WO2022047585A1 - Alternative one-pot process for making cam precursor using metal feedstocks - Google Patents
Alternative one-pot process for making cam precursor using metal feedstocks Download PDFInfo
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- WO2022047585A1 WO2022047585A1 PCT/CA2021/051216 CA2021051216W WO2022047585A1 WO 2022047585 A1 WO2022047585 A1 WO 2022047585A1 CA 2021051216 W CA2021051216 W CA 2021051216W WO 2022047585 A1 WO2022047585 A1 WO 2022047585A1
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- lithium ion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/54—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [Mn2O4]-, e.g. Li(NixMn2-x)O4, Li(MyNixMn2-x-y)O4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention is related to an improved method of forming fine and ultrafine powders and nanopowders of cathode active materials (CAM) for batteries.
- CAM cathode active materials
- the present invention is related to, but not limited to, lithium ion battery cathodes and an efficient method of preparing the CAMs with a minimal waste of material and a reduction in the number of process steps some of which are detrimental to sintering and calcining.
- Lithium ion batteries comprising a lithium metal oxide cathode as the CAM, are highly advantageous as a suitable battery for most applications and they have found favor across the spectrum of applications. Still, there is a desire for an improvement in, particularly, the storage capability, recharge time, cost and storage stability of lithium ion batteries.
- the preparation of lithium ion batteries comprising lithium and transition metal based cathodes in a rock-salt crystalline form are described in U.S. Pat. Nos.
- Cathode materials having a rock-salt crystalline form have general formula :
- Cathode materials having the spinel crystalline structure have general formula:
- the CAM either rock-salt or spinel, is formed by the digestion of metal carbonates in oxalic acid with Li2COs to make a mixed oxalate precursor.
- the mixed oxalate precursor is then calcined to make the CAM.
- the supply chain for transition metal carbonates is not well established since the supply chain is primarily based on the formation of metal sulfates.
- Metal carbonates are typically made from metal sulfates.
- Metal sulfates are very low in metal content, 21 wt% for nickel for example, and therefore the cost associated with formation of metal carbonates from metal sulfates significantly mitigates the cost efficiencies associated with the oxalate process discussed above.
- the transition metals are extracted from the original source, often purified as metals, and then redissolved as acids. Therefore, the formation of metal carbonates, from metal sulfates, creates a Na2SO4 waste stream and the purity would typically be insufficient for use in the formation of CAMs for battery production unless additional, expensive, purification steps are utilized.
- the present invention is related to improvements in the formation of precursors for CAM which eliminates the necessity of forming the metal sulfate and therefore eliminates the need of converting the metal sulfate to metal carbonate which streamlines the metal precursor production.
- a particular advantage of the instant invention is in the ability to form high nickel CAMs wherein the precursor materials have been particularly difficult to obtain at a cost and purity level suitable for the formation of high nickel CAMs.
- An embodiment of the invention is provided in a method of forming a lithium ion cathode material.
- the method comprises reacting elemental metal with a multicarboxylic acid to form an oxide precursor and heating the oxide precursor to form the lithium ion cathode material.
- the elemental mixture comprises at least two of Ni, Mn, Co and Al.
- An embodiment of the invention is provided in a method of forming a lithium ion cathode material comprising: reacting element nickel with nitric acid to form nickel nitrate; reacting the nickel nitrate with a multi-carboxylic acid to form an oxide precursor; and heating the oxide precursor to form the lithium ion cathode material.
- Fig. 1 is an XRD scan of control and inventive examples.
- Fig. 2 is a graphical illustration of half cell data for a control and inventive sample.
- Fig. 3 is an XRD scan of control and inventive examples.
- Fig. 4 is an XRD scan of control and inventive examples.
- Figs. 5 and 6 are graphical illustrations of half cell data for a control and inventive sample.
- Fig. 7 is an XRD scan of control and inventive examples.
- Fig. 8 is a graphical illustration of half cell data for a control and inventive sample.
- the instant invention is specific to an improved method for preparing a lithium ion battery, and particularly the CAM of a lithium ion battery. More particularly, the present invention is specific to an improved process for forming cathodes for use in a lithium ion battery wherein the cathode is in a spinel crystalline form or a rock-salt form with preferred rock salt forms being NMC and NCA materials. Even more specifically, the present invention is directed to the formation of metal salt precursors, from elemental metal, directly without the requirement for the formation of sulfates and carbonates.
- the CAM of the instant invention comprises a lithium metal compound in a spinel crystal structure defined by the Formula I:
- the spinel crystal structure of Formula I has 0.5 ⁇ x ⁇ 0.6; 1 .4 ⁇ y ⁇ 1 .5 and z ⁇ 0.9. More preferably 0.5 ⁇ x ⁇ 0.55, 1 .45 ⁇ y ⁇ 1 .5 and z ⁇ 0.05. In a preferred embodiment neither x nor y is zero.
- the Mn/Ni ratio is no more than 3, preferably at least 2.33 to less than 3 and most preferably at least 2.6 to less than 3.
- the rock-salt crystal structure of Formula II is a high nickel NMC wherein 0.5 ⁇ a ⁇ 0.9 and more preferably 0.58 ⁇ a ⁇ 0.62 as represented by NMC 622 or 0.78 ⁇ a ⁇ 0.82 as represented by NMC 811.
- the term NMCxxx is a shorthand notation used in the art to represent the nominal relative ratio of nickel, manganese and cobalt.
- NMC811 for example, represents LiNio.8Mno.1Xo.1O2.
- the lithium is defined stoichiometrically to balance charge with the understanding that the lithium is mobile between the anode and cathode. Therefore, at any given time the cathode may be relatively lithium rich or relatively lithium depleted. In a lithium depleted cathode the lithium will be below stoichiometric balance and upon discharging the lithium may be above stoichiometric balance.
- the metals are represented in charge balance with the understanding that the metal may be slightly rich or slightly depleted, as determined by elemental analysis, due to the inability to formulate a perfectly balanced stoichiometry in practice.
- Dopants can be added to enhance the properties of the oxide such as electronic conductivity and stability.
- the dopant is preferably a substitutional dopant added in concert with the primary nickel, manganese and optional cobalt or aluminum.
- the dopant preferably represents no more than 10 mole% and preferably no more than 5 mole % of the oxide.
- Preferred dopants include Al, Gd, Ti, Zr, Mg, Ca, Sr, Ba, Mg, Or, Cu, Fe, Zn, V, Bi, Nb and B with Al and Gd being particularly preferred.
- Dopants and coating materials may be added to the reactor either as carbonates, oxides or metals as appropriate to make the desired composition.
- the cathode is formed from an oxide precursor comprising salts of Li, Ni, Mn, Co, Al or Fe as will be more fully described herein.
- the oxide precursor is calcined to form the cathode material as a lithium metal oxide.
- the cathode material is optionally treated with a phosphate salt, XPO4, wherein X is the atoms necessary to balance the charge and X may be a monovalent atom, a divalent atom or a trivalent with the understanding that combinations may be used as desired. It is particularly preferred that X be easily removed either by washing or vaporization after application.
- the phosphate salt is applied to the surface of the metal oxide wherein the phosphate moiety forms MnPCM on the surface of the metal oxide, or is bonded to the surface of the metal oxide.
- the manganese is preferably predominantly in the +3 oxidation state with preferably less than 10 % of the surface manganese being in the +2 oxidation state and the manganese thereby stabilized against reduction to Mn 2+ at the surface.
- the reaction liberates X which is removed by washing or vaporization.
- X is selected from NH4 + , H + , Li + , Na + , and combinations thereof.
- Particularly preferred phosphates include (NH4)3PO4, (NH4)2HPO4, (NH4)H2PO4, and H3PO4 due to the ease of removal of X after formation of the surface manganese phosphate. It is preferred that the native manganese oxide of the calcined oxide precursor be reacted with phosphate as opposed to an added manganese or other metal. Therefore, it is preferred that the added phosphate be relatively free of Mn and more preferably less than 1 wt% manganese. It is preferable that no Mn +2 be added with the phosphate or after formation of the oxide. It is preferable that there be no separate manganese phosphate phase such as manganese phosphate as a distinct phase on the surface. It is preferable that the phosphate ligate the surface of the metal oxide.
- the oxide precursors are formed by reacting multi-carboxylic acids, preferably oxalic acid, with elemental metal powders to form insoluble salts without having to first form a sulfate salt or carbonate salt.
- the reaction rate of Co with multi-carboxylic acids is faster than Mn which is faster than Ni.
- the metal powders are added to a saturated suspension of multi-carboxylic acids, preferably oxalic acid, resulting in the liberation of H2(g) and the precipitation of metal salt with metal oxalate being exemplary of the metal multi-carboxylic acids.
- a particular advantage is that the, preferably oxalic, acid does not need to be completely dissolved at room temperature and therefore the amount of solvent, preferably water, required for the reaction can remain quite low which minimizes the energy required for removal of the water.
- the reactor may be stirred or agitated to ensure continued reaction.
- the reaction may be accomplished in a horizontal bead-mill to increase the reaction rate. It is preferable to heat the metal powder and multi-carboxylic acids to increase the reaction rate.
- the reaction will proceed at low temperature, such as 10°C, however slow reaction rate is undesirable.
- the reaction can be heated to over 100°C however, since water is a preferred solvent it is preferable not to exceed 100°C unless a reflux system is employed.
- the water may be replaced with an azeotropic mixture of water and alcohols which reduces the cost of drying.
- An exemplary azeotrope is 87.7wt% propan-2-ol which boils at 80.4°C without limit thereto.
- the reaction may also be heated to above 100°C either directly or partly through the bead-milling process.
- the reaction may be done in a reactor such as a horizontal ball mill using ZrO2 balls or a bead mill using ZrO2 beads.
- the reaction may take place in an autoclave so that temperatures above 100°C may be used such as up to 200°C.
- Li2COs are not particularly critical. If U2CO3 is added early in the process lithium salts, such as lithium oxalate, are formed by digestion of the carbonate and the lithium salt remains. Alternatively, the Li2COs can be added after the transition metal reaction is complete. The metals are oxidized by the acidic proton thereby producing H2 gas which is preferably handled in a manner consistent with conventional laboratory or manufacturing practice. In one embodiment the reactor may be under inert gas, such as N2 or He, or the vessel may be actively vented to avoid the risk of explosion.
- inert gas such as N2 or He
- reaction time is dependent on temperature and agitation, however, the reaction is allowed to continue until completion which is indicated by a colour change in the slurry or in the stabilization of the slurry pH.
- the slurry must be dried, such as by spray drying or drum drying, followed by calcining as usual in air and/ or O2 depending upon the final formulation of the CAM.
- the metal powder is mixed in the intended ratios in the ultimate CAM.
- the metal powder would have 8 molar parts Ni, 1 molar part Mn and 1 molar part Co with one molar part Li added prior to calcining.
- the elemental metal feedstock particle size may be adjusted so that the elemental metals react at similar rate.
- the particle size may be inversely related to the reaction rate such that the surface area increase mitigates the difference in reaction rate. Since the reaction rate follows the relationship Co>Mn>Ni it may be advantageous to utilize particle size differences which follow the same relationship.
- Sulfur concentration is particularly important for nickel wherein higher sulfur concentrations increase the reaction rate. It would be understood to those in the art that sulfur is undesirable for electrical performance and therefore sulfur is typically to be avoided, or below detectable limits. However, a small level of impurity may be acceptable to balance the reaction rate with electrical performance.
- a sulfur impurity of no more than 0.05 wt%, relative to nickel metal, can be effective at sufficiently increasing the reaction rate with the carbonate without significant decrease in electrical performance.
- reaction rate of nickel can be enhanced by the introduction of nitric acid prior to the introduction of the carbonate.
- Ni powder is first dissolved in nitric acid and allowed to cool to ambient temperature to form a nickel nitrate solution.
- a molar quantity of multi-carboxylic acid, preferably oxalic acid, is dispersed in water and, while stirring, the nickel nitrate solution is slowly added to the multi-carboxylic acid suspension forming a nickel, preferably oxalate, precipitate the completion of which is indicated by the absence of green supernatant solution.
- the required amounts of Li2COs with Mn metal powder, Co metal powder and doping and coating materials, dispersed in water slowly added to the Ni slurry while stirring until reaction is complete.
- the slurry is then spray dried and calcined as usual.
- Divalent metal oxalates such as NiC2O4, MnC2O4, COC2O4, ZnC2O4, etc. are highly insoluble, however monovalent metal oxalates such as Li2C2O4 are somewhat soluble with a solubility of 8g/100mL at 25°C in water. If it is necessary to have the lithium oxalate in solution and homogeneously dispersed throughout a mixed metal oxalate precipitate, then keeping the water volume above the solubility limit of lithium oxalate may be desirable.
- Multi-carboxylic acids comprise at least two carboxyl groups.
- a particularly preferred multi-carboxylic acid is oxalic acid due, in part, to the minimization of carbon which must be removed during calcining.
- Other low molecular weight di-carboxylic acids can be used such as malonic acid, succinic acid, glutaric acid and adipic acid.
- Higher molecular weight di-carboxylic acids can be use, particularly with an even number of carbons which have a higher solubility, however the necessity of removing additional carbons and decreased solubility renders them less desirable.
- the dried powders may be transferred into the calcining system batch-wise or by means of a conveyor belt. In large scale production, this transfer may be continuous or batch.
- the calcining system may be a box furnace utilizing ceramic trays or saggers as containers, a rotary calciner, a fluidized bed, which may be co-current or countercurrent, a rotary tube furnace and other similar equipment without limit thereto.
- the heating rate and cooling rate during calcinations depend on the type of final product desired. Generally, a heating rate of about 5°C per minute is preferred but the usual industrial heating rates are also applicable.
- the final powder obtained after the calcining step is a fine, ultrafine or nanosize powder that may not require additional crushing, grinding or milling as is currently done in conventional processing. Particles are relatively soft and not sintered as in conventional processing.
- the final calcined oxide powder is preferably characterized for surface area, particle size by electron microscopy, porosity, chemical analyses of the elements and also the performance tests required by the preferred specialized application.
- the spray dried oxide precursor is preferably very fine and nanosize.
- a modification of the spray dryer collector such that an outlet valve opens and closes as the spray powder is transferred to the calciner can be implemented.
- the spray dried powder in the collector can be transferred into trays or saggers and moved into a calciner.
- a rotary calciner or fluidized bed calciner can be used to demonstrate the invention.
- the calcination temperature is determined by the composition of the powder and the final phase purity desired. For most oxide type powders, the calcination temperatures range from as low as 400 °C to slightly higher than 1000 °C. After calcination, the powders are sieved as these are soft and not sintered. The calcined oxide does not require long milling times nor classifying to obtain narrow particle size distribution.
- the LilV CM spinel oxide has a preferred crystallite size of 1-5pm.
- the LiMC rock salt oxide has a preferred crystallite size of about 50-250 nm and more preferably about 150-200 nm.
- a particular advantage of the present invention is the formation of metal chelates of multi-carboxylic acids as opposed to acetates.
- Acetates function as a combustion fuel during subsequent calcining of the oxide precursor and additional oxygen is required for adequate combustion.
- Lower molecular weight multi-carboxylic acids, particularly lower molecular weight dicarboxylic acids, and more particularly oxalic acid decompose at lower temperatures without the introduction of additional oxygen.
- the oxalates for example, decompose at about 300°C, without additional oxygen, thereby allowing for more accurate control of the calcining temperature. This may allow for reduced firing temperatures thereby facilitating the formation of disordered Fd3m spinel crystalline structures with minimal impurity phase occurring as seen at high temperature
- the process is easily scalable for large scale manufacturing using presently available equipment and/or innovations of the present industrial equipment.
- Composite electrodes would be prepared by mixing the active material with
- Coin cells would be assembled in an argon-filled glovebox.
- Lithium foil (340 pm) would be used as counter and reference electrodes in half-cells, and commercial Li4TisOi 2 (LTO) composite electrodes would be used as counter and reference electrodes in full-cells.
- LiPFe in 7:3 (vol%) ethylene carbonate (EC):diethylene carbonate (DEC) would be used as the electrolyte.
- the electrodes would be separated by one or two 25pm thick sheets of Celgard® membranes in half-cells, and one sheet of Celgard membrane full-cells.
- the spinel cathode cells would be galvanostatically cycled in the voltage range of 3.5 V - 4.9 V at various C-rates (1 C rate equivalent to 146 mAg -1 ) at 25 °C, using an Arbin Instrument battery tester (model number BT 2000).
- a constant voltage charging step at 4.9 V for 10 minutes would be applied to the cells at the end of 1 C or higher rate galvanostatic charging steps.
- the rock-salt NMC cells would be galvanostatically cycled in the voltage range of 2.7 V - 4.35 V at various C-rates (1 C rate equivalent to 200 mAg -1 ) at 25 °C.
- a constant voltage charging step at 4.35 V for 10 minutes would be applied to the cells at the end of 1 C or higher rate galvanostatic charging step.
- the resultant slurry was dried using a Buchi benchtop spray dryer to produce a complete precursor powder.
- the precursor was placed in alumina saggars and fired in an oxygen flow in the following way. Heat from ambient to 120°C in 20 minutes and hold at that temperature for 1 hour. Heat to 860°C in 142 minutes and hold for 15 hours. Cool to 550°C in 60 minutes and then to 120°C in 3 hours. Allow passive cooling to ⁇ 100°C when the sample is removed, ground and passed through a 325 mesh sieve before vacuum packing in a metallized polymer bag.
- XRD x-ray diffraction
- Ni powder is first dissolved in 9M nitric acid and allowed to cool to ambient temperature.
- the required oxalic acid is dispersed in water and, while stirring, the nickel nitrate solution is slowly added to the oxalic acid suspension and the nickel oxalate precipitation proceeds until there is no green supernatant solution.
- the required amounts of U2CO3 with Mn, Co, metal powders doping and coating materials, dispersed in water are slowly added to the Ni oxalate slurry while stirring and left to react with the acid until reaction is complete.
- Fig. 3 shows the X-ray diffractograms of oxalates produced from the carbonate method as a control (blue) and the inventive method involving the initial formation of nickel nitrate (red).
- the peak locations align with a few exceptions which can be accounted for by the lower pH of the reaction mixture which influences the relative proportions of Li2HC2O4 and Li2C2O4 in the solid oxalate powder.
- NMC811 is produced as seen in the X- ray diffractograms shown in Fig. 4.
- the targeted 8:1 :1 ratio of Ni:Mn:Co is further corroborated by the atomic absorption data presented in Table 1 wherein the metal content is expressed as normalized to the total amount of transition metals present.
- Figs. 5 and 6 show the first five cycles at C/10 followed immediately by the 100 cycles at 1 C (left) as well as just the 1 C cycles normalized to the first cycle.
- the first five cycles at the lower charging rate are indicative of the maximum discharge capacity that can be obtained from the material where as the trajectory and final capacity after the 100 cycles at 1 C indicate the capacity retention upon repeated aggressive cycling.
- reaction mixture is the spray dried to yield 79.12g fine light turquoise powder.
- 18g of oxalate precursors are placed in two alumina saggars and calcined in a tube furnace under 0.76L oxygen per minute according to the following temperature profile: ramp up from room temperature to 120°C over 20 minutes and hold for 1 hour, ramp up from 143°C to 830°C over 142 minutes and hold for 15 hours, ramp down to 550°C over 1 hour then continue to ramp down to 120°C for 3 hours.
- the tube furnace is then allowed to passively cool until below 100°C at which point the resulting NMC811 is removed, ground in an agate mortar and pestle and sieved through 325mesh, and finally sealed in an aluminum vacuum bag and stored in a dessicator.
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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EP21863156.2A EP4208907A1 (en) | 2020-09-03 | 2021-09-02 | Alternative one-pot process for making cam precursor using metal feedstocks |
KR1020237008271A KR20230048131A (en) | 2020-09-03 | 2021-09-02 | An Alternative One-Pot Process for Manufacturing CAM Precursors Using Metal Feedstocks |
JP2023513982A JP2023543552A (en) | 2020-09-03 | 2021-09-02 | Alternative one-pot method for producing CAM precursors using metal raw materials |
CN202180054609.5A CN116235329A (en) | 2020-09-03 | 2021-09-02 | Alternative one-pot method for preparing CAM precursors using metal starting materials |
CA3190981A CA3190981A1 (en) | 2020-09-03 | 2021-09-02 | Alternative one-pot process for making cam precursor using metal feedstocks |
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US202063074025P | 2020-09-03 | 2020-09-03 | |
US63/074,025 | 2020-09-03 | ||
US202163161664P | 2021-03-16 | 2021-03-16 | |
US63/161,664 | 2021-03-16 |
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CA3048267A1 (en) * | 2017-01-18 | 2018-07-26 | Nano One Materials Corp. | One-pot synthesis for lithium ion battery cathode material precursors |
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- 2021-09-02 WO PCT/CA2021/051216 patent/WO2022047585A1/en active Search and Examination
- 2021-09-02 EP EP21863156.2A patent/EP4208907A1/en active Pending
- 2021-09-02 CN CN202180054609.5A patent/CN116235329A/en active Pending
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CA3048267A1 (en) * | 2017-01-18 | 2018-07-26 | Nano One Materials Corp. | One-pot synthesis for lithium ion battery cathode material precursors |
Non-Patent Citations (4)
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