  • the one or more mixing devices can include one or more hypersonic mixing devices.
  • the one or more reaction vessels used to carry out the process 100 can also include and/or be coupled to one or more temperature control devices.
  • the one or more temperature control devices can operate to at least one of heat or cool liquids within the one or more reaction vessels.
  • the one or more temperature control devices can include at least one of one or more electric heating elements, one or more chemical heating elements, one or more flame-based heating elements, one or more heat exchangers, one or more refrigeration cooling elements, one or more fans, or one or more ventilation devices.
  • the process 100 can include, at 102, preparing an initial solution.
  • the initial solution can include an aqueous solution and one or more co-solvents.
  • the preparation of the initial solution can include operation 104.
  • the process 100 can include combining water and one or more co-sol vents that can be soluble in water and can be soluble with respect to each other.
  • the one or more cosolvents can be soluble in water and with respect to each other at temperatures from about 15 °C to about 30 °C and at standard pressures of about 101 kilopascals (kPa).
  • the one or more co-solvents can be soluble in water and with respect to each other at temperatures greater than about 30 °C and at pressures greater than about 101 kPa.
  • the one or more co-solvents can include one or more alcohols.
  • the one or more co-solvents can include one or more alcohols having a carbon chain with no greater than 10 carbon atoms, no greater than 9 carbon atoms, no greater than 8 carbon atoms, no greater than 7 carbon atoms, no greater than 6 carbon atoms, no greater than 5 carbon atoms, no greater than 4 carbon atoms, no greater than 3 carbon atoms, no greater than 2 carbon atoms, or no greater than 1 carbon atom.
  • the one or more cosolvents can include one or more alcohols having one or more rings with individual rings having no greater than 6 carbon atoms, no greater than 5 carbon atoms, or no greater than 4 carbon atoms.
  • the one or more co-solvents can include one or more alcohols having an aliphatic chain.
  • the one or more co-solvents can include one or more alcohols having a carbon chain with at least one alkenyl group.
  • the one or more cosolvents can include one or more single bonded cyclic alcohols or one or more phenolic alcohols.
  • the one or more co-solvents can include one or more alcohols with unsubstituted carbon atoms. In still other examples, the one or more cosolvents can include one or more alcohols with one or more substituted carbon atoms. In situations where the one or more co-solvents include one or more alcohols with one or more substituted carbon atoms, the carbon atoms can be substituted with at least one of a methyl group, an amine group, a carboxylate group, or a nitro group. In various illustrative examples, the one or more co-solvents can include methanol. In one or more additional scenarios, the one or more co-solvents can include ethanol.
  • water and the one or more co-solvents can be combined such that at least 40% by volume of the initial solution can be water, at least 45% by volume of the initial solution is can be water, at least 50% by volume of the initial solution can be water, at least 55% by volume of the initial solution can be water, a least 60% of the volume of the initial solution can be water, at least 65% of the volume of the initial solution can be water, or at least 70% of the volume of the initial solution can be water.
  • the initial solution can include from about 40% by volume water to about 75% by volume water, from about 50% by volume water to about 70% by volume water, from about 45% by volume water to about 55% by volume water, from about 50% by volume water to about 60% by volume water, from about 55% by volume water to about 65% by volume water, from about 60% by volume water to about 70% by volume water, or from about 65% by volume water to about 75% by volume water.
  • At least 25% by volume of the initial solution can be one or more co-solvents
  • at least 30% by volume of the initial solution can be one or more co-solvents
  • at least 35% by volume of the initial solution can be co-solvents
  • at least 40% by volume of the initial solution can be one or more co-solvents
  • at least 45% by volume of the initial solution is can be one or more co-solvents
  • at least 50% by volume of the initial solution can be one or more co-solvents
  • at least 55% by volume of the initial solution can be one or more co-solvents.
  • the initial solution can include from about 25% by volume of one or more co-sol vents to about 60% by volume of one or more co-sol vents, from about 30% by volume of one or more co-solvents to about 50% by volume of one or more co-solvents, from about 40% by volume of one or more co-solvents to about 50% by volume of one or more co-solvents, from about 45% by volume of one or more co-solvents to about 55% by volume of one or more co-solvents, or from about 50% by volume of one or more co-solvents to about 60% by volume of one or more co-solvents.
  • a volume ratio of the amount of the one or more cosolvents present in the initial solution in relation to the amount of water present in the initial solution can be from about 0.7: 1.3 to about 1.3:0.7, from about 0.8: 1.2 to about 1.2:0.8, from about 0.85: 1.15 to about 1.15:0.85, from about 1.1 : 0.9 to about 0.9: 1.1, from about 0.95: 1.05 to about 1.05:0.95.
  • a volume ratio of the amount of the one or more cosolvents present in the aqueous solution in relation to the amount of water present in the aqueous solution can be about 1 : 1.
  • the initial solution can contain about 50% by volume water and about 50% by volume of one or more alcohols.
  • the one or more alcohols can include methanol or ethanol.
  • Water and the one or more co-solvents can be combined at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C.
  • the initial solution can also be prepared at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa.
  • the water and the one or more co-sol vents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 3 minutes, from about 2 minutes to about 4 minutes, or from about 3 minutes to about 5 minutes.
  • the preparation of the initial solution can include, at 106, combining water with at least two immiscible reagents.
  • the at least two immiscible reagents can include one or more first reagents.
  • the one or more first reagents can 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 glymes, or one or more ethers.
  • the one or more first reagents can include butanol.
  • the at least two immiscible reagents can also include one or more second reagents.
  • the one or more second reagents can include one or more surfactants.
  • the one or more surfactants can include one or more non-ionic surfactants.
  • the one or more non-ionic surfactants can include igepal, triton, brij, myij, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, pluronic, or one or more combinations thereof.
  • the one or more surfactants can include one or more anionic surfactants.
  • the one or more anionic surfactants can include sodium bis(2-ethylhexyl)sulfosuccinate (AOT), Sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), Sodium Dodecylbenzene Sulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulphated castor oil, or one or more combinations thereof.
  • the one or more surfactants can include one or more cationic surfactants.
  • the one or more cationic surfactants can include Cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), Hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or one or more combinations thereof.
  • CTAB Cetrimonium bromide
  • TMA tetramethylammonium
  • BTA benzotriazole
  • TMOA trimethylamine-N-oxide
  • HDTMA Hexadecyltrimethylammonium
  • BDTA benzyldimethyltetradecylammonium
  • the one or more surfactants can include one or more zwitterionic surfactants.
  • the one or more zwitterionic surfactants can include cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB 12, SB 16,
  • the one or more surfactants can include a fluorinated molecule. In one or more illustrative examples, the one or more surfactants can include a perfluoro polyether. In one or more additional illustrative examples, the one or more surfactants can include a glycol. To illustrate, the one or more surfactants can include a polyethylene glycol. In one or more illustrative examples, the one or more second reagents can include one or more quaternary ammonium salts. In various illustrative examples, the one or more second reagents can include Cetrimonium bromide.
  • the combination of water with one or more first reagents and the one or more second reagents can produce an initial solution that comprises a microemulsion.
  • an amount of at least one first reagent in the initial solution can be from about 10% by weight to about 50% by weight or from about 20% by weight to about 40% by weight
  • an amount of a second solvent can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight
  • a remainder of the at least one additional first reagents or the one or more second reagents can be from about 10% by weight to about 50% by weight or from about 20% by weight to about 40% by weight
  • an amount of a second solvent can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight
  • a remainder of the at least one additional first reagents or the one or more second reagents can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight
  • the initial solution in implementations where the initial solution includes at least one or more surfactants and one or more solvents, where the one or more solvents can include water, can include from about 10% by weight to about 80% by weight of the one or more solvents, from about 20% by weight to about 60% by weight of the one or more solvents, or from about 40% by weight to about 80% by weight of one or more solvents.
  • the initial solution can also include from about 5% by weight to about 40% by weight of one or more surfactants, from about 10% by weight to about 30% by weight of one or more surfactants, or from about 5% by weight to about 25% by weight of one or more surfactants.
  • a remainder of the initial solution can include one or more additional reagents.
  • the initial solution can include no greater than about 50% by weight water and no greater than about 20% by weight of one or more alcohols with a remainder of the mixture comprising one or more reagents, such as one or more surfactants.
  • Water and the immiscible reagents can be combined at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C.
  • the initial solution can also be prepared at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa.
  • the water and the immiscible reagents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 3 minutes, from about 2 minutes to about 4 minutes, or from about 3 minutes to about 5 minutes.
  • the amounts of individual reagents included in initial solution can be based on the reagents used to produce the initial solution.
  • the amounts of individual reagents included in the initial solution can be based on solubility limits of one or more individual reagents with respect to one or more additional reagents of the initial solution.
  • amounts of one or more reagents included in the initial solution can be based on solubility limits of the one or more reagents in water.
  • the process 100 can include adding one or more reagents to the initial solution to produce an aqueous solution including one or more co-solvents.
  • the one or more reagents added to the initial solution can include one or more acidic compounds.
  • the one or more acidic compounds can include an unsubstituted acid having no greater than 6 carbon atoms.
  • the one or more acidic compounds can include a substituted carboxylic acid having an aliphatic chain of no greater than 6 carbon atoms.
  • the one or more acidic compounds can include an unsubstituted carbon chain having at least one alkenyl group.
  • the one or more acidic compounds can include an unsubstituted carbon chain having at least one alkenyl group.
  • the chains can be substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxide group, or a carboxyl group.
  • the one or more reagents added to the initial solution can include one or more carboxylic acids.
  • the one or more reagents added to the initial solution can include one or more dicarboxylic acids. In one or more further illustrative examples, the one or more reagents added to the initial solution can include succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, citric acid, formic acid, or one or more combinations thereof.
  • the one or more reagents can be added to the initial solution at 108 at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C.
  • the one or more reagents can be added to the initial solution at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa.
  • the one or more reagents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 4 minutes, from about 2 minutes to about 6 minutes, from about 3 minutes to about 8 minutes, or from about 4 minutes to about 10 minutes.
  • the process 100 can include, at 110, producing a lithium-containing aqueous solution.
  • one or more lithium-containing compounds can be added to the aqueous produced at 108 to produce the lithium-containing aqueous solution.
  • the one or more lithium-containing compounds can include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof.
  • the one or more lithium-containing compounds can be added to the aqueous solution, at 110, at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C.
  • the one or more lithium-containing compounds can be added to the aqueous solution, at 110, at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa. Further, the one or more lithium-containing compounds and the aqueous solution can be mixed, at 110, for a duration from about 3 minutes to about 45 minutes, from about 5 minutes to about 30 minutes, from about 10 minutes to about 20 minutes, from about 5 minutes to about 10 minutes, from about 10 minutes to about 15 minutes, from about 15 minutes to about 20 minutes, from about 20 minutes to about 25 minutes, or from about 25 minutes to about 30 minutes.
  • the process 100 can include causing precipitation of the lithium- containing aqueous solution to produce precipitate including lithium-containing particles.
  • the precipitation process can form a precipitant that includes the lithium-containing particles and a supernatant that includes the residual liquid.
  • the lithium- containing particles can include a lithium-containing salt.
  • the precipitation of the lithium- containing aqueous solution can include performing at least one of one or more mechanical process or one or more chemical processes.
  • the precipitation of the lithium-containing aqueous solution can take place when the lithium-containing reagent from operation 110 is added to the aqueous solution and the lithium-containing reagent dissolves in the aqueous solution.
  • the reaction that produces the lithium- containing compound can take place.
  • the lithium-containing compound can crystallize to produce the lithium-containing particles.
  • one or more alcohols present in the aqueous solution can cause the crystallization of the lithium-containing compound to form the lithium-containing particles.
  • the lithium-containing reagent can dissolve in the aqueous solution with sufficient mixing at relatively low temperatures, such as no greater than 30 °C.
  • the lithium-containing reagent can also dissolve in the aqueous solution with less mixing at relatively higher temperatures, such as temperatures of at least 30 °C.
  • the precipitation of the lithium-containing solution can take place in response to one or more additional reagents being added to the lithium-containing aqueous solution.
  • the aqueous solution produced at 108 can include at least two phases.
  • the at least two phases can include an aqueous phase and a second phase including droplets that are disposed in the first phase.
  • the second phase can include droplets encased in a barrier.
  • the barrier can be comprised of surfactant molecules.
  • the addition of the lithium-containing reagent to the aqueous solution at 110 can cause lithium-containing compounds to form within the droplets of the second phase.
  • the disruption of the barriers of the second phase can cause the lithium-containing compounds formed within the second phase to precipitate out of the droplets.
  • the barrier of the second phase can be disrupted through at least one of one or more physical processes or one or more chemical processes.
  • the barriers of the droplets can be disrupted using one or more mixing devices.
  • the barriers of the droplets can also be disrupted by heating the lithium-containing aqueous solution.
  • the barriers of the droplets can be broken by disrupting the equilibrium of the microemulsion by adding one or more additional reagents to the lithium-containing aqueous solution. To illustrate, adding a sufficient amount of acetone to the lithium-containing aqueous solution can cause the lithium-containing compounds to be released from the droplets.
  • At least a portion of the amount of additional reagent added to disrupt the equilibrium of the microemulsion can be recycled.
  • an amount of the additional reagent recovered from the barrier disruption process can be re-used in one or more other operations of the process 100 where appropriate.
  • lithium-containing particles can be formed within the droplets, while in other examples, lithium-containing particles can be formed when lithium- containing compounds formed in the droplets are released.
  • the process 100 can include performing one or more separations processes.
  • the one or more separation processes can separate the lithium-containing particles from residual liquid.
  • the one or more separations processes can include centrifugation.
  • the one or more separations processes can include one or more filtration processes.
  • the one or more separations processes can include one or more vacuum filtration processes.
  • the process 100 can include performing a drying process for the lithium - containing particles.
  • the drying process can be performed at temperatures 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.
  • the drying process can take place at temperatures from about 50 °C to about 500 °C, from about 75 °C to about 300 °C, from about 100 °C to about 250 °C, from about 50 °C to about 250 °C, from about 100 °C to about 300 °C, from about 300 °C to about 500 °C, from about 100 °C to about 200 °C, from about 150 °C to about 250 °C, from about 200 °C to about 300 °C, or from about 250 °C to about 350 °C.
  • the drying process can take place for a duration 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.
  • the drying process can be performed for durations from about 15 minutes to about 12 hours, from about 30 minutes to about 6 hours, from about 30 minutes to about 2 hours, from about 1 hour to about 3 hours, from about 2 hours to about 4 hours, from about 3 hours to about 5 hours, or from about 4 hours to about 6 hours.
  • the process 100 can include, at 118, performing one or more washes between the one or more separations process performed at 114 and the drying process performed at 116.
  • the one or more washes can be performed with one or more reagents that comprise the initial solution.
  • the one or more washes can be performed using one or more alcohols present in the initial solution.
  • the one or more washes can be performed using butanol.
  • an amount of the reagent used to perform the one or more washes can be recycled and re-used in subsequent washing operations.
  • performing the one or more alcohol washes at 118 can include performing a first butanol wash, a second butanol wash, and a third butanol wash.
  • butanol recovered from the first butanol wash can be used in the second butanol wash and butanol recovered from at least one of the first butanol wash or the second butanol wash can be used in the third butanol wash.
  • the lithium-containing particles can have a number of shapes.
  • the lithium-containing particles can be shaped as spheres, pellets, or rods.
  • the lithium-containing particles can have a coefficient of variation in the aspect ratio of the lithium-containing particles that can be no greater than 1%, no greater than 5%, no greater than 10%, no greater than 15%, no greater than 20%, no greater than 25%, or no greater than 30%.
  • the coefficient of variation can correspond to a ratio of a standard deviation of a size distribution of the lithium-containing particles with respect to a mean of the size distribution of the lithium-containing particles.
  • the spheres can have an aspect ratio of about 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more illustrative examples, the spheres can have an aspect ratio from about 0.9 to about 1.25, from about 0.95 to about 1.15, or from about 1 to 1.1.
  • the pellets can have an aspect ratio 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 one or more additional illustrative examples, the pellets can have an aspect ratio from about 0.9 to about 1.4, from about 1 to about 1.3, from about 1.1 to about 1.2, from about 1 to about 1.2, or from about 0.9 to about 1.2.
  • the rods can have an aspect ratio 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.
  • the lithium-containing particles can have one or more dimensions no greater than 5 micrometers (pm), no greater than 2 pm, no greater than 1 pm, no greater than 0.8 pm, no greater than 0.6 pm, no greater than 0.4 pm, no greater than 0.2 pm, no greater than 0.1 pm, or no greater than 0.05 pm.
  • the battery material particles can have dimensions from about 0.05 pm to about 5 pm, from about 0.1 pm to about 1 pm, from about 0.3 pm to about 3 pm, from about 0.5 pm to about 2 pm, or from about 0.05 pm to about 0.8 pm.
  • the lithium- containing particles can be in the form of rods having a diameter from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 5 pm.
  • a yield of the process 100 can be at least 80%, at least 85%, at least 90%, at least 95%, or at least 99%. In one or more illustrative examples, the yield can be from about 80% to about 99.9%, from about 85% to about 99.5%, from about 90% to about 99%, from about 90% to about 99.9%, or from about 95% to about 99.9%. The yield can be calculated based on a weight of the lithium-containing particles produced in relation to an amount of the lithium-containing reagent used in the process 100 at 110.
  • a conductive additive can be added to the initial solution.
  • the conductive additive can include a carbon-containing material.
  • the carbon-based additive can include carbon black or carbon nanotubes.
  • reaction conditions for at least one of operations 102, 108, 110, or 112 can increase.
  • the product produced by the process 100 when a conductive additive is used in the non-microemulsion implementations can include lithium-containing particles disposed on a matrix of the conductive additive.
  • the lithium-containing compound particles can be used in the production of lithium ion batteries.
  • the lithium-containing compound particles can be included in anodes of lithium ion batteries.
  • the lithium- containing compound particles can comprise active materials of anodes of lithium ion batteries.
  • the process 100 has been described with respect to the production of lithium- containing particles.
  • the process 100 can also be implemented to produce particles having a different composition.
  • the process 100 can be implemented to produce nickel hydroxide particles.
  • a nickel-containing compound can be added to the aqueous solution to produce a nickel-containing solution.
  • the nickel-containing compound can include a nickel II salt.
  • Nickel hydroxide particles can then be precipitated from the nickel- containing solution.
  • potassium hydroxide can be used to form the nickel hydroxide.
  • Figure 2 illustrates a framework 200 to produce battery material particles using a microemulsion, in accordance with one or more example implementations.
  • the framework 200 can implement one or more of the operations performed with respect to the microemulsion implementations of the process 100 described in relation to Figure 1. Additionally, at least some of the operations performed in relation to the framework 200 can correspond to one or more operations performed with respect to the microemulsion implementations of the process 100 described in relation to Figure 1. Further, 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 of the microemulsion implementations of the process 100 described in relation to Figure 1.
  • the framework can include a reaction vessel 202.
  • the reaction vessel 202 can have a volume, such as 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.
  • the reaction vessel 202 can include one or more mixing devices 204.
  • the one or more mixing devices 204 can include one or more agitation mixing devices.
  • the one or more mixing devices 204 can include one or more rotating paddles.
  • the one or more mixing devices 204 can include one or more jet mixing devices.
  • the one or more mixing devices 204 can include one or more hypersonic mixing devices.
  • a first solution 206 can be added to the reaction vessel 202.
  • the first solution 206 can include one or more first solvents.
  • the one or more first solvents can include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more glymes, one or more ethers, or one or more combinations thereof.
  • a second solution 208 can also be added to the reaction vessel 202.
  • the second solution 208 can include one or more second solvents.
  • the one or more solvents included in the second solution 208 can be selected such that the second solution 208 and the first solution 206 are immiscible.
  • At least one of the one or more solutions 206, 208 can include one or more reagents.
  • the one or more reagents can be dissolved in the one or more solutions 206, 208.
  • an amount of a first solvent can be from about 10% by weight to about 50% by weight or from about 20% by weight to about 40% by weight
  • an amount of a second solvent can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight
  • a remainder of the at least one of the first solution or the second solution can include one or more reagents.
  • the mixture can include from about 10% by weight to about 80% by weight, from about 20% by weight to about 60% by weight, or from about 40% by weight to about 80% by weight of one or more solvents, from about 5% by weight to about 40% by weight, from about 10% by weight to about 30% by weight, or from about 5% by weight to about 25% by weight of one or more surfactants 210, and a remainder of the mixture can include one or more reagents.
  • a mixture including the first solution 206 and the second solution 208 can include no greater than about 50% by weight water and no greater than about 20% by weight of one or more alcohols with a remainder of the mixture comprising one or more reagents.
  • the amounts of individual reagents included in at least one of the first solution 206 or the second solution 208 can be based on the composition of the first solution 206 and/or the composition of the second solution 208.
  • the amounts of individual reagents included in at least one of the first solution or the second solution 208 can be based on solubility limits of one or more individual reagents in at least one of the first solution 206 or the second solution 208.
  • amounts of one or more reagents included in at least one of the first solution 206 or the second solution 208 can be based on solubility limits of the one or more reagents in water.
  • first phase 212 can comprise the first solution 206 and, in at least some instances, one or more additional liquids, such as one or more surfactants 210.
  • second phase 214 can include droplets that comprise at least the second phase 214.
  • the second phase 214 can include droplets of the second solution 208 encased in a barrier.
  • the barrier can be comprised of surfactant molecules.
  • the first phase 212 and the second phase 214 can comprise a microemulsion.
  • the first solution 206, the second solution 208, and optionally the one or more surfactants 210 can be combined under temperature and pressure conditions that cause a microemulsion to be formed within the reaction vessel 202 that includes the first phase 212 and the second phase 214.
  • the first solution 206, the second solution 208, and, optionally the one or more surfactants 210 can be combined at temperatures from about 10 °C to about 100 °C, from about 20 °C to about 90 °C, from about 30 °C to about 80 °C, from about 20 °C to about 50 °C, or from about 25 °C to about 75 °C to produce a microemulsion within the reaction vessel 202.
  • first solution 206, the second solution 208, and optionally the one or more surfactants 210 can be combined at pressures from about 90 kilopascals (kPa) to about 120 kPa or from about 95 kPa to about 105 kPa produce a microemulsion within the reaction vessel 202.
  • kPa kilopascals
  • a microemulsion can be formed at temperatures and pressures that cause CO2 to behave as a supercritical fluid.
  • a microemulsion can be formed at temperatures of at least about 30 °C and pressures of at least about 7 megapascals (MPa).
  • the one or more reagents can include one or more lithium- containing components.
  • the one or more reagents can include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof.
  • the one or more reagents can include one or more transition metal halides.
  • the one or more reagents can include at least one of FeCh, NiCh.
  • the one or more reagents can include one or more transition metal sulfates.
  • the one or more reagents can include at least one of FeSCU or NiSCU.
  • the one or more reagents can include one or more basic compounds.
  • the one or more reagents can include sodium hydroxide, ammonium hydroxide, lithium hydroxide, or one or more combinations thereof.
  • the one or more reagents can also include one or more organic acids.
  • the one or more reagents can include succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, or one or more combinations thereof.
  • the one or more surfactants can include one or more non-ionic surfactants.
  • the one or more non-ionic surfactants can include igepal, triton, brij, myrj, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, pluronic, or one or more combinations thereof.
  • the one or more surfactants can include one or more anionic surfactants.
  • the one or more anionic surfactants can include sodium bis(2- ethylhexyl)sulfosuccinate (AOT), Sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), Sodium Dodecylbenzene Sulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulphated castor oil, or one or more combinations thereof.
  • the one or more surfactants can include one or more cationic surfactants.
  • the one or more cationic surfactants can include Cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), Hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or one or more combinations thereof.
  • CTAB Cetrimonium bromide
  • TMA tetramethylammonium
  • BTA benzotriazole
  • TMOA trimethylamine-N-oxide
  • HDTMA Hexadecyltrimethylammonium
  • BDTA benzyldimethyltetradecylammonium
  • the one or more surfactants can include one or more zwitterionic surfactants.
  • the one or more zwitterionic surfactants can include cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB12, SB
  • the one or more surfactants can include a fluorinated molecule. In one or more illustrative examples, the one or more surfactants can include a perfluoro polyether. In one or more additional illustrative examples, the one or more surfactants can include a glycol. To illustrate, the one or more surfactants can include a polyethylene glycol.
  • the one or more surfactants 210 can include one or more cosurfactants.
  • the one or more surfactants 210 can include a first surfactant and a co-surfactant.
  • the first surfactant can include at least one of a non-ionic surfactant, an anionic surfactant, a cationic surfactant, a zwitterionic surfactant, a surfactant including a fluorinated molecule, or a glycol.
  • the one or more cosurfactants can include one or more alcohols.
  • the one or more co-surfactants can include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, sorbitol, or one or more combinations thereof.
  • the one or more co-surfactants can include at least one of Benzalkonium Chloride (BZK) or Stearin.
  • the first solution 206 and the second solution 208 and, optionally the one or more surfactants 210 can be combined in the reaction vessel 202 at reaction conditions 216 to cause the one or more reagents to participate in one or more reactions that produce battery material particles 218.
  • the reaction conditions 216 can include effective temperatures, pressures, and amounts of reagents to produce the battery material particles 218.
  • reagents included in the first solution 206 and the second solution 208 can be combined at the reaction conditions 216 to cause precipitation of the battery material particles 218.
  • one or more reagents included in the first phase 212 can migrate into the second phase 214 and react with one or more additional reagents included in the second phase to produce the battery material particles 218.
  • the reaction conditions 216 can include temperatures from 10 °C to about 100 °C and pressures from about 90 kPa to about 120 kPa.
  • the battery material particles 218 can include one or more cathode active material precursors.
  • X can include a dianionic radical.
  • the dianionic radical can include CO3 or C2O4.
  • X can include two monovalent anions.
  • the two monovalent anions can include (OH) 2 or OH 2 -VF.
  • A can include one or more cationic dopants.
  • the one or more cationic dopants can include Al, Mg, Ti, Zr, Cr, Ru, Mo, V, or one or more combinations thereof.
  • the battery material particles 218 can also include one or more lithium-containings.
  • the battery material particles 218 can 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 hydroxyl amine, lithium oxalate, lithium succinate, lithium dimethyl succinate, lithium fumarate, lithium 2-methylfumarate, maleic acid dilithium- containing, 2-m ethyl maleic acid dilithium-containing, 1,4-hydroquinone dilithium - containing, catechol dilithium-containing, lithium poly(hydroquinone), lithium (1S,2S)- cyclopentane-l,2-dicarboxylate, lithium (lS,2S)-cyclohexane-l,2-dicarboxylate, lithium mal onate, hydrazin
  • the battery material particles 218 can include one or more cathode active materials.
  • the one or more cathode active materials can include one or more transition metal fluorides.
  • A can include one or more cationic dopants.
  • the one or more cationic dopants can include at least one of Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.
  • the battery material particles 218 can include one or more anode active materials.
  • the one or more anode active materials can include at least one of Li ⁇ isOn, LiNbsOs, or hydroxyamine hydrochloride.
  • the battery material particles 218 can include one or more anode active material precursors.
  • the one or more anode active material precursors can include at least one of TiO 2 or NbCh.
  • the battery material particles 218 can have various characteristics.
  • the battery material particles 218 can have a coefficient of variation in the aspect ratio of the battery material particles 218 that can be no greater than 1%, no greater than 5%, no greater than 10%, no greater than 15%, no greater than 20%, no greater than 25%, or no greater than 30%.
  • the coefficient of variation can correspond to a ratio of a standard deviation of a size distribution of the battery material particles with respect to a mean of the size distribution of the battery material particles.
  • the battery material particles 218 can include nanospheres.
  • the nanospheres can have an aspect ratio of about 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more illustrative examples, the nanospheres can have an aspect ratio from about 0.9 to about 1.25, from about 0.95 to about 1.15, or from about 1 to 1.1. In one or more further examples, the battery material particles 218 can include nanopellets.
  • the nanopellets can have an aspect ratio 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 one or more additional illustrative examples, the nanopellets can have an aspect ratio from about 0.9 to about 1.4, from about 1 to about 1.3, from about 1.1 to about 1.2, from about 1 to about 1.2, or from about 0.9 to about 1.2. Further, the battery material particles 218 can include nanorods.
  • the nanorods can have an aspect ratio 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.
  • the battery material particles 218 can have one or more dimensions no greater than 5 micrometers (pm), no greater than 2 pm, no greater than 1 pm, no greater than 0.8 pm, no greater than 0.6 pm, no greater than 0.4 pm, no greater than 0.2 pm, no greater than 0.1 pm, or no greater than 0.05 pm.
  • the battery material particles can have dimensions from about 0.05 pm to about 5 pm, from about 0.1 pm to about 1 pm, from about 0.3 pm to about 3 pm, from about 0.5 pm to about 2 pm, or from about 0.05 pm to about 0.8 pm.
  • the battery material particles 218 can have electrical conductivity of no greater than 9 x 10' 2 Siemens/centimeter (S/cm), no greater than 8 x 10' 2 S/cm, 7 x 10' 2 S/cm, 6 x 10' 2 S/cm, 5 x 10' 2 S/cm, 4 x 10' 2 S/cm, 3 x 10' 2 S/cm, 2 x 10' 2 S/cm, 1 x 10' 2 S/cm, 0.8 x 10' 2 S/cm, 0.5 x 10' 2 S/cm, or 0.2 x 10' 2 S/cm.
  • S/cm Siemens/centimeter
  • ligands can be coupled to the battery materials particles 218.
  • the ligands can minimize agglomeration between the battery material particles 218.
  • the ligands can stabilize the surface of the battery material particles 218.
  • the ligand can control morphology of the battery material particles 218.
  • water-soluble ligands can be used to control the morphology of the battery material particles 218.
  • the ligands can include polymeric ligands.
  • the polymeric ligands can include at least one of polyacrylic acid (PAA) or polyvinyl pyrrolidone (PVP).
  • PAA polyacrylic acid
  • PVP polyvinyl pyrrolidone
  • the ligands can include monomer units that include one or more carboxylic acids.
  • the one or more carboxylic acids can include hexanoic acid or oleic acid.
  • the ligands can include monomer units that include one or more alkanethiols.
  • the one or more alkanethiols can include hexanethiol or octanethiol.
  • the ligands can include monomer units that include one or more mercaptoalkanoic acids.
  • the ligands can include mercaptohexadecanoic acid.
  • the ligands can also include monomer units that include one or more phosphines.
  • the ligands can include trioctylphosphine oxide or phosphinic acid.
  • the ligands can include monomer units that include one or more amines.
  • the one or more amines can include amine-terminated polyethylene glycol.
  • the battery material particles 218 can be separated from the second phase 214 at operation 120.
  • the battery material particles 218 can be removed from the second phase 214 by rupturing the barriers of droplets of the second phase 214 within the microemulsion.
  • rupturing the barriers of the droplets of the second phase 214 can be temporary.
  • the barriers of the droplets of the second phase 214 can be broken by applying heat to the mixture of the first phase 212 and the second phase 214.
  • the battery material particles 218 can be removed from the droplets of the second phase 214 by adding an additional solvent to disrupt equilibrium of the microemulsion and cause the battery material particles 218 to precipitate out of the droplets of the second phase 214.
  • the one or more liquid/solid separation processes 222 can be performed to produce the battery material particles 218 and a residual liquid phase 224.
  • the battery material particles 218 can be removed from the droplets of the second phase 214 using one or more centrifugation processes.
  • the battery material particles 218 can be removed from the droplets of the second phase 214 using a filtration process.
  • the battery material particles 218 can be removed from the droplets of the second phase 214 by decanting the battery material particles 218 from the residual liquid phase 224 after the battery material particles 218 have settled in the reaction vessel 202. In one or more further illustrative examples, the battery material particles 218 can settle in the reaction vessel 202 and the residual liquid phase 224 can be decanted without breaking the droplets of the second phase 214. In these scenarios, the battery material particle separation at 220 may not be performed.
  • the residual liquid phase 224 can be stored in an additional vessel 126.
  • the residual liquid phase 224 can be separated into components that include at least one of the first solution 206, the second solution 208, and/or the one or more surfactants 210 and added to the reaction vessel 202 to implement one or more additional cycles of the process to form additional battery material particles. In this way, the residual liquid phase 224 can be recycled in one or more subsequent cycles of the process to form additional battery material particles.
  • the battery material particles 218 can be formed into a first layer 228 on a second layer examples, prior to being formed into the first layer 228, heat can be applied to the battery material particles 218 at temperatures from about 900 °C to 1000 °C to produce agglomerated battery material particles.
  • the agglomerated battery material particles have dimensions from about 1 pm to about 50 pm.
  • the battery material particles 218 can be used to form one or more cathode layers of the battery 232.
  • the battery material particles 218 can be used to form one or more anode layers of the battery 232.
  • the battery material particles 218 can be deposited on the second layer 230 using one or more liquid phase deposition techniques. In one or more additional illustrative 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 can include a current collector layer. In one or more scenarios, the battery 232 can include a lithium-ion battery.
  • the first solution 206 can include a first microemulsion and the second solution 206 can include a second microemulsion.
  • the first microemulsion and the second microemulsion can be combined in the reaction vessel to produce a mixture of microemulsions.
  • the mixture of microemulsions can include a first number of droplets that correspond to the first microemulsion and a second number of droplets that correspond to the second microemulsion.
  • the first number of droplets and the second number of droplets can be combined to cause reactions to take place between one or more first reagents included in the first number of droplets and one or more second reagents included in the second number of droplets to produce the battery material particles 218.
  • Example l is a process comprising: providing a first solution and a second solution in a reaction vessel, wherein: the first solution includes one or more first solvents and the second solution includes one or more second solvents, the one or more first solvents are immiscible in the one or more second solvents, and at least one of the first solution or the second solution including one or more reagents; combining the first solution and the second solution to produce a microemulsion that includes a first phase comprising the one or more first solvents and a second phase including a plurality of droplets comprising the one or more second solvents; causing the one or more reagents to produce battery material particles within the plurality of droplets, the battery material particles having at least one dimension no greater than one micrometer (pm); and removing the battery material particles from the plurality of droplets.
  • the first solution includes one or more first solvents and the second solution includes one or more second solvents, the one or more first solvents are immiscible in the one or more second solvents, and at least
  • Example 2 the subject matter of example 1, wherein the battery material particles are removed from the plurality of droplets by applying heat to the plurality of droplets.
  • Example 3 the subject matter of example 1 of 2, wherein the battery material particles are removed from the plurality of droplets by adding an additional solvent to disrupt equilibrium of the microemulsion and cause the battery material particles to precipitate out of the plurality of droplets.
  • Example 4 the subject matter of any one of examples 1-3, comprising: causing surfaces of the plurality of droplets to rupture to remove the battery material particles from the plurality of droplets.
  • Example 5 the subject matter of example 4, wherein the surfaces of the plurality of droplets are temporarily ruptured to remove the battery material particles from the plurality of droplets.
  • Example 6 the subject matter of any one of examples 1-3, wherein the battery material particles are removed from the plurality of droplets without rupturing surfaces of the plurality of droplets.
  • Example 7 the subject matter of any one of examples 1-6, comprising performing one or more separation processes to separate the battery material particles from a residual liquid phase, wherein the residual liquid phase includes the one or more first solvents and the one or more second solvents.
  • Example 8 the subject matter of example 7, wherein the residual liquid phase is produced during a first cycle of a battery material particle production process and the process comprises: recycling the residual liquid phase in a second cycle of a battery material particle production process.
  • Example 9 the subject matter of example 7 or 8, comprising: performing one or more centrifugation processes to separate the battery material particles from the residual liquid phase.
  • Example 10 the subject matter of any one of claims 7-9, comprising: performing one or more filtration processes to separate the battery material particles and the residual liquid phase.
  • Example 11 the subject matter of example 7, comprising: causing the battery material particles to settle in the reaction vessel; and performing one or more decanting processes to separate the battery material particles from the residual liquid phase.
  • Example 12 the subject matter of any one of examples 1-11, comprising: applying heat to the battery material particles at temperatures from about 900 °C to 1000 °C to produce agglomerated battery material particles.
  • Example 13 the subject matter of example 12, wherein the agglomerated battery material particles have dimensions from about 1 pm to about 50 pm.
  • Example 14 the subject matter of any one of examples 1-13, wherein at least one of the one or more first solvents or the one or more second solvents include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more glymes, one or more ethers, or one or more combinations thereof.
  • the one or more first solvents or the one or more second solvents include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane
  • Example 15 the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more lithium-containing components.
  • Example 16 the subject matter of example 15, wherein the one or more lithium- containing components include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof.
  • Example 17 the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more transition metal halides.
  • Example 18 the subject matter of example 17, wherein the one or more transition metal halides include at least one of FeCh or NiCh.
  • Example 19 the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more transition metal sulfates.
  • Example 20 the subject matter of example 19, wherein the one or more transition metal sulfates include at least one of FeSCU or NiSC
  • Example 21 the subject matter of any one of examples 1-20, wherein the one or more reagents include one or more basic compounds.
  • Example 22 the subject matter of example 21, wherein the one or more basic compounds include at least one of sodium hydroxide, ammonium hydroxide, or lithium hydroxide.
  • Example 23 the subject matter of any one of examples 1-20, wherein the one or more reagents include one or more acidic compounds.
  • Example 24 the subject matter of example 23, wherein the one or more acidic compounds include succinic acid, malonic acid, oxalic acid, glutaric acid, or adipic acid.
  • Example 25 the subject matter of any one of examples 1-24, wherein the battery material particles include one or more cathode active material precursors.
  • Example 27 the subject matter of example 26, wherein the dianionic radical includes CO3 or C2O4.
  • Example 28 the subject matter of example 26, wherein the combination of two monovalent anions include (OH)2 or OFE-vFv.
  • Example 29 the subject matter of example 26, wherein the cationic dopant includes Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.
  • Example 30 the subject matter of any one of examples 1-24, wherein the battery material particles include one or more lithium-containings.
  • Example 31 the subject matter of example 30, wherein the one or more lithium-containings include at least one of lithium succinate, lithium oxalate, lithium ketomal onate, 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 oxalate, lithium succinate, lithium dimethyl succinate, lithium fumarate, lithium 2-methylfumarate, maleic acid dilithium-containing, 2- methyl maleic acid dilithium-containing, 1,4-hydroquinone dilithium-containing, catechol dilithium-containing, lithium poly(hydroquinone), lithium (lS,2S)-cyclopentane-l,2- dicarboxylate, lithium (lS,2S)-cyclohexane-l,2-dicarboxylate, lithium malonate, hydrazine l,2-bis(trimethylsilyl
  • Example 32 the subject matter of any one of examples 1-24, wherein the battery material particles include one or more cathode active materials.
  • Example 33 the subject matter of example 32, wherein the one or more cathode active materials include one or more transition metal fluorides.
  • Example 35 the subject matter of example 34, wherein the cationic dopant includes Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.
  • Example 36 the subject matter of any one of examples 1-24, wherein the battery material particles include one or more anode active materials.
  • Example 37 the subject matter of example 36, wherein the one or more anode active materials include at least one of Li ⁇ isOn, LiNbsOs, or hydroxyamine hydrochloride.
  • Example 38 the subject matter of any one of examples 1-24, wherein the battery material particles include one or more anode active material precursors.
  • Example 39 the subject matter of example 38, wherein the one or more anode active material precursors include at least one of TiO2 or NbO x .
  • Example 40 the subject matter of any one of examples 1-39, wherein a coefficient of variation in an aspect ratio of the battery material particles is no greater than about 25%.
  • Example 41 the subject matter of any one of examples 1-40, wherein the battery material particles form nanospheres.
  • Example 42 the subject matter of example 41, wherein the nanospheres have an aspect ratio from about 1 to about 1.1.
  • Example 43 the subject matter of any one of examples 1-40, wherein the battery material particles form nanopellets.
  • Example 44 the subject matter of example 43, wherein the nanopellets have an aspect ratio from about 1.1 to about 3.
  • Example 45 the subject matter of any one of examples 1-40, wherein the battery material particles form nanorods.
  • Example 46 the subject matter of example 45, wherein the nanorods have an aspect ratio of at least about 3.
  • Example 47 the subject matter of any one of examples 1-46, wherein the battery material particles have an electrical conductivity of no greater than about 1 x 10' 2 Siemens/centimeter.
  • Example 48 the subject matter of any one of examples 1-47, wherein ligands are coupled to one or more surfaces of individual battery material particles.
  • Example 49 the subject matter of example 48, wherein the ligands include one or more polymeric materials.
  • Example 50 the subject matter of example 49, wherein the one or more polymeric materials include at least one of polyacrylic acid or polyvinyl pyrrolidone.
  • Example 51 the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more carboxylic acids.
  • Example 52 the subject matter of example 51, wherein the one or more carboxylic acids include at least one of hexanoic acid or oleic acid.
  • Example 53 the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more alkanethiols.
  • Example 54 the subject matter of example 53, wherein the one or more alkanethiols include at least one of hexanethiol or octanethiol.
  • Example 55 the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more mercaptoalkanoic acids.
  • Example 56 the subject matter of example 55, wherein the one or more mercaptoalkanoic acids include mercaptohexadecanoic acid.
  • Example 57 the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more phosphines.
  • Example 58 the subject matter of example 57, wherein the one or more phosphines include trioctylphosphine oxide or phosphinic acid.
  • Example 59 the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more amines.
  • Example 60 the subject matter of example 59, wherein the one or more polymeric materials include amine-terminated polyethylene glycol.
  • Example 61 the subject matter of any one of examples 1-60, comprising: combining the first solution and the second solution with one or more surfactants.
  • Example 62 the subject matter of example 61, wherein the one or more surfactants include one or more non-ionic surfactants.
  • Example 63 the subject matter of example 62, wherein the one or more nonionic surfactants include at least one of igepal, triton, brij, myij, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, or pluronic.
  • the one or more nonionic surfactants include at least one of igepal, triton, brij, myij, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, or pluronic.
  • Example 64 the subject matter of example 61, wherein the one or more surfactants include one or more anionic surfactants.
  • Example 65 the subject matter of example 64, wherein the one or more anionic surfactants includes at least one of AOT, SDS, SLS, SDBS, stearic acid, oleic acid, lauric acid, or sulphated castor oil.
  • the one or more anionic surfactants includes at least one of AOT, SDS, SLS, SDBS, stearic acid, oleic acid, lauric acid, or sulphated castor oil.
  • Example 66 the subject matter of example 61, wherein the one or more surfactants include one or more cationic surfactants.
  • Example 67 the subject matter of example 66, wherein the one or more cationic surfactants include at least one of CTAB, TMA, BTA, TMOA, HDTMA, or BDTA.
  • Example 68 the subject matter of example 61, wherein the one or more surfactants include one or more zwitterionic surfactants.
  • Example 69 the subject matter of example 68, wherein the one or more zwitterionic surfactants include at least one of cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB12, SB16, or lecithin.
  • the one or more zwitterionic surfactants include at least one of cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB12, SB16, or lecithin.
  • Example 70 the subject matter of example 61, wherein the one or more surfactants include a fluorinated molecule.
  • Example 71 the subject matter of example 70, wherein the fluorinated molecule includes a perfluoro polyether.
  • Example 72 the subject matter of example 61, wherein the one or more surfactants include a glycol.
  • Example 73 the subject matter of example 72, wherein the glycol includes a polyethylene glycol.
  • Example 74 the subject matter of example 61, wherein the one or more surfactants include one or more first surfactants and one or more co-surfactants.
  • Example 75 the subject matter of example 74, wherein the one or more first surfactants include at least one of a non-ionic surfactant, an anionic surfactant, a cationic surfactant, a zwitterionic surfactant, a surfactant including a fluorinated molecule, or a glycol.
  • the one or more co-surfactants include one or more alcohols.
  • Example 77 the subject matter of example 76, wherein the one or more alcohols include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, or sorbitol.
  • the one or more alcohols include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, or sorbitol.
  • Example 78 the subject matter of example 75, wherein the one or more cosurfactants include at least one of BZK or Stearin.
  • Example 79 is a method comprising: producing an aqueous solution including a co-solvent; adding a lithium-containing reagent to the aqueous solution to produce a lithium- containing aqueous solution; and causing precipitation of the lithium-containing aqueous solution to produce precipitate including particles comprised of a lithium-containing compound, the particles having at least one dimension less than 10 micrometers.
  • Example 80 the subject matter of example 79, wherein the co-solvent is an alcohol.
  • Example 81 the subject matter of example 80, wherein the alcohol is an unsubstituted alcohol having no greater than 4 carbon atoms or a substituted alcohol having an aliphatic chain of no greater than 4 carbon atoms and being substituted at one or more positions with a methyl group.
  • Example 82 the subject matter of example 80 or 81, wherein the alcohol is methanol or ethanol.
  • Example 83 the subject matter of any one of examples 79-82, wherein producing the aqueous solution includes adding an acid to an initial solution including water and the co-solvent.
  • Example 84 the subject matter of example 83, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
  • the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least
  • Example 85 the subject matter of example 83 or 84, wherein the acid is a carboxylic acid.
  • Example 86 the subject matter of example 85, wherein the carboxylic acid is a dicarboxylic acid.
  • Example 87 the subject matter of any one of examples 83-86, wherein the acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
  • Example 88 the subject matter of any one of examples 83-87, comprising: mixing the acid with the initial solution for a duration from about 3 minutes to about 8 minutes at temperatures from about 15 °C to about 60 °C.
  • Example 89 the subject matter of any one of examples 79-88, comprising: mixing the lithium-containing reagent with the aqueous solution for a duration from about 12 minutes to about 20 minutes at temperatures from about 15 °C to about 60 °C.
  • Example 90 the subject matter of any one of examples 79-89, comprising: performing a centrifugation process to separate the precipitate from supernatant.
  • Example 91 the subject matter of any one of examples 79-89, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
  • Example 92 the subject matter of any one of examples 79-91, comprising: performing a drying process of the precipitate.
  • Example 93 the subject matter of example 92, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours.
  • Example 94 the subject matter of any one of examples 79-85, wherein an amount of the lithium-containing reagent present in the aqueous solution is from about 1% by weight to about 10% by weight.
  • Example 95 the subject matter of any one of examples 83-88, wherein an amount the acid present in the aqueous solution is from about 5% by weight to about 15% by weight.
  • Example 96 the subject matter of any one of examples 79-95, wherein a ratio of an amount of water to an amount of the co-solvent present in the aqueous solution is from about 0.8 grams (g) to about 1.2 grams of water to about 0.8 grams to about 1.2 grams of the co-solvent.
  • Example 97 the subject matter of any one of examples 79-96, wherein an amount of water present in the aqueous solution is from about 30% by weight to about 50% by weight.
  • Example 98 the subject matter of any one of examples 79-97, wherein an amount of the co-solvent present in the aqueous solution is from about 30% by weight to about 50% by weight.
  • Example 99 the subj ect matter of any one of examples 79-98, wherein a yield of the lithium-containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
  • Example 100 the subject matter of any one of examples 79-99, comprising: prior to producing the aqueous solution, adding a carbon-based additive to a solution comprising water and the co-solvent.
  • Example 101 the subject matter of example 100, wherein the carbon-based additive is carbon black or carbon nanotubes.
  • Example 102 the subject matter of example 100 or 101, wherein a product of the precipitation is a matrix of the carbon-based additive with the lithium-containing compound being disposed in the matrix of the carbon-based additive.
  • Example 103 the subject matter of example 102, wherein the product includes from about 15% by weight to about 25% by weight of the carbon-based additive and from about 75% by weight to about 85% by weight of the lithium-containing compound.
  • Example 104 the subject matter of any one of examples 79-103, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm.
  • Example 105 the subject matter of any one of examples 79-104, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
  • Example 106 the subject matter of example 81, wherein the co-solvent is butanol.
  • Example 107 the subject matter of example 79 or 106, wherein the aqueous solution is produced by mixing water, the co-solvent, and a quaternary ammonium salt.
  • Example 108 the subject matter of example 107, wherein the quaternary ammonium salt includes Cetrimonium bromide, tetramethylammonium bromide, tetramethylammonium hydroxide, Hexadecyltrimethylammonium chloride, or b enzy 1 dim ethyl tetradecylammonium chi ori de .
  • Example 109 the subject matter of example 79 or 107, wherein producing the aqueous solution includes adding an amount of an acid to an initial solution comprising water and the co-solvent.
  • Example 110 the subject matter of example 109, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
  • the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one
  • Example 111 the subject matter of example 109 or 110, wherein the acid is a carboxylic acid.
  • Example 112 the subject matter of example 111, wherein the carboxylic acid is a dicarboxylic acid.
  • Example 113 the subject matter of example 112, wherein the carboxylic acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
  • Example 114 the subject matter of example 79 or any one of examples 105-
  • Example 115 the subject matter of example 79 or any one of examples 1 OS-
  • Example 116 the subject matter of example 79 or any one of examples 1 OS- 115, wherein adding the lithium-containing reagent to the aqueous solution produces an emulsion.
  • Example 117 the subject matter of any one of examples 105-116, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm.
  • Example 118 the subject matter of any one of examples 105-117, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
  • Example 119 the subject matter of any one of examples 105-118, comprising: performing a centrifugation process to separate the precipitate from supernatant.
  • Example 120 the subject matter of any one of examples 105-118, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
  • Example 121 the subject matter of any one of examples 105-120, comprising: performing a drying process of the precipitate.
  • Example 122 the subject matter of example 121, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours.
  • Example 123 the subject matter of any one of examples 105-122, wherein a yield of the particles comprised of the lithium-containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
  • Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of ethanol or methanol.
  • the volume ratio of water to ethanol or methanol was about 50% water to about 50% ethanol or methanol.
  • Oxalic acid was added to the initial solution and mixed for about 5 minutes to produce an intermediate solution.
  • Lithium hydroxide was added to the intermediate solution and mixed for about 15 minutes.
  • a centrifugation process was performed and followed by a drying process. The operations were performed at standard temperatures and pressures.
  • Lithium oxalate particles were produced having shapes of rods. The yield from the process was about 99.3%.
  • the lithium oxalate particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm.
  • Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of butanol and an amount of CTAB.
  • Oxalic acid was added to the initial solution and mixed for a suitable time to produce an intermediate solution that forms a microemulsion.
  • Lithium hydroxide was added to the intermediate solution and mixed for a suitable time.
  • Acetone was added to the resulting solution followed by a centrifugation process.
  • Three butanol washes were performed followed by a drying process. The operations were performed at standard temperatures and pressures. Lithium oxalate particles were produced having shapes of rods.
  • FIG 4 is a scanning electron microscope image 402 of lithium oxalate particles produced in this example and an x-ray diffraction analysis 404 of the lithium oxalate particles.
  • the lithium oxalate particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm.
  • Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of ethanol or methanol.
  • the volume ratio of water to ethanol or methanol was about 50% water to about 50% ethanol or methanol.
  • a carbon black additive was added to the initial solution and mixed for about 10 minutes.
  • Oxalic acid was then 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 and followed by a drying process. The operations were performed at standard temperatures and pressures.
  • Lithium oxalate particles were produced having shapes of rods. The yield from the process was about 95.4%.
  • the lithium-containing particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm and are disposed in a carbon black matrix.

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Abstract

Systems and methods of the present disclosure describe techniques for the synthesis of nanosized battery materials. The present disclosure provides, in one or more examples, one or more frameworks to precisely control the size and morphology of battery materials during synthesis using a microemulsion. The present disclosure also provides, in one or more examples, one or more frameworks to precisely control the size and morphology of battery materials during synthesis when a microemulsion is not formed.

Description

SYNTHESIS OF NANOSTRUCTURED BATTERY MATERIALS
CLAIM OF PRIORITY
[0001] This patent application claims the benefit of priority to U.S. Application Serial No. 63/514,721, filed July 20, 2023, which is incorporated by reference herein in its entirety.
FIELD OF THE DISCLOSURE
[0002] This application generally relates to compositions of battery materials and the methods of fabrication thereof.
BACKGROUND
[0003] The energy density of a lithium-ion battery is typically limited by the specific capacity of its cathode. High-Nickel stoichiometries of the state-of-the-art lithium-ion cathode material LiNixMnyCozO2, where x ranges from -0.4-0.95, have demonstrated sufficiently high cycle lifetime to warrant use in applications such as electric vehicles, but their specific capacity is still limited to a maximum of approximately 200 milliampere hours (mAh)/gram (g) at full state-of-charge. In contrast, the state-of-the-art anode active material, graphite, yields a much higher specific capacity of 350-372 mAh/g at full state-of-charge. As a result, increasing the specific capacity of the cathode generally provides the greatest relative improvement to the cell-level energy density of a lithium-ion battery.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] Figure 1 illustrates a process to produce battery material particles using one or more co-solvents in an aqueous solution to produce battery material particles, in accordance with one or more example implementations.
[0005] Figure 2 illustrates a framework to produce battery material particles using a microemulsion, in accordance with one or more example implementations.
DETAILED DESCRIPTION
[0006] Cathode materials such as LiNixMnyCozO2 can be charged to specific capacities greater than 200 mAh/g by increasing their voltage limit during charging but doing so drastically reduces their cycle lifetime. Failure at high voltage is primarily due to the mechanical stress and strain experienced by the cathode during repeated insertion and removal of lithium across a wide range of lithium mole fraction, which fatigues and eventually cracks cathode particles. The cathode materials, which are polycrystalline “secondary” particles composed of numerous primary crystallites, tend to fracture along the grain boundaries between primary crystallites during cycling. When this occurs, new cathode surfaces are exposed to electrolyte, allowing for more locations where high impedance decomposition products can accumulate, and from where transition metals can be leached out of the cathode crystal lattice, effectively destroying active material. Furthermore, cracked fragments of cathode material can become electrically disconnected from the remainder of the electrode matrix, thereby becoming inactive material. [0007] If the cumulative area of grain boundaries per mass of cathode active material can be reduced, such surface related degradation phenomena could be mitigated. One way to greatly reduce the proportion of grain boundaries in cathode active material is to increase the primary crystallite size, mainly through calcination at higher temperatures (i.e., >~950°C). Higher calcination temperature promotes larger grain growth, which then reduces the electrochemically available surface area in the event of secondary particle fracture.
[0008] However, increasing the calcination temperature when synthesizing cathode active materials via state-of-the-art co-precipitation processes has the deleterious side effect of causing excessive secondary particle agglomeration. This requires that the final synthesized secondary particles be ground and sieved in order to yield an acceptable particle size distribution, which adds an undesirable additional manufacturing step. Furthermore, ground secondary particles often require a second annealing step at slightly lower temperature than calcination in order to repair defects introduced during grinding, which is yet another undesirable additional manufacturing step.
[0009] Traditional co-precipitation processes for synthesizing cathode active material precursors can be easily optimized to yield desired particle sizes in the range of ~1 pm - 50 pm, with a median particle size of ~10 pm. The precursors, which are typically mixed metal hydroxides or carbonates, form primary crystallites that rapidly aggregate to form secondary particles in the range of 1-50 pm during their synthesis. If the temperature during the subsequent calcination process, which is needed to convert the active material precursors to their final oxide analogues, is kept below approximately 900°C, little agglomeration between secondary particles is observed and the desired particle size distribution is maintained. However, at calcination temperatures >950°C, the same mechanism that promotes grain growth of primary crystallites also promotes sintering between secondary particles, thereby resulting in particle agglomeration. [0010] A more precise control of secondary particle size at the precursor stage of synthesis would greatly assist in yielding a desired final particle size distribution, even at high calcination temperatures. If precursor secondary particles could be reproducibly synthesized to sizes substantially less than 1 pm, for example, with a narrow particle size distribution, a final calcination at 900 °C - 1000 °C could result in final secondary particle dimensions in the desired range of 1 pm -50 pm, thereby obviating any further need for grinding, milling, sieving or annealing. Therefore, a need exists for a new synthetic technique for uniformly fabricating primary particles for battery active materials with a particle size < 1 pm.
[0011] Besides the state-of-the-art lithium-ion cathode material LiNixMnyCozO2, there are numerous other battery materials whose performance is greatly improved by reducing their particle dimensions to the nanoscale. For example, the cathode material LiFePCU, whose specific power is limited by the relatively poor solid-state diffusivity of lithium through its crystal lattice, is observed to have substantially improved rate capability when its particle dimensions are reduced to < 1 pm. Other cathode materials with poor electronic conductivity, such as the conversion cathode FeFs, also demonstrate improved rate capability when their active material particle size is reduced to the nanoscale. In yet another example, the compound lithium ketomalonate, which is a typically inactive and highly resistive lithium-containing possessing a high specific capacity of > 400 mAh/g, can be rendered electrochemically active, with a reasonable oxidation potential of ~4 V vs. Li/Li+, when its constituent particles are nanosized. Finally, anode materials such as lithium titanate, which also suffers from poor electronic and ionic conductivity, are also observed to have greatly improved rate capability when their particle sizes are reduced to the nanoscale.
[0012] A useful feature of the co-precipitation process for battery material fabrication is that secondary particles typically do not grow to sizes substantially larger than 50 pm. The 1 pm - 50 pm secondary particle size provides good lithium intercalation kinetics for reasonably rate- capable materials such as LiNixMnyCozO2. Furthermore, the co-precipitation process tends to produce spherical particles, which also provides satisfactory tap density while minimizing active material surface area, thereby mitigating surface-related degradation phenomena.
[0013] However, though co-precipitation processes reproducibly yield particle sizes in the range of 1 pm - 50 pm, achieving particle sizes less than 1 pm, with a narrow size distribution and with similar electrochemical and morphological properties as compared to larger particles, is difficult. This is because the reaction conditions required to achieve the desired stoichiometry and morphology of co-precipitated cathode material precursors is strongly coupled to the resulting particle size. For example, for the precursor NixMnyCoz(OH)2, synthesis at high pH (i.e., >~11.5) results in smaller particles, but at the cost of irregular morphology and a wide size distribution. In contrast, synthesis at a more moderate pH of 10.5-11 yields smooth, spherical particles with narrow size distribution, but with much larger average particle size. Therefore, there is currently no way to decouple cathode precursor particle size control from size distribution and morphology using existing co-precipitation processes.
[0014] One way to limit cathode precursor size during synthesis is to limit reagent access to the surface of precursor nuclei through some form of particle confinement or surface protection. This approach is commonly exploited in the solution-phase synthesis of colloidal suspensions of nanoparticles, for instance, where nanoparticle surfaces can be stabilized through the addition of “ligands”. Ligands are typically short chain molecules possessing one end moiety which strongly coordinates to the nanoparticle surface after nucleation, and another end which strongly coordinates to solvent molecules and helps maintain particle suspension. The ligands form a capping shell around the nanoparticle, which prevents additional reagent from reacting with the particle surface, thereby limiting any further growth. Utilizing ligandbased particle confinement is particularly useful for creating fairly monodisperse nanoparticle dispersions with average size on the order of a few nanometers.
[0015] For synthesizing larger nanoparticles or microparticles in a confined manner, microemulsions provide another option. Microemulsions are dispersions of two immiscible solvents that are stabilized through the presence of surfactants. Microemulsions are typically characterized as oil-in-water (o/w) or water-in-oil (w/o) dispersions, though the concept can be generalized to various combinations of solvents that simply differ sufficiently in their polarity/miscibility. Microemulsions often appear to be macroscopically homogeneous, but in reality, they possess a fine dispersion of microscopic micelles comprising one phase within the other, where the small size of the micelles and their uniform distribution renders the overall mixture non-scattering and optically transparent. Microemulsions can be useful for the controlled synthesis of nanoparticles with uniform distribution and morphology, because the micelles within the emulsion provide “nanoreactors” within which size-confined synthesis can take place.
[0016] Microemulsions can be well suited for the synthesis of battery materials because they provide a means to uniformly control particle dimensions within the desired range of singledigit nanometers to several microns. The morphology and particle size of the battery materials can be precisely controlled by varying the compositions and relative amounts of the two immiscible phases, the primary surfactant and the co-surfactant, as well as by varying process parameters such as temperature and ambient pressure. [0017] Implementations herein are directed to producing battery material particles with one or more dimensions no greater than 1 micrometer without using a grinding process or other process to reduce the size of the particles formed by the processes and methods described herein. For example, microemulsions can be produced that can be used to produce battery material particles. The microemulsions can include a first phase comprised of a first solution and a second phase comprised of a second solution. In various examples, the second phase can include droplets that are dispersed throughout the first phase. The composition of the second solution can include precursors of battery material particles. In one or more examples, one or more reactions can take place with respect to the compounds included in the second solution to produce battery material particles within the droplets. The droplets can have dimensions that limit the size of battery material particles produced within the droplets. For example, the droplets can have dimensions that limit one or more dimensions of the battery material particles to less than 1 pm.
[0018] In one or more additional examples, a way to influence the particle size during precipitation of battery materials and battery material precursors from solution is to introduce additional co-solvents besides water into the reaction solution. In these implementations, battery material particles can also be produced having at least one dimension no greater than 1 pm without performing a grinding process or another process to reduce the size of the particles that have been formed using the methods and processes herein.
[0019] In one example, a 50:50 mixture by volume of water and methanol is used in place of 100% water for the synthesis of a battery material precursor such as Ni(0H)2. In such an example, the pH of the solution and precipitation of hydroxide can be controlled through the addition of ammonia. In another example, a lithium-containing compound such as lithium ketomalonate can be synthesized using a water: methanol solvent mixture. In this example, LiOH can first be added to a 50:50 mixture (by volume) of water and methanol. Once the hydroxide is dissolved, ketomalonic acid can be added to the reaction solution. As the product, lithium ketomalonate, is highly insoluble in the reaction solution, it will precipitate.
[0020] The use of multiple solvents in the reaction solution impacts precipitate particle size in many ways. For example, the solubility of the final product, such as a metal hydroxide or salt, will be substantially different, and often lower, in an organic solvent as compared to water. This is likely to promote faster nucleation, and as a result, smaller particle size. The addition of alternate solvents besides water also impacts the dielectric constant of the whole medium, which affects ion solvation and ion-pair interactions. This can also lead to higher local supersaturation and faster nucleation, further reducing particle size. [0021] Figure 1 illustrates a process 100 to produce battery material particles using one or more co-solvents in an aqueous solution to produce battery material particles, in accordance with one or more example implementations. The process 100 can be performed to produce battery material particles according to a number of techniques. For example, the process 100 can include operations of a microemulsion process that can be implemented to produce battery material particles. Additionally, the process 100 can include operations of a non-microemulsion process to produce battery material particles. Further, although some operations of the process 100 can generally be the same between the microemulsion process and the non-microemulsion process, the specific implementation of these operations can be different.
[0022] The process 100 can be performed in one or more reaction vessels with individual reaction vessels having a volume of 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 illustrative examples, the process 100 can be performed in one or more reaction vessels with individual reaction vessels having a volume from about 0.1 L to about 500 L, from about 1 L to about 400 L, from about 2 L to about 300 L, from about 5 L to about 200 L, from about 10 L to about 100 L, from about 0.1 L to about 1 L, from about 1 L to about 10 L, from about 10 L to about 50 L, from about 50 L to about 100 L, from about 100 L to about 150 L, from about 150 L to about 200 L, from about 200 L to about 250 L, from about 250 L to about 500 L, or from about 500 L to about 1000 L. In one or more examples, the one or more reaction vessels used to carry out the process 100 can include one or more mixing devices. The one or more mixing devices can include one or more agitation mixing devices. For example, the one or more mixing devices can include one or more rotating paddles. In one or more additional examples, the one or more mixing devices can include one or more jet mixing devices. In one or more further examples, the one or more mixing devices can include one or more hypersonic mixing devices. The one or more reaction vessels used to carry out the process 100 can also include and/or be coupled to one or more temperature control devices. The one or more temperature control devices can operate to at least one of heat or cool liquids within the one or more reaction vessels. The one or more temperature control devices can include at least one of one or more electric heating elements, one or more chemical heating elements, one or more flame-based heating elements, one or more heat exchangers, one or more refrigeration cooling elements, one or more fans, or one or more ventilation devices.
[0023] The process 100 can include, at 102, preparing an initial solution. The initial solution can include an aqueous solution and one or more co-solvents. For non-microemulsion implementations, the preparation of the initial solution can include operation 104. At 104, the process 100 can include combining water and one or more co-sol vents that can be soluble in water and can be soluble with respect to each other. In various examples, the one or more cosolvents can be soluble in water and with respect to each other at temperatures from about 15 °C to about 30 °C and at standard pressures of about 101 kilopascals (kPa). In one or more additional examples, the one or more co-solvents can be soluble in water and with respect to each other at temperatures greater than about 30 °C and at pressures greater than about 101 kPa.
[0024] In one or more examples, the one or more co-solvents can include one or more alcohols. For example, the one or more co-solvents can include one or more alcohols having a carbon chain with no greater than 10 carbon atoms, no greater than 9 carbon atoms, no greater than 8 carbon atoms, no greater than 7 carbon atoms, no greater than 6 carbon atoms, no greater than 5 carbon atoms, no greater than 4 carbon atoms, no greater than 3 carbon atoms, no greater than 2 carbon atoms, or no greater than 1 carbon atom. Additionally, the one or more cosolvents can include one or more alcohols having one or more rings with individual rings having no greater than 6 carbon atoms, no greater than 5 carbon atoms, or no greater than 4 carbon atoms. In one or more illustrative examples, the one or more co-solvents can include one or more alcohols having an aliphatic chain. In one or more additional illustrative examples, the one or more co-solvents can include one or more alcohols having a carbon chain with at least one alkenyl group. In one or more further illustrative examples, the one or more cosolvents can include one or more single bonded cyclic alcohols or one or more phenolic alcohols. In at least some illustrative examples, the one or more co-solvents can include one or more alcohols with unsubstituted carbon atoms. In still other examples, the one or more cosolvents can include one or more alcohols with one or more substituted carbon atoms. In situations where the one or more co-solvents include one or more alcohols with one or more substituted carbon atoms, the carbon atoms can be substituted with at least one of a methyl group, an amine group, a carboxylate group, or a nitro group. In various illustrative examples, the one or more co-solvents can include methanol. In one or more additional scenarios, the one or more co-solvents can include ethanol.
[0025] In one or more additional examples, water and the one or more co-solvents can be combined such that at least 40% by volume of the initial solution can be water, at least 45% by volume of the initial solution is can be water, at least 50% by volume of the initial solution can be water, at least 55% by volume of the initial solution can be water, a least 60% of the volume of the initial solution can be water, at least 65% of the volume of the initial solution can be water, or at least 70% of the volume of the initial solution can be water. In one or more illustrative examples, the initial solution can include from about 40% by volume water to about 75% by volume water, from about 50% by volume water to about 70% by volume water, from about 45% by volume water to about 55% by volume water, from about 50% by volume water to about 60% by volume water, from about 55% by volume water to about 65% by volume water, from about 60% by volume water to about 70% by volume water, or from about 65% by volume water to about 75% by volume water.
[0026] Further, at least 25% by volume of the initial solution can be one or more co-solvents, at least 30% by volume of the initial solution can be one or more co-solvents, at least 35% by volume of the initial solution can be co-solvents, at least 40% by volume of the initial solution can be one or more co-solvents, at least 45% by volume of the initial solution is can be one or more co-solvents, at least 50% by volume of the initial solution can be one or more co-solvents, or at least 55% by volume of the initial solution can be one or more co-solvents. In one or more additional illustrative examples, the initial solution can include from about 25% by volume of one or more co-sol vents to about 60% by volume of one or more co-sol vents, from about 30% by volume of one or more co-solvents to about 50% by volume of one or more co-solvents, from about 40% by volume of one or more co-solvents to about 50% by volume of one or more co-solvents, from about 45% by volume of one or more co-solvents to about 55% by volume of one or more co-solvents, or from about 50% by volume of one or more co-solvents to about 60% by volume of one or more co-solvents.
[0027] In one or more further examples, a volume ratio of the amount of the one or more cosolvents present in the initial solution in relation to the amount of water present in the initial solution can be from about 0.7: 1.3 to about 1.3:0.7, from about 0.8: 1.2 to about 1.2:0.8, from about 0.85: 1.15 to about 1.15:0.85, from about 1.1 : 0.9 to about 0.9: 1.1, from about 0.95: 1.05 to about 1.05:0.95. In still other examples, a volume ratio of the amount of the one or more cosolvents present in the aqueous solution in relation to the amount of water present in the aqueous solution can be about 1 : 1. In various illustrative examples, the initial solution can contain about 50% by volume water and about 50% by volume of one or more alcohols. The one or more alcohols can include methanol or ethanol.
[0028] Water and the one or more co-solvents can be combined at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C. The initial solution can also be prepared at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa. In one or more examples, the water and the one or more co-sol vents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 3 minutes, from about 2 minutes to about 4 minutes, or from about 3 minutes to about 5 minutes.
[0029] In scenarios where a microemulsion is produced by the process 100, the preparation of the initial solution can include, at 106, combining water with at least two immiscible reagents. In one or more examples, the at least two immiscible reagents can include one or more first reagents. The one or more first reagents can 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 glymes, or one or more ethers. In one or more illustrative examples, the one or more first reagents can include butanol.
[0030] The at least two immiscible reagents can also include one or more second reagents. The one or more second reagents can include one or more surfactants. The one or more surfactants can include one or more non-ionic surfactants. The one or more non-ionic surfactants can include igepal, triton, brij, myij, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, pluronic, or one or more combinations thereof. In one or more additional examples, the one or more surfactants can include one or more anionic surfactants. The one or more anionic surfactants can include sodium bis(2-ethylhexyl)sulfosuccinate (AOT), Sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), Sodium Dodecylbenzene Sulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulphated castor oil, or one or more combinations thereof. In one or more further examples, the one or more surfactants can include one or more cationic surfactants. The one or more cationic surfactants can include Cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), Hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or one or more combinations thereof. In still other examples, the one or more surfactants can include one or more zwitterionic surfactants. The one or more zwitterionic surfactants can include cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB 12, SB 16, lecithin, or one or more combinations thereof. In various examples, the one or more surfactants can include a fluorinated molecule. In one or more illustrative examples, the one or more surfactants can include a perfluoro polyether. In one or more additional illustrative examples, the one or more surfactants can include a glycol. To illustrate, the one or more surfactants can include a polyethylene glycol. In one or more illustrative examples, the one or more second reagents can include one or more quaternary ammonium salts. In various illustrative examples, the one or more second reagents can include Cetrimonium bromide.
[0031] The combination of water with one or more first reagents and the one or more second reagents can produce an initial solution that comprises a microemulsion. In one or more examples, an amount of at least one first reagent in the initial solution can be from about 10% by weight to about 50% by weight or from about 20% by weight to about 40% by weight, an amount of a second solvent can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight, and a remainder of the at least one additional first reagents or the one or more second reagents. In one or more additional examples, in implementations where the initial solution includes at least one or more surfactants and one or more solvents, where the one or more solvents can include water, the initial solution can include from about 10% by weight to about 80% by weight of the one or more solvents, from about 20% by weight to about 60% by weight of the one or more solvents, or from about 40% by weight to about 80% by weight of one or more solvents. The initial solution can also include from about 5% by weight to about 40% by weight of one or more surfactants, from about 10% by weight to about 30% by weight of one or more surfactants, or from about 5% by weight to about 25% by weight of one or more surfactants. In various examples, a remainder of the initial solution can include one or more additional reagents. In one or more further illustrative examples, the initial solution can include no greater than about 50% by weight water and no greater than about 20% by weight of one or more alcohols with a remainder of the mixture comprising one or more reagents, such as one or more surfactants.
[0032] Water and the immiscible reagents can be combined at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C. The initial solution can also be prepared at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa. In one or more examples, the water and the immiscible reagents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 3 minutes, from about 2 minutes to about 4 minutes, or from about 3 minutes to about 5 minutes. In one or more examples, the amounts of individual reagents included in initial solution can be based on the reagents used to produce the initial solution. For example, the amounts of individual reagents included in the initial solution can be based on solubility limits of one or more individual reagents with respect to one or more additional reagents of the initial solution. In at least some illustrative examples where the initial solution comprises water, amounts of one or more reagents included in the initial solution can be based on solubility limits of the one or more reagents in water.
[0033] At 108, the process 100 can include adding one or more reagents to the initial solution to produce an aqueous solution including one or more co-solvents. The one or more reagents added to the initial solution can include one or more acidic compounds. The one or more acidic compounds can include an unsubstituted acid having no greater than 6 carbon atoms. In one or more additional examples, the one or more acidic compounds can include a substituted carboxylic acid having an aliphatic chain of no greater than 6 carbon atoms. In one or more further examples, the one or more acidic compounds can include an unsubstituted carbon chain having at least one alkenyl group. In still other examples, the one or more acidic compounds can include an unsubstituted carbon chain having at least one alkenyl group. In scenarios where 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 with at least one alkenyl group, the chains can be substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, a hydroxide group, or a carboxyl group. In one or more illustrative examples, the one or more reagents added to the initial solution can include one or more carboxylic acids. In one or more further illustrative examples, the one or more reagents added to the initial solution can include one or more dicarboxylic acids. In one or more further illustrative examples, the one or more reagents added to the initial solution can include succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, citric acid, formic acid, or one or more combinations thereof.
[0034] In one or more examples, the one or more reagents can be added to the initial solution at 108 at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C. Additionally, the one or more reagents can be added to the initial solution at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa. Further, the one or more reagents can be mixed for a duration from about 15 seconds to about 30 minutes, from about 1 minute to about 20 minutes, from about 2 minutes to about 10 minutes, from about 30 seconds to about 5 minutes, from about 1 minute to about 4 minutes, from about 2 minutes to about 6 minutes, from about 3 minutes to about 8 minutes, or from about 4 minutes to about 10 minutes. [0035] The process 100 can include, at 110, producing a lithium-containing aqueous solution. In one or more examples, at 110, one or more lithium-containing compounds can be added to the aqueous produced at 108 to produce the lithium-containing aqueous solution. In various examples, the one or more lithium-containing compounds can include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof.
[0036] In at least some examples, the one or more lithium-containing compounds can be added to the aqueous solution, at 110, at temperatures from about 10 °C to about 60 °C, from about 15 °C to about 50 °C, from about 20 °C to about 40 °C, from about 15 °C to about 25 °C, from about 20 °C to about 30 °C, from about 25 °C to about 35 °C, or from about 30 °C to about 40 °C. Additionally, the one or more lithium-containing compounds can be added to the aqueous solution, at 110, at pressures from about 80 kPa to about 130 kPa, from about 90 kPa to about 120 kPa, or from about 100 kPa to about 110 kPa. Further, the one or more lithium-containing compounds and the aqueous solution can be mixed, at 110, for a duration from about 3 minutes to about 45 minutes, from about 5 minutes to about 30 minutes, from about 10 minutes to about 20 minutes, from about 5 minutes to about 10 minutes, from about 10 minutes to about 15 minutes, from about 15 minutes to about 20 minutes, from about 20 minutes to about 25 minutes, or from about 25 minutes to about 30 minutes.
[0037] Additionally, at 112, the process 100 can include causing precipitation of the lithium- containing aqueous solution to produce precipitate including lithium-containing particles. The precipitation process can form a precipitant that includes the lithium-containing particles and a supernatant that includes the residual liquid. In one or more illustrative examples, the lithium- containing particles can include a lithium-containing salt. The precipitation of the lithium- containing aqueous solution can include performing at least one of one or more mechanical process or one or more chemical processes. In one or more illustrative examples, for the nonmicroemulsion process, the precipitation of the lithium-containing aqueous solution can take place when the lithium-containing reagent from operation 110 is added to the aqueous solution and the lithium-containing reagent dissolves in the aqueous solution. Upon the lithium- containing reagent dissolving in the aqueous solution, the reaction that produces the lithium- containing compound can take place. In at least some examples, as the reaction to produce the lithium-containing compound is taking place, the lithium-containing compound can crystallize to produce the lithium-containing particles. In one or more examples, one or more alcohols present in the aqueous solution can cause the crystallization of the lithium-containing compound to form the lithium-containing particles. The lithium-containing reagent can dissolve in the aqueous solution with sufficient mixing at relatively low temperatures, such as no greater than 30 °C. The lithium-containing reagent can also dissolve in the aqueous solution with less mixing at relatively higher temperatures, such as temperatures of at least 30 °C.
[0038] In scenarios where the microemulsion process is being implemented, the precipitation of the lithium-containing solution can take place in response to one or more additional reagents being added to the lithium-containing aqueous solution. In one or more examples, the aqueous solution produced at 108 can include at least two phases. In at least some examples, the at least two phases can include an aqueous phase and a second phase including droplets that are disposed in the first phase. In various examples, the second phase can include droplets encased in a barrier. In one or more additional illustrative examples, the barrier can be comprised of surfactant molecules. The addition of the lithium-containing reagent to the aqueous solution at 110 can cause lithium-containing compounds to form within the droplets of the second phase. The disruption of the barriers of the second phase can cause the lithium-containing compounds formed within the second phase to precipitate out of the droplets. The barrier of the second phase can be disrupted through at least one of one or more physical processes or one or more chemical processes. In various examples, the barriers of the droplets can be disrupted using one or more mixing devices. Additionally, the barriers of the droplets can also be disrupted by heating the lithium-containing aqueous solution. Further, the barriers of the droplets can be broken by disrupting the equilibrium of the microemulsion by adding one or more additional reagents to the lithium-containing aqueous solution. To illustrate, adding a sufficient amount of acetone to the lithium-containing aqueous solution can cause the lithium-containing compounds to be released from the droplets. In at least some examples, at least a portion of the amount of additional reagent added to disrupt the equilibrium of the microemulsion can be recycled. For example, an amount of the additional reagent recovered from the barrier disruption process can be re-used in one or more other operations of the process 100 where appropriate. In various examples, lithium-containing particles can be formed within the droplets, while in other examples, lithium-containing particles can be formed when lithium- containing compounds formed in the droplets are released.
[0039] Further, at 114, the process 100 can include performing one or more separations processes. The one or more separation processes can separate the lithium-containing particles from residual liquid. The one or more separations processes can include centrifugation. In one or more additional examples, the one or more separations processes can include one or more filtration processes. In at least some examples, the one or more separations processes can include one or more vacuum filtration processes. [0040] At 116, the process 100 can include performing a drying process for the lithium - containing particles. The drying process can be performed at temperatures 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 illustrative examples, the drying process can take place at temperatures from about 50 °C to about 500 °C, from about 75 °C to about 300 °C, from about 100 °C to about 250 °C, from about 50 °C to about 250 °C, from about 100 °C to about 300 °C, from about 300 °C to about 500 °C, from about 100 °C to about 200 °C, from about 150 °C to about 250 °C, from about 200 °C to about 300 °C, or from about 250 °C to about 350 °C. Further, the drying process can take place for a duration 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 additional illustrative examples, the drying process can be performed for durations from about 15 minutes to about 12 hours, from about 30 minutes to about 6 hours, from about 30 minutes to about 2 hours, from about 1 hour to about 3 hours, from about 2 hours to about 4 hours, from about 3 hours to about 5 hours, or from about 4 hours to about 6 hours.
[0041] In implementations where a microemulsion has been used to produce the lithium- containing particles, the process 100 can include, at 118, performing one or more washes between the one or more separations process performed at 114 and the drying process performed at 116. In one or more examples, the one or more washes can be performed with one or more reagents that comprise the initial solution. For example, the one or more washes can be performed using one or more alcohols present in the initial solution. In one or more illustrative examples, the one or more washes can be performed using butanol. In at least some examples, an amount of the reagent used to perform the one or more washes can be recycled and re-used in subsequent washing operations. To illustrate, performing the one or more alcohol washes at 118 can include performing a first butanol wash, a second butanol wash, and a third butanol wash. In these scenarios, butanol recovered from the first butanol wash can be used in the second butanol wash and butanol recovered from at least one of the first butanol wash or the second butanol wash can be used in the third butanol wash.
[0042] The lithium-containing particles can have a number of shapes. For example, the lithium-containing particles can be shaped as spheres, pellets, or rods. In one or more examples, the lithium-containing particles can have a coefficient of variation in the aspect ratio of the lithium-containing particles that can be no greater than 1%, no greater than 5%, no greater than 10%, no greater than 15%, no greater than 20%, no greater than 25%, or no greater than 30%. The coefficient of variation can correspond to a ratio of a standard deviation of a size distribution of the lithium-containing particles with respect to a mean of the size distribution of the lithium-containing particles.
[0043] In scenarios where the lithium-containing particles are spheres, the spheres can have an aspect ratio of about 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more illustrative examples, the spheres can have an aspect ratio from about 0.9 to about 1.25, from about 0.95 to about 1.15, or from about 1 to 1.1. In situations where the lithium-containing particles are pellets, the pellets can have an aspect ratio 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 one or more additional illustrative examples, the pellets can have an aspect ratio from about 0.9 to about 1.4, from about 1 to about 1.3, from about 1.1 to about 1.2, from about 1 to about 1.2, or from about 0.9 to about 1.2. In still other instances where the lithium-containing particles comprise rods, the rods can have an aspect ratio 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.
[0044] In one or more examples, the lithium-containing particles can have one or more dimensions no greater than 5 micrometers (pm), no greater than 2 pm, no greater than 1 pm, no greater than 0.8 pm, no greater than 0.6 pm, no greater than 0.4 pm, no greater than 0.2 pm, no greater than 0.1 pm, or no greater than 0.05 pm. In one or more illustrative examples, the battery material particles can have dimensions from about 0.05 pm to about 5 pm, from about 0.1 pm to about 1 pm, from about 0.3 pm to about 3 pm, from about 0.5 pm to about 2 pm, or from about 0.05 pm to about 0.8 pm. In one or more illustrative examples, the lithium- containing particles can be in the form of rods having a diameter from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 5 pm.
[0045] In various examples, a yield of the process 100 can be at least 80%, at least 85%, at least 90%, at least 95%, or at least 99%. In one or more illustrative examples, the yield can be from about 80% to about 99.9%, from about 85% to about 99.5%, from about 90% to about 99%, from about 90% to about 99.9%, or from about 95% to about 99.9%. The yield can be calculated based on a weight of the lithium-containing particles produced in relation to an amount of the lithium-containing reagent used in the process 100 at 110.
[0046] In at least some examples of the non-microemulsion implementations of the process 100, a conductive additive can be added to the initial solution. The conductive additive can include a carbon-containing material. In one or more illustrative examples, the carbon-based additive can include carbon black or carbon nanotubes. In implementations where the conductive additive is part of the non-microemulsion process, reaction conditions for at least one of operations 102, 108, 110, or 112 can increase. In one or more examples, the product produced by the process 100 when a conductive additive is used in the non-microemulsion implementations can include lithium-containing particles disposed on a matrix of the conductive additive.
[0047] In various examples, the lithium-containing compound particles can be used in the production of lithium ion batteries. For example, the lithium-containing compound particles can be included in anodes of lithium ion batteries. In one or more examples, the lithium- containing compound particles can comprise active materials of anodes of lithium ion batteries. [0048] Although the process 100 has been described with respect to the production of lithium- containing particles. The process 100 can also be implemented to produce particles having a different composition. For example, the process 100 can be implemented to produce nickel hydroxide particles. To illustrate, rather than producing a lithium-containing solution at operation 110, a nickel-containing compound can be added to the aqueous solution to produce a nickel-containing solution. In one or more examples, the nickel-containing compound can 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 the nickel hydroxide.
[0049] Figure 2 illustrates a framework 200 to produce battery material particles using a microemulsion, in accordance with one or more example implementations. In at least some examples, the framework 200 can implement one or more of the operations performed with respect to the microemulsion implementations of the process 100 described in relation to Figure 1. Additionally, at least some of the operations performed in relation to the framework 200 can correspond to one or more operations performed with respect to the microemulsion implementations of the process 100 described in relation to Figure 1. Further, 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 of the microemulsion implementations of the process 100 described in relation to Figure 1.
[0050] The framework can include a reaction vessel 202. The reaction vessel 202 can have a volume, such as 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 can include one or more mixing devices 204. The one or more mixing devices 204 can include one or more agitation mixing devices. For example, the one or more mixing devices 204 can include one or more rotating paddles. In one or more additional examples, the one or more mixing devices 204 can include one or more jet mixing devices. In one or more further examples, the one or more mixing devices 204 can include one or more hypersonic mixing devices.
[0051] A first solution 206 can be added to the reaction vessel 202. The first solution 206 can include one or more first solvents. In one or more examples, the one or more first solvents can include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more glymes, one or more ethers, or one or more combinations thereof. A second solution 208 can also be added to the reaction vessel 202. In various examples, the second solution 208 can include one or more second solvents. In one or more examples, the one or more solvents included in the second solution 208 can be selected such that the second solution 208 and the first solution 206 are immiscible.
[0052] At least one of the one or more solutions 206, 208 can include one or more reagents. In various examples, the one or more reagents can be dissolved in the one or more solutions 206, 208. In implementations where at least one of the first solution 206 or the second solution 208 comprise multiple solvents, an amount of a first solvent can be from about 10% by weight to about 50% by weight or from about 20% by weight to about 40% by weight, an amount of a second solvent can be from about 5% by weight to about 30% by weight or from about 10% by weight to about 20% by weight, and a remainder of the at least one of the first solution or the second solution can include one or more reagents. In one or more additional examples, in implementations where the first solution 206 and the second solution 208 are combined with one or more surfactants 210 to form a mixture, the mixture can include from about 10% by weight to about 80% by weight, from about 20% by weight to about 60% by weight, or from about 40% by weight to about 80% by weight of one or more solvents, from about 5% by weight to about 40% by weight, from about 10% by weight to about 30% by weight, or from about 5% by weight to about 25% by weight of one or more surfactants 210, and a remainder of the mixture can include one or more reagents. In one or more further illustrative examples, a mixture including the first solution 206 and the second solution 208 can include no greater than about 50% by weight water and no greater than about 20% by weight of one or more alcohols with a remainder of the mixture comprising one or more reagents. In one or more examples, the amounts of individual reagents included in at least one of the first solution 206 or the second solution 208 can be based on the composition of the first solution 206 and/or the composition of the second solution 208. For example, the amounts of individual reagents included in at least one of the first solution or the second solution 208 can be based on 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 illustrative examples where at least one of the first solution 206 or the second solution 208 comprise water, amounts of one or more reagents included in at least one of the first solution 206 or the second solution 208 can be based on solubility limits of the one or more reagents in water.
[0053] Combining the first solution 206, the second solution 208, and, optionally, one or more surfactants 210 can produce a first phase 212 and a second phase 214. In one or more illustrative examples, the first phase 212 can comprise the first solution 206 and, in at least some instances, one or more additional liquids, such as one or more surfactants 210. Additionally, the second phase 214 can include droplets that comprise at least the second phase 214. In various examples, the second phase 214 can include droplets of the second solution 208 encased in a barrier. In one or more additional illustrative examples, the barrier can be comprised of surfactant molecules.
[0054] In one or more scenarios, the first phase 212 and the second phase 214 can comprise a microemulsion. To illustrate, the first solution 206, the second solution 208, and optionally the one or more surfactants 210, can be combined under temperature and pressure conditions that cause a microemulsion to be formed within the reaction vessel 202 that includes the first phase 212 and the second phase 214. In one or more illustrative examples, the first solution 206, the second solution 208, and, optionally the one or more surfactants 210, can be combined at temperatures from about 10 °C to about 100 °C, from about 20 °C to about 90 °C, from about 30 °C to about 80 °C, from about 20 °C to about 50 °C, or from about 25 °C to about 75 °C to produce a microemulsion within the reaction vessel 202. Additionally, the first solution 206, the second solution 208, and optionally the one or more surfactants 210, can be combined at pressures from about 90 kilopascals (kPa) to about 120 kPa or from about 95 kPa to about 105 kPa produce a microemulsion within the reaction vessel 202. In situations where supercritical CO2 is a solvent included in at least one of the first solution 206 or the second solution 208, a microemulsion can be formed at temperatures and pressures that cause CO2 to behave as a supercritical fluid. To illustrate, in situations where supercritical CO2 is a solvent included in at least one of the first solution 206 or the second solution 208, a microemulsion can be formed at temperatures of at least about 30 °C and pressures of at least about 7 megapascals (MPa).
[0055] In one or more examples, the one or more reagents can include one or more lithium- containing components. For example, the one or more reagents can include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof. In addition, the one or more reagents can include one or more transition metal halides. To illustrate, the one or more reagents can include at least one of FeCh, NiCh. Further, the one or more reagents can include one or more transition metal sulfates. In one or more illustrative examples, the one or more reagents can include at least one of FeSCU or NiSCU. In one or more additional examples, the one or more reagents can include one or more basic compounds. In one or more additional illustrative examples, the one or more reagents can include sodium hydroxide, ammonium hydroxide, lithium hydroxide, or one or more combinations thereof. The one or more reagents can also include one or more organic acids. In one or more further illustrative examples, the one or more reagents can include succinic acid, malonic acid, oxalic acid, glutaric acid, adipic acid, or one or more combinations thereof.
[0056] The one or more surfactants can include one or more non-ionic surfactants. The one or more non-ionic surfactants can include igepal, triton, brij, myrj, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, pluronic, or one or more combinations thereof. In one or more additional examples, the one or more surfactants can include one or more anionic surfactants. The one or more anionic surfactants can include sodium bis(2- ethylhexyl)sulfosuccinate (AOT), Sodium dodecyl sulfate (SDS), sodium laureth sulfate (SLS), Sodium Dodecylbenzene Sulfonate (SDBS), stearic acid, oleic acid, lauric acid, sulphated castor oil, or one or more combinations thereof. In one or more further examples, the one or more surfactants can include one or more cationic surfactants. The one or more cationic surfactants can include Cetrimonium bromide (CTAB), tetramethylammonium (TMA), benzotriazole (BTA), trimethylamine-N-oxide (TMOA), Hexadecyltrimethylammonium (HDTMA), benzyldimethyltetradecylammonium (BDTA), or one or more combinations thereof. In still other examples, the one or more surfactants can include one or more zwitterionic surfactants. The one or more zwitterionic surfactants can include cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB12, SB16, lecithin, or one or more combinations thereof. In various examples, the one or more surfactants can include a fluorinated molecule. In one or more illustrative examples, the one or more surfactants can include a perfluoro polyether. In one or more additional illustrative examples, the one or more surfactants can include a glycol. To illustrate, the one or more surfactants can include a polyethylene glycol.
[0057] In at least some examples, the one or more surfactants 210 can include one or more cosurfactants. In one or more examples, the one or more surfactants 210 can include a first surfactant and a co-surfactant. In various examples, the first surfactant can include at least one of a non-ionic surfactant, an anionic surfactant, a cationic surfactant, a zwitterionic surfactant, a surfactant including a fluorinated molecule, or a glycol. Additionally, the one or more cosurfactants can include one or more alcohols. For example, the one or more co-surfactants can include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, sorbitol, or one or more combinations thereof. In various examples, the one or more co-surfactants can include at least one of Benzalkonium Chloride (BZK) or Stearin.
[0058] In various examples, the first solution 206 and the second solution 208 and, optionally the one or more surfactants 210 can be combined in the reaction vessel 202 at reaction conditions 216 to cause the one or more reagents to participate in one or more reactions that produce battery material particles 218. In one or more examples, the reaction conditions 216 can include effective temperatures, pressures, and amounts of reagents to produce the battery material particles 218. In one or more illustrative examples, reagents included in the first solution 206 and the second solution 208 can be combined at the reaction conditions 216 to cause precipitation of the battery material particles 218. In one or more illustrative examples, one or more reagents included in the first phase 212 can migrate into the second phase 214 and react with one or more additional reagents included in the second phase to produce the battery material particles 218. In one or more additional illustrative examples, the reaction conditions 216 can include temperatures from 10 °C to about 100 °C and pressures from about 90 kPa to about 120 kPa.
[0059] The battery material particles 218 can include one or more cathode active material precursors. For example, the battery material particles 218 can include FePCU, NiPCU, CoPO4, FexMnyPO4, CoX, NiX, MnX, NkMnyCozX„ Ni.vCoyA-X, NiwCoxMnyAzX where w + x + y + z =1. In one or more examples, X can include a dianionic radical. In one or more illustrative examples, the dianionic radical can include CO3 or C2O4. In one or more additional examples, X can include two monovalent anions. To illustrate, the two monovalent anions can include (OH)2 or OH2-VF. Additionally, A can include one or more cationic dopants. In one or more additional illustrative examples, the one or more cationic dopants can include Al, Mg, Ti, Zr, Cr, Ru, Mo, V, or one or more combinations thereof.
[0060] The battery material particles 218 can also include one or more lithium-containings. For example, the battery material particles 218 can 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 hydroxyl amine, lithium oxalate, lithium succinate, lithium dimethyl succinate, lithium fumarate, lithium 2-methylfumarate, maleic acid dilithium- containing, 2-m ethyl maleic acid dilithium-containing, 1,4-hydroquinone dilithium - containing, catechol dilithium-containing, lithium poly(hydroquinone), lithium (1S,2S)- cyclopentane-l,2-dicarboxylate, lithium (lS,2S)-cyclohexane-l,2-dicarboxylate, lithium mal onate, hydrazine l,2-bis(trimethyl silyl) dilithium-containing, pyromellitic diimide lithium- containing, naphthalenediimide lithium-containing, lithium cyanurate, or one or more combinations thereof.
[0061] Additionally, the battery material particles 218 can include one or more cathode active materials. The one or more cathode active materials can include one or more transition metal fluorides. In various examples, the one or more transition metal fluorides can include FeFs, CuF2, C0F3, NiF2, MnF2, or LiFePC , LiMnAFe1PO4. LiNiAMn1Co-O2, LiNiACo1AAO2, LiNillCoAMn1AAO2, where w + x + y + z =l. In various examples, A can include one or more cationic dopants. In one or more illustrative examples, the one or more cationic dopants can include at least one of Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.
[0062] Further, the battery material particles 218 can include one or more anode active materials. In one or more illustrative examples, the one or more anode active materials can include at least one of Li^isOn, LiNbsOs, or hydroxyamine hydrochloride.
[0063] In still other examples, the battery material particles 218 can include one or more anode active material precursors. In one or more examples, the one or more anode active material precursors can include at least one of TiO2 or NbCh.
[0064] The battery material particles 218 can have various characteristics. For example, the battery material particles 218 can have a coefficient of variation in the aspect ratio of the battery material particles 218 that can be no greater than 1%, no greater than 5%, no greater than 10%, no greater than 15%, no greater than 20%, no greater than 25%, or no greater than 30%. The coefficient of variation can correspond to a ratio of a standard deviation of a size distribution of the battery material particles with respect to a mean of the size distribution of the battery material particles.
[0065] Additionally, the battery material particles 218 can include nanospheres. The nanospheres can have an aspect ratio of about 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2, or 1.25. In one or more illustrative examples, the nanospheres can have an aspect ratio from about 0.9 to about 1.25, from about 0.95 to about 1.15, or from about 1 to 1.1. In one or more further examples, the battery material particles 218 can include nanopellets. The nanopellets can have an aspect ratio 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 one or more additional illustrative examples, the nanopellets can have an aspect ratio from about 0.9 to about 1.4, from about 1 to about 1.3, from about 1.1 to about 1.2, from about 1 to about 1.2, or from about 0.9 to about 1.2. Further, the battery material particles 218 can include nanorods. The nanorods can have an aspect ratio 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. [0066] In one or more examples, the battery material particles 218 can have one or more dimensions no greater than 5 micrometers (pm), no greater than 2 pm, no greater than 1 pm, no greater than 0.8 pm, no greater than 0.6 pm, no greater than 0.4 pm, no greater than 0.2 pm, no greater than 0.1 pm, or no greater than 0.05 pm. In one or more illustrative examples, the battery material particles can have dimensions from about 0.05 pm to about 5 pm, from about 0.1 pm to about 1 pm, from about 0.3 pm to about 3 pm, from about 0.5 pm to about 2 pm, or from about 0.05 pm to about 0.8 pm.
[0067] In at least some examples, the battery material particles 218 can have electrical conductivity of no greater than 9 x 10'2 Siemens/centimeter (S/cm), no greater than 8 x 10'2 S/cm, 7 x 10'2 S/cm, 6 x 10'2 S/cm, 5 x 10'2 S/cm, 4 x 10'2 S/cm, 3 x 10'2 S/cm, 2 x 10'2 S/cm, 1 x 10'2 S/cm, 0.8 x 10'2 S/cm, 0.5 x 10'2 S/cm, or 0.2 x 10'2 S/cm.
[0068] In still other examples, ligands can be coupled to the battery materials particles 218. In one or more examples, the ligands can minimize agglomeration between the battery material particles 218. For example, the ligands can stabilize the surface of the battery material particles 218. In one or more additional examples, the ligand can control morphology of the battery material particles 218. To illustrate, water-soluble ligands can be used to control the morphology of the battery material particles 218.
[0069] In one or more examples, the ligands can include polymeric ligands. In one or more illustrative examples, the polymeric ligands can include at least one of polyacrylic acid (PAA) or polyvinyl pyrrolidone (PVP). In one or more additional examples, the ligands can include monomer units that include one or more carboxylic acids. In one or more additional illustrative examples, the one or more carboxylic acids can include hexanoic acid or oleic acid. In one or more further examples, the ligands can include monomer units that include one or more alkanethiols. In one or more further illustrative examples, the one or more alkanethiols can include hexanethiol or octanethiol. In still other examples, the ligands can include monomer units that include one or more mercaptoalkanoic acids. For example, the ligands can include mercaptohexadecanoic acid. The ligands can also include monomer units that include one or more phosphines. To illustrate, the ligands can include trioctylphosphine oxide or phosphinic acid. In various examples, the ligands can include monomer units that include one or more amines. In at least some examples, the one or more amines can include amine-terminated polyethylene glycol. [0070] After formation of the battery material particles 218 within the second phase 214, the battery material particles 218 can be separated from the second phase 214 at operation 120. In one or more examples, the battery material particles 218 can be removed from the second phase 214 by rupturing the barriers of droplets of the second phase 214 within the microemulsion. In at least some examples, rupturing the barriers of the droplets of the second phase 214 can be temporary. In various examples, the barriers of the droplets of the second phase 214 can be broken by applying heat to the mixture of the first phase 212 and the second phase 214. In one or more 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 equilibrium of the microemulsion and cause the battery material particles 218 to precipitate out of the droplets of the second phase 214.
[0071] Subsequent to removal of the battery material particles 218 from the second phase 214, the one or more liquid/solid separation processes 222 can be performed to produce the battery material particles 218 and a residual liquid phase 224. In one or more illustrative examples, the battery material particles 218 can be removed from the droplets of the second phase 214 using one or more centrifugation processes. In one or more additional illustrative examples, the battery material particles 218 can be removed from the droplets of the second phase 214 using a filtration process. In one or more further illustrative examples, the battery material particles 218 can be removed from the droplets of the second phase 214 by decanting the battery material particles 218 from the residual liquid phase 224 after the battery material particles 218 have settled in the reaction vessel 202. In one or more further illustrative examples, the battery material particles 218 can settle in the reaction vessel 202 and the residual liquid phase 224 can be decanted without breaking the droplets of the second phase 214. In these scenarios, the battery material particle separation at 220 may not be performed.
[0072] In various examples, the residual liquid phase 224 can be stored in an additional vessel 126. In at least some examples, the residual liquid phase 224 can be separated into components that include at least one of the first solution 206, the second solution 208, and/or the one or more surfactants 210 and added to the reaction vessel 202 to implement one or more additional cycles of the process to form additional battery material particles. In this way, the residual liquid phase 224 can be recycled in one or more subsequent cycles of the process to form additional battery material particles.
[0073] The battery material particles 218 can be formed into a first layer 228 on a second layer
Figure imgf000025_0001
examples, prior to being formed into the first layer 228, heat can be applied to the battery material particles 218 at temperatures from about 900 °C to 1000 °C to produce agglomerated battery material particles. In one or more illustrative examples, the agglomerated battery material particles have dimensions from about 1 pm to about 50 pm. In one or more additional examples, the battery material particles 218 can be used to form one or more cathode layers of the battery 232. In one or more further examples, 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 one or more additional illustrative 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 can include a current collector layer. In one or more scenarios, the battery 232 can include a lithium-ion battery.
[0074] In one or more additional examples, the first solution 206 can include a first microemulsion and the second solution 206 can include a second microemulsion. In this way, the first microemulsion and the second microemulsion can be combined in the reaction vessel to produce a mixture of microemulsions. In various examples, the mixture of microemulsions can include a first number of droplets that correspond to the first microemulsion and a second number of droplets that correspond to the second microemulsion. In one or more illustrative examples, the first number of droplets and the second number of droplets can be combined to cause reactions to take place between one or more first reagents included in the first number of droplets and one or more second reagents included in the second number of droplets to produce the battery material particles 218.
[0075] In view of the above-described implementations of subject matter this application discloses the following list of examples, wherein one feature of an example in isolation or more than one feature of an example, taken in combination and, optionally, in combination with one or more features of one or more further examples are further examples also falling within the disclosure of this application.
[0076] Example l is a process comprising: providing a first solution and a second solution in a reaction vessel, wherein: the first solution includes one or more first solvents and the second solution includes one or more second solvents, the one or more first solvents are immiscible in the one or more second solvents, and at least one of the first solution or the second solution including one or more reagents; combining the first solution and the second solution to produce a microemulsion that includes a first phase comprising the one or more first solvents and a second phase including a plurality of droplets comprising the one or more second solvents; causing the one or more reagents to produce battery material particles within the plurality of droplets, the battery material particles having at least one dimension no greater than one micrometer (pm); and removing the battery material particles from the plurality of droplets.
[0077] In Example 2, the subject matter of example 1, wherein the battery material particles are removed from the plurality of droplets by applying heat to the plurality of droplets.
[0078] In Example 3, the subject matter of example 1 of 2, wherein the battery material particles are removed from the plurality of droplets by adding an additional solvent to disrupt equilibrium of the microemulsion and cause the battery material particles to precipitate out of the plurality of droplets.
[0079] In Example 4, the subject matter of any one of examples 1-3, comprising: causing surfaces of the plurality of droplets to rupture to remove the battery material particles from the plurality of droplets.
[0080] In Example 5, the subject matter of example 4, wherein the surfaces of the plurality of droplets are temporarily ruptured to remove the battery material particles from the plurality of droplets.
[0081] In Example 6, the subject matter of any one of examples 1-3, wherein the battery material particles are removed from the plurality of droplets without rupturing surfaces of the plurality of droplets.
[0082] In Example 7, the subject matter of any one of examples 1-6, comprising performing one or more separation processes to separate the battery material particles from a residual liquid phase, wherein the residual liquid phase includes the one or more first solvents and the one or more second solvents.
[0083] In Example 8, the subject matter of example 7, wherein the residual liquid phase is produced during a first cycle of a battery material particle production process and the process comprises: recycling the residual liquid phase in a second cycle of a battery material particle production process.
[0084] In Example 9, the subject matter of example 7 or 8, comprising: performing one or more centrifugation processes to separate the battery material particles from the residual liquid phase. [0085] In Example 10, the subject matter of any one of claims 7-9, comprising: performing one or more filtration processes to separate the battery material particles and the residual liquid phase.
[0086] In Example 11, the subject matter of example 7, comprising: causing the battery material particles to settle in the reaction vessel; and performing one or more decanting processes to separate the battery material particles from the residual liquid phase. [0087] In Example 12, the subject matter of any one of examples 1-11, comprising: applying heat to the battery material particles at temperatures from about 900 °C to 1000 °C to produce agglomerated battery material particles.
[0088] In Example 13, the subject matter of example 12, wherein the agglomerated battery material particles have dimensions from about 1 pm to about 50 pm.
[0089] In Example 14, the subject matter of any one of examples 1-13, wherein at least one of the one or more first solvents or the one or more second solvents include water, isopropanol, ethanol, butanol, pentanol, hexanol, heptanol, octanol, dimethyl sulfoxide, cyclohexane, isooctane, heptane, octane, nonane, decane, supercritical CO2, one or more glymes, one or more ethers, or one or more combinations thereof.
[0090] In Example 15, the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more lithium-containing components.
[0091] In Example 16, the subject matter of example 15, wherein the one or more lithium- containing components include lithium hydroxide, lithium nitrate, lithium oxalate, lithium fluorosulfonimide, or one or more combinations thereof.
[0092] In Example 17, the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more transition metal halides.
[0093] In Example 18, the subject matter of example 17, wherein the one or more transition metal halides include at least one of FeCh or NiCh.
[0094] In Example 19, the subject matter of any one of examples 1-14, wherein the one or more reagents include one or more transition metal sulfates.
[0095] In Example 20, the subject matter of example 19, wherein the one or more transition metal sulfates include at least one of FeSCU or NiSC
[0096] In Example 21, the subject matter of any one of examples 1-20, wherein the one or more reagents include one or more basic compounds.
[0097] In Example 22, the subject matter of example 21, wherein the one or more basic compounds include at least one of sodium hydroxide, ammonium hydroxide, or lithium hydroxide.
[0098] In Example 23, the subject matter of any one of examples 1-20, wherein the one or more reagents include one or more acidic compounds.
[0099] In Example 24, the subject matter of example 23, wherein the one or more acidic compounds include succinic acid, malonic acid, oxalic acid, glutaric acid, or adipic acid.
[00100] In Example 25, the subject matter of any one of examples 1-24, wherein the battery material particles include one or more cathode active material precursors. [00101] In Example 26, the subject matter of example 25, wherein the one or more cathode active material precursors include at least one of FePC , NiPCU, CoPO4, FexMnyPCU, CoX, NiX, MnX, NixMny _,_,CozX,, NixCoyAzX, NiwCoxMnyAzX where w + x + y + z =1, wherein X represents either a dianionic radical or a combination of two monovalent anions and A represents a cationic dopant.
[00102] In Example 27, the subject matter of example 26, wherein the dianionic radical includes CO3 or C2O4.
[00103] In Example 28, the subject matter of example 26, wherein the combination of two monovalent anions include (OH)2 or OFE-vFv.
[00104] In Example 29, the subject matter of example 26, wherein the cationic dopant includes Al, Mg, Ti, Zr, Cr, Ru, Mo, or V.
[00105] In Example 30, the subject matter of any one of examples 1-24, wherein the battery material particles include one or more lithium-containings.
[00106] In Example 31, the subject matter of example 30, wherein the one or more lithium-containings include at least one of lithium succinate, lithium oxalate, lithium ketomal onate, 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 oxalate, lithium succinate, lithium dimethyl succinate, lithium fumarate, lithium 2-methylfumarate, maleic acid dilithium-containing, 2- methyl maleic acid dilithium-containing, 1,4-hydroquinone dilithium-containing, catechol dilithium-containing, lithium poly(hydroquinone), lithium (lS,2S)-cyclopentane-l,2- dicarboxylate, lithium (lS,2S)-cyclohexane-l,2-dicarboxylate, lithium malonate, hydrazine l,2-bis(trimethylsilyl) dilithium-containing, pyromellitic diimide lithium-containing, naphthalenediimide lithium-containing, or lithium cyanurate.
[00107] In Example 32, the subject matter of any one of examples 1-24, wherein the battery material particles include one or more cathode active materials.
[00108] In Example 33, the subject matter of example 32, wherein the one or more cathode active materials include one or more transition metal fluorides.
[00109] In Example 34, the subject matter of example 33, wherein the one or more transition metal fluorides include at least one of FeFs, CuF2, C0F3, N1F2, MnF2, LiFePCU, LiMnxFeyPO4, LiNixMny _,-CozO2, LiNixCoyAzO2, LiNiwCoxMnyAzO2, where w + x + y + z = l and A represents a cationic dopant.
[00110] In Example 35, the subject matter of example 34, wherein the cationic dopant includes Al, Mg, Ti, Zr, Cr, Ru, Mo, or V. [00111] In Example 36, the subject matter of any one of examples 1-24, wherein the battery material particles include one or more anode active materials.
[00112] In Example 37, the subject matter of example 36, wherein the one or more anode active materials include at least one of Li^isOn, LiNbsOs, or hydroxyamine hydrochloride.
[00113] In Example 38, the subject matter of any one of examples 1-24, wherein the battery material particles include one or more anode active material precursors.
[00114] In Example 39, the subject matter of example 38, wherein the one or more anode active material precursors include at least one of TiO2 or NbOx.
[00115] In Example 40, the subject matter of any one of examples 1-39, wherein a coefficient of variation in an aspect ratio of the battery material particles is no greater than about 25%.
[00116] In Example 41, the subject matter of any one of examples 1-40, wherein the battery material particles form nanospheres.
[00117] In Example 42, the subject matter of example 41, wherein the nanospheres have an aspect ratio from about 1 to about 1.1.
[00118] In Example 43, the subject matter of any one of examples 1-40, wherein the battery material particles form nanopellets.
[00119] In Example 44, the subject matter of example 43, wherein the nanopellets have an aspect ratio from about 1.1 to about 3.
[00120] In Example 45, the subject matter of any one of examples 1-40, wherein the battery material particles form nanorods.
[00121] In Example 46, the subject matter of example 45, wherein the nanorods have an aspect ratio of at least about 3.
[00122] In Example 47, the subject matter of any one of examples 1-46, wherein the battery material particles have an electrical conductivity of no greater than about 1 x 10'2 Siemens/centimeter.
[00123] In Example 48, the subject matter of any one of examples 1-47, wherein ligands are coupled to one or more surfaces of individual battery material particles.
[00124] In Example 49, the subject matter of example 48, wherein the ligands include one or more polymeric materials.
[00125] In Example 50, the subject matter of example 49, wherein the one or more polymeric materials include at least one of polyacrylic acid or polyvinyl pyrrolidone.
[00126] In Example 51, the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more carboxylic acids. [00127] In Example 52, the subject matter of example 51, wherein the one or more carboxylic acids include at least one of hexanoic acid or oleic acid.
[00128] In Example 53, the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more alkanethiols.
[00129] In Example 54, the subject matter of example 53, wherein the one or more alkanethiols include at least one of hexanethiol or octanethiol.
[00130] In Example 55, the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more mercaptoalkanoic acids.
[00131] In Example 56, the subject matter of example 55, wherein the one or more mercaptoalkanoic acids include mercaptohexadecanoic acid.
[00132] In Example 57, the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more phosphines.
[00133] In Example 58, the subject matter of example 57, wherein the one or more phosphines include trioctylphosphine oxide or phosphinic acid.
[00134] In Example 59, the subject matter of example 49, wherein the one or more polymeric materials include monomer units having one or more amines.
[00135] In Example 60, the subject matter of example 59, wherein the one or more polymeric materials include amine-terminated polyethylene glycol.
[00136] In Example 61, the subject matter of any one of examples 1-60, comprising: combining the first solution and the second solution with one or more surfactants.
[00137] In Example 62, the subject matter of example 61, wherein the one or more surfactants include one or more non-ionic surfactants.
[00138] In Example 63, the subject matter of example 62, wherein the one or more nonionic surfactants include at least one of igepal, triton, brij, myij, np80, np95, tergitol, decyl glucoside, lauryl glucoside, sucrose laurate, Tween85, or pluronic.
[00139] In Example 64, the subject matter of example 61, wherein the one or more surfactants include one or more anionic surfactants.
[00140] In Example 65, the subject matter of example 64, wherein the one or more anionic surfactants includes at least one of AOT, SDS, SLS, SDBS, stearic acid, oleic acid, lauric acid, or sulphated castor oil.
[00141] In Example 66, the subject matter of example 61, wherein the one or more surfactants include one or more cationic surfactants.
[00142] In Example 67, the subject matter of example 66, wherein the one or more cationic surfactants include at least one of CTAB, TMA, BTA, TMOA, HDTMA, or BDTA. [00143] In Example 68, the subject matter of example 61, wherein the one or more surfactants include one or more zwitterionic surfactants.
[00144] In Example 69, the subject matter of example 68, wherein the one or more zwitterionic surfactants include at least one of cocamidopropyl betaine, dimethyllaurylamine n-oxide, myristamine oxide, SB12, SB16, or lecithin.
[00145] In Example 70, the subject matter of example 61, wherein the one or more surfactants include a fluorinated molecule.
[00146] In Example 71, the subject matter of example 70, wherein the fluorinated molecule includes a perfluoro polyether.
[00147] In Example 72, the subject matter of example 61, wherein the one or more surfactants include a glycol.
[00148] In Example 73, the subject matter of example 72, wherein the glycol includes a polyethylene glycol.
[00149] In Example 74, the subject matter of example 61, wherein the one or more surfactants include one or more first surfactants and one or more co-surfactants.
[00150] In Example 75, the subject matter of example 74, wherein the one or more first surfactants include at least one of a non-ionic surfactant, an anionic surfactant, a cationic surfactant, a zwitterionic surfactant, a surfactant including a fluorinated molecule, or a glycol. [00151] In Example 76, the subject matter of example 74 or 75, wherein the one or more co-surfactants include one or more alcohols.
[00152] In Example 77, the subject matter of example 76, wherein the one or more alcohols include isoamyl alcohol, hexanol, dodecanol, glycerin butanol, glycerol, or sorbitol.
[00153] In Example 78, the subject matter of example 75, wherein the one or more cosurfactants include at least one of BZK or Stearin.
[00154] Example 79 is a method comprising: producing an aqueous solution including a co-solvent; adding a lithium-containing reagent to the aqueous solution to produce a lithium- containing aqueous solution; and causing precipitation of the lithium-containing aqueous solution to produce precipitate including particles comprised of a lithium-containing compound, the particles having at least one dimension less than 10 micrometers.
[00155] In Example 80, the subject matter of example 79, wherein the co-solvent is an alcohol.
[00156] In Example 81, the subject matter of example 80, wherein the alcohol is an unsubstituted alcohol having no greater than 4 carbon atoms or a substituted alcohol having an aliphatic chain of no greater than 4 carbon atoms and being substituted at one or more positions with a methyl group.
[00157] In Example 82, the subject matter of example 80 or 81, wherein the alcohol is methanol or ethanol.
[00158] In Example 83, the subject matter of any one of examples 79-82, wherein producing the aqueous solution includes adding an acid to an initial solution including water and the co-solvent.
[00159] In Example 84, the subject matter of example 83, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
[00160] In Example 85, the subject matter of example 83 or 84, wherein the acid is a carboxylic acid.
[00161] In Example 86, the subject matter of example 85, wherein the carboxylic acid is a dicarboxylic acid.
[00162] In Example 87, the subject matter of any one of examples 83-86, wherein the acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
[00163] In Example 88, the subject matter of any one of examples 83-87, comprising: mixing the acid with the initial solution for a duration from about 3 minutes to about 8 minutes at temperatures from about 15 °C to about 60 °C.
[00164] In Example 89, the subject matter of any one of examples 79-88, comprising: mixing the lithium-containing reagent with the aqueous solution for a duration from about 12 minutes to about 20 minutes at temperatures from about 15 °C to about 60 °C.
[00165] In Example 90, the subject matter of any one of examples 79-89, comprising: performing a centrifugation process to separate the precipitate from supernatant.
[00166] In Example 91, the subject matter of any one of examples 79-89, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
[00167] In Example 92, the subject matter of any one of examples 79-91, comprising: performing a drying process of the precipitate.
[00168] In Example 93, the subject matter of example 92, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours. [00169] In Example 94, the subject matter of any one of examples 79-85, wherein an amount of the lithium-containing reagent present in the aqueous solution is from about 1% by weight to about 10% by weight.
[00170] In Example 95, the subject matter of any one of examples 83-88, wherein an amount the acid present in the aqueous solution is from about 5% by weight to about 15% by weight.
[00171] In Example 96, the subject matter of any one of examples 79-95, wherein a ratio of an amount of water to an amount of the co-solvent present in the aqueous solution is from about 0.8 grams (g) to about 1.2 grams of water to about 0.8 grams to about 1.2 grams of the co-solvent.
[00172] In Example 97, the subject matter of any one of examples 79-96, wherein an amount of water present in the aqueous solution is from about 30% by weight to about 50% by weight.
[00173] In Example 98, the subject matter of any one of examples 79-97, wherein an amount of the co-solvent present in the aqueous solution is from about 30% by weight to about 50% by weight.
[00174] In Example 99, the subj ect matter of any one of examples 79-98, wherein a yield of the lithium-containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
[00175] In Example 100, the subject matter of any one of examples 79-99, comprising: prior to producing the aqueous solution, adding a carbon-based additive to a solution comprising water and the co-solvent.
[00176] In Example 101, the subject matter of example 100, wherein the carbon-based additive is carbon black or carbon nanotubes.
[00177] In Example 102, the subject matter of example 100 or 101, wherein a product of the precipitation is a matrix of the carbon-based additive with the lithium-containing compound being disposed in the matrix of the carbon-based additive.
[00178] In Example 103, the subject matter of example 102, wherein the product includes from about 15% by weight to about 25% by weight of the carbon-based additive and from about 75% by weight to about 85% by weight of the lithium-containing compound.
[00179] In Example 104, the subject matter of any one of examples 79-103, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm. [00180] In Example 105, the subject matter of any one of examples 79-104, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
[00181] In Example 106, the subject matter of example 81, wherein the co-solvent is butanol.
[00182] In Example 107, the subject matter of example 79 or 106, wherein the aqueous solution is produced by mixing water, the co-solvent, and a quaternary ammonium salt.
[00183] In Example 108, the subject matter of example 107, wherein the quaternary ammonium salt includes Cetrimonium bromide, tetramethylammonium bromide, tetramethylammonium hydroxide, Hexadecyltrimethylammonium chloride, or b enzy 1 dim ethyl tetradecylammonium chi ori de .
[00184] In Example 109, the subject matter of example 79 or 107, wherein producing the aqueous solution includes adding an amount of an acid to an initial solution comprising water and the co-solvent.
[00185] In Example 110, the subject matter of example 109, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
[00186] In Example 111, the subject matter of example 109 or 110, wherein the acid is a carboxylic acid.
[00187] In Example 112, the subject matter of example 111, wherein the carboxylic acid is a dicarboxylic acid.
[00188] In Example 113, the subject matter of example 112, wherein the carboxylic acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
[00189] In Example 114, the subject matter of example 79 or any one of examples 105-
113, comprising: adding an amount of acetone to the lithium-containing aqueous solution to cause precipitation of the particles comprised of the lithium-containing compound.
[00190] In Example 115, the subject matter of example 79 or any one of examples 1 OS-
114, comprising: performing one or more washes of the precipitate using additional amounts of the co-solvent. [00191] In Example 116, the subject matter of example 79 or any one of examples 1 OS- 115, wherein adding the lithium-containing reagent to the aqueous solution produces an emulsion.
[00192] In Example 117, the subject matter of any one of examples 105-116, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm.
[00193] In Example 118, the subject matter of any one of examples 105-117, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
[00194] In Example 119, the subject matter of any one of examples 105-118, comprising: performing a centrifugation process to separate the precipitate from supernatant.
[00195] In Example 120, the subject matter of any one of examples 105-118, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
[00196] In Example 121, the subject matter of any one of examples 105-120, comprising: performing a drying process of the precipitate.
[00197] In Example 122, the subject matter of example 121, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours.
[00198] In Example 123, the subject matter of any one of examples 105-122, wherein a yield of the particles comprised of the lithium-containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
EXPERIMENTAL EXAMPLES
Example 1
[00199] Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of ethanol or methanol. The volume ratio of water to ethanol or methanol was about 50% water to about 50% ethanol or methanol. Oxalic acid was added to the initial solution and mixed for about 5 minutes to produce an intermediate solution. Lithium hydroxide was added to the intermediate solution and mixed for about 15 minutes. A centrifugation process was performed and followed by a drying process. The operations were performed at standard temperatures and pressures. Lithium oxalate particles were produced having shapes of rods. The yield from the process was about 99.3%. In particular, the lithium oxalate particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm.
Figure imgf000037_0001
[00200] Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of butanol and an amount of CTAB. Oxalic acid was added to the initial solution and mixed for a suitable time to produce an intermediate solution that forms a microemulsion. Lithium hydroxide was added to the intermediate solution and mixed for a suitable time. Acetone was added to the resulting solution followed by a centrifugation process. Three butanol washes were performed followed by a drying process. The operations were performed at standard temperatures and pressures. Lithium oxalate particles were produced having shapes of rods. Figure 4 is a scanning electron microscope image 402 of lithium oxalate particles produced in this example and an x-ray diffraction analysis 404 of the lithium oxalate particles. In particular, the lithium oxalate particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm.
Example 3
[00201] Battery material particles were produced using a process that formed an initial solution having an amount of water and an amount of ethanol or methanol. The volume ratio of water to ethanol or methanol was about 50% water to about 50% ethanol or methanol. A carbon black additive was added to the initial solution and mixed for about 10 minutes. Oxalic acid was then 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 and followed by a drying process. The operations were performed at standard temperatures and pressures. Lithium oxalate particles were produced having shapes of rods. The yield from the process was about 95.4%. In particular, the lithium-containing particles are comprised of lithium oxalate nanorods having a diameter of about 0.3 pm and a length of about 2 pm and are disposed in a carbon black matrix.

Claims

CLAIMS What is claimed is:
1. A method comprising: producing an aqueous solution including a co-solvent; adding a lithium-containing reagent to the aqueous solution to produce a lithium- containing aqueous solution; and causing precipitation of the lithium-containing aqueous solution to produce precipitate including particles comprised of a lithium-containing compound, the particles having at least one dimension less than 10 micrometers.
2. The method of claim 1, wherein the co-solvent is an alcohol.
3. The method of claim 2, wherein the alcohol is an unsubstituted alcohol having no greater than 4 carbon atoms or a substituted alcohol having an aliphatic chain of no greater than 4 carbon atoms and being substituted at one or more positions with a methyl group.
4. The method of claim 2, wherein the alcohol is methanol or ethanol.
5. The method of claim 1, wherein producing the aqueous solution includes adding an acid to an initial solution including water and the co-solvent.
6. The method of claim 5, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
7. The method of claim 5, wherein the acid is a carboxylic acid.
8. The method of claim 7, wherein the carboxylic acid is a dicarboxylic acid.
9. The method of claim 5, wherein the acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
10. The method of claim 5, comprising: mixing the acid with the initial solution for a duration from about 3 minutes to about 8 minutes at temperatures from about 15 °C to about 60 °C.
11. The method of claim 1, comprising: mixing the lithium-containing reagent with the aqueous solution for a duration from about 12 minutes to about 20 minutes at temperatures from about 15 °C to about 60 °C.
12. The method of claim 1, comprising: performing a centrifugation process to separate the precipitate from supernatant.
13. The method of claim 1, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
14. The method of claim 1, comprising: performing a drying process of the precipitate.
15. The method of claim 14, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours.
16. The method of claim 1, wherein an amount of the lithium-containing reagent present in the aqueous solution is from about 1% by weight to about 10% by weight.
17. The method of claim 5, wherein an amount the acid present in the aqueous solution is from about 5% by weight to about 15% by weight.
18. The method of claim 1, wherein a ratio of an amount of water to an amount of the co-solvent present in the aqueous solution is from about 0.8 milliliters (mL) to about 1.2 mL of water to about 0.8 mL to about 1.2 mL of the co-solvent.
19. The method of claim 1, wherein an amount of water present in the aqueous solution is from about 30% by weight to about 50% by weight.
20. The method of claim 1, wherein an amount of the co-solvent present in the aqueous solution is from about 30% by weight to about 50% by weight.
21. The method of claim 1, wherein a yield of the lithium-containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
22. The method of claim 1, comprising: prior to producing the aqueous solution, adding a carbon-based additive to a solution comprising water and the co-solvent.
23. The method of claim 22, wherein the carbon-based additive is carbon black or carbon nanotubes.
24. The method of claim 22, wherein a product of the precipitation is a matrix of the carbon-based additive with the lithium-containing compound being disposed in the matrix of the carbon-based additive.
25. The method of claim 24, wherein the product includes from about 15% by weight to about 25% by weight of the carbon-based additive and from about 75% by weight to about 85% by weight of the lithium-containing compound.
26. The method of claim 1, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm.
27. The method of claim 1, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
28. The method of claim 3, wherein the co-solvent is butanol.
29. The method of claim 1, wherein the aqueous solution is produced by mixing water, the co-solvent, and a quaternary ammonium salt.
30. The method of claim 29, wherein the quaternary ammonium salt includes Cetrimonium bromide, tetramethylammonium bromide, tetramethylammonium hydroxide, Hexadecyltrimethylammonium chloride, or benzyldimethyltetradecylammonium chloride.
31. The method of claim 29, wherein producing the aqueous solution includes adding an amount of an acid to an initial solution comprising water and the co-solvent.
32. The method of claim 31, wherein the acid is an unsubstituted acid having no greater than 6 carbon atoms or a substituted carboxylic acid having (i) an aliphatic chain of no greater than 6 carbon atoms or (ii) a carbon chain having at least one alkenyl group, wherein the aliphatic chain or the carbon chain having at least one alkenyl group are optionally substituted at one or more positions with at least one of a methyl group, an ethyl group, a propyl group, an hydroxide group, or a carboxyl group.
33. The method of claim 31, wherein the acid is a carboxylic acid.
34. The method of claim 33, wherein the carboxylic acid is a dicarboxylic acid.
35. The method of claim 34, wherein the carboxylic acid is oxalic acid, malonic acid, citric acid, succinic acid, citric acid, or formic acid.
36. The method of claim 29, comprising: adding an amount of acetone to the lithium-containing aqueous solution to cause precipitation of the particles comprised of the lithium-containing compound.
37. The method of claim 29, comprising: performing one or more washes of the precipitate using additional amounts of the cosolvent.
38. The method of claim 29, wherein adding the lithium-containing reagent to the aqueous solution produces an emulsion.
39. The method of claim 29, wherein the particles comprised of the lithium-containing compound are shaped as rods having a width from about 0.1 pm to about 0.8 pm and a length from about 1 pm to about 3 pm.
40. The method of claim 29, wherein the particles comprised of the lithium-containing compound have an aspect ratio from about 2 to 8.
41. The method of claim 29, comprising: performing a centrifugation process to separate the precipitate from supernatant.
42. The method of claim 29, comprising: performing a vacuum filtration process to separate the precipitate from supernatant.
43. The method of claim 29, comprising: performing a drying process of the precipitate.
44. The method of claim 43, wherein the drying process includes heating the precipitate at temperatures from about 75 °C to about 300 °C for a duration from about 1 hour to about 3 hours.
45. The method of claim 29, wherein a yield of the particles comprised of the lithium- containing compound in relation to an amount of the lithium-containing reagent present in the aqueous solution is from about 85% to about 99%.
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