WO2023233144A1 - Procédé de production d'un matériau de cathode pour batteries rechargeables au lithium et/ou au sodium-ion - Google Patents

Procédé de production d'un matériau de cathode pour batteries rechargeables au lithium et/ou au sodium-ion Download PDF

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Publication number
WO2023233144A1
WO2023233144A1 PCT/GB2023/051425 GB2023051425W WO2023233144A1 WO 2023233144 A1 WO2023233144 A1 WO 2023233144A1 GB 2023051425 W GB2023051425 W GB 2023051425W WO 2023233144 A1 WO2023233144 A1 WO 2023233144A1
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intercalatable
ion
process according
typically
minutes
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PCT/GB2023/051425
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English (en)
Inventor
Dr. Shutao WANG
Dr Thomas Edward ASHTON
Professor Jawwad Arshad DARR
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Ucl Business Ltd
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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
    • 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
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C01P2006/40—Electric properties

Definitions

  • the present invention relates to a cathode material for a rechargeable lithium (Li) and/or sodium (Na)-ion battery and to a process of production of such a cathode material.
  • the cathode materials can include metal oxide mixtures in specific structures such as layered structures.
  • metal oxides containing mixtures of nickel, manganese and cobalt have been widely employed. These mixtures may also contain additional dopants or other elements which confer specific favourable properties.
  • the amounts of the three main elements can vary from 0 to nearly 100%. While the nickel content is maximised to achieve greater energy density, the amount of cobalt is being reduced due to political and/or sustainability issues and cost.
  • Ni, Mn, Co nickel and low amounts of cobalt also confer instability issues during battery operation unless mitigating precautions are taken.
  • These materials are known as the NMC (Ni, Mn, Co) family and/or NCA (Ni, Co, Al) and/or similar high nickel cathode materials.
  • CHFS Continuous Hydrothermal Flow Synthesis
  • CJM Confined Jet Mixer
  • cathode material with a high energy density or capacity at high power.
  • the cathode materials are particularly effective when the battery is charged or discharged rapidly such as at >1 C.
  • a process for the production of a cathode material for a rechargeable Li and/or Na-ion battery comprising the steps of a. preparing an uncalcined precursor blend of one or more metal compounds suitable to form a Li and/or Na-ion intercalatable structure upon solid state thermal treatment; b. further blending the uncalcined precursor blend produced in step a. with a Li and/or Na-ion source; c. drying the Li and/or Na-ion containing mixture produced in step b.; d. flash heating the uncalcined Li and/or Na-ion containing mixture produced in step c.
  • step d quenching the intercalatable structure produced in step d; wherein the flash heating and quenching rate whether heating or cooling is from 2400 to 100°C per minute.
  • the metal compounds are not restricted and may be any compound that forms a suitable intercalatable structure for the Li and/or Na-ions at the cathode.
  • the metals are selected from manganese, nickel, iron, cobalt, copper and aluminium.
  • the metal compounds in step a. are in the form of oxides, hydroxides, oxyhydroxides or a combination thereof.
  • the metal compounds in step d. are in the form of oxides or hydroxides, or a combination thereof.
  • Suitable metal compounds are transition metal oxides and/or hydroxides such as nickel, manganese and cobalt oxides and/or hydroxides; mixed metal oxides and/or hydroxides of nickel and manganese; nickel, manganese and cobalt; and/or nickel, cobalt and aluminium.
  • Li x NiaMnbCocC>2 where a + b + c 1 ⁇ 0.1 , and where x is from 0.9 to 1 .1 , typically x is about 1 ; iv. LixMriaC where x is from 0.9 to 1.1 , typically x is about 1 , and where a is from 1 .8 to 2.2; and/or v. LixNiaMnbC where x is from 0.9 to 1 .1 , typically x is about 1 , and where a + b is from 1 .8 to 2.2, typically is about 2;
  • intercalatable structures may not only be based on intercalatable metal compounds and can also include suitable dopants and surface treatments known to the skilled person.
  • the blend produced in step a. may have any suitable average particle size.
  • the average particle size may be ⁇ 25 pm, such as, ⁇ 15 pm, such as, ⁇ 5 pm.
  • the blend produced in step a. may have an average particle size range of 1-25 pm, more typically, 1-15 pm, most typically, 1 to 5 pm.
  • the process of the present invention may be a batch or continuous process.
  • the flash heating may be carried out in a continuous heating process (for example using a mobile conveyor that allows rapid heating and cooling).
  • the flash heating may be carried out in a batch/semi batch heating process in which the material is rapidly heated and cooled for set time periods.
  • a suitable method for producing the precursor blend in step a. may be a wet chemical process such as precipitation.
  • a suitable wet precipitation process is one in which a precursor blend is produced that contains an intimate mixture of the elements, such as oxides and/or hydroxides and/or oxyhydroxides.
  • a suitable process may be the continuous hydrothermal flow synthesis process, which produces very small particles of precursor blend.
  • the metal compounds may be mixed in aqueous solution and then precipitated through the process to form the precursor blend.
  • This precursor blend may be washed and cleaned to remove residual chemicals from the manufacture.
  • the resulting wet solid precursor may be dried.
  • the dry precursor blend produced in step a. is typically in the form of a powder.
  • the dry precursor blend may then be mixed thoroughly with a Li and/or Na-ion source such as lithium hydroxide and/or sodium hydroxide in the presence of a suitable liquid or solvent, such as water, and then dried.
  • a Li and/or Na-ion source such as lithium hydroxide and/or sodium hydroxide
  • a suitable liquid or solvent such as water
  • the Li and/or Na-ion source should remain well mixed after drying.
  • the dry mixture produced in step c., flash heated in step d. and quenched in step e. is in the form of a powder.
  • the powder produced has a homogenous distribution of elements, preferably at the micro or nanoparticle level.
  • Flash heating comprises the steps of exposing the precursor mixture to an elevated temperature for a short period of time, typically less than two hours, more typically less than 1 hour, such as less than 40 minutes.
  • the flash heating step may be carried out for any suitable time period.
  • the time period for carrying out the flash heating step may be ⁇ 90 minutes, such as ⁇ 60 minutes, such as ⁇ 45 minutes, such as ⁇ 30 minutes, for example ⁇ 25, ⁇ 15, ⁇ 10 or ⁇ 5 minutes.
  • the flash heating is for >1 second, such >5 seconds, such as >20 seconds, such as >30 seconds, for example >50, >100, >200 or >400 seconds.
  • the flash heating step may be carried out for 1 second to 90 minutes, typically, 5 seconds to 60 minutes, more typically 20 seconds to 45 minutes, most typically, 30 seconds to 30 minutes, such as 50 seconds to 30 minutes, such as 100 seconds to 30 minutes, such as 200 seconds to 30 minutes, such as 400 seconds to 30 minutes.
  • the flash heating step d. may be carried out at any suitable temperature.
  • the flash heating temperature to which the Li and/or Na-ion containing mixture produced in step c. is exposed may be ⁇ 1600°C, such as ⁇ 1400°C, such as ⁇ 1200°C.
  • Typical temperature ranges for the flash heating step d. are from above the sintering temperature of the mixture, for example >700°C, such as >750°C, such as >800°C.
  • Typical ranges for the flash heating step may be 700 to 1600°C, more typically, 750 to 1250°C, most typically, 800 to 1200°C.
  • the flash heating step d. may be carried out at a rate and temperature that minimises Li and/or Na evaporation, and allows an efficient solid state reaction.
  • the sample is generally at room temperature or at least in the range 0 to 45°C.
  • the intercalatable structure produced in step d. is then quenched in step e. so as to “freeze” the state of the material through rapid and controlled cooling.
  • Rapid and controlled cooling of the sample in step e. is operable to lock in the desired defect structure resulting from the flash heating.
  • the quenching time is determined by the time necessary to effectively lock in structure, typically the desired structure containing the desired amount and type of defects for optimal performance.
  • the quenching step e. may be carried out for any suitable time period to effect the desired material properties, in particular the freezing of the defective structure produced in step d.
  • the quenching time may be carried out for between 1 second to 1 hour, more typically, between 20 seconds to 30 minutes, most typically, 1 to 10 minutes.
  • the quenching time may be carried out for ⁇ 55 minutes, more typically, ⁇ 45 minutes, most typically, ⁇ 25 minutes, such as ⁇ 15 minutes or ⁇ 5 minutes. Rapid quenching may be achieved using suitable refrigerants.
  • the quenching time may be taken as the time taken to reduce the temperature of the heated sample from its temperature at the end of the flash heating step in step d. to ⁇ 100°C.
  • Flash heating and quenching rates are from 2400 to 100°C per minute.
  • the flash heating and quenching rate whether heating or cooling is from 1200 to 150°C per minute, such as from 600 to 200 °C.
  • the flash heating and quenching steps may be part of a batch process where the samples are introduced one-by-one into a static furnace or may be part of a continuous process where the samples pass into or through a furnace to heat up and subsequently cool down again, or via a process where a heater is moved over a bed of sample.
  • the invention provides high-performance cathode materials using considerably less energy than current industrial processes which typically involve heating the materials to >800°C for 12 hours or more. Further ramping and cooling of the temperature each add several additional hours to the process.
  • the invention provides the possibility for materials to be heated and cooled in as little as 20 minutes or less.
  • a cathode material for a Li ion and/or Na-ion battery comprising a metal compound intercalatable structure and a Li ion and/or Na-ion source intercalated into said structure wherein the said metal compound intercalatable structure is defective.
  • the intercalatable structure is at least 1 % defective, such as at least 2% defective, such as at least 3% defective, such as at least 4% defective, or even at least 5 or 6% defective.
  • the intercalatable structure may be up to 10% defective, such as up to 9% defective, such as up to 8% defective, such as up to 7% defective.
  • the intercalatable structure may have defects present in the range of from 1 to 10%, more typically from 2 to 9%, most typically from 3 to 8%, especially from 4 to 7%.
  • the nature of such defects are typically anti-site defects, i.e. Li + /M x+ or Na + /M x+ cation mixing.
  • the amount of defects(%) are measurable with structural techniques, such as XRD (X- ray Powder Diffraction) or NPD (Neutron powder diffraction). Unless indicated otherwise, the % defects refers to the degree of this anti-site mixing as determined by XRD or NPD, more typically, XRD.
  • the average particle size of the particles produced by the process of the invention or the cathode material product of the invention may be any suitable average particle size.
  • the average particle size may be ⁇ 20 pm, such as ⁇ 10 pm, such as ⁇ 5 pm.
  • the average particle size may be 1 to 20 pm, more typically, 1 to 10 pm, most typically, 1 to 5 pm.
  • intercalatable is meant the structure may accommodate intercalated Li and/or Na-ions therein, and may be effective to allow migration thereof to the anode of Li and/or Na-ions during charging, and may be effective to accommodate the return of the Li and/or Na-ions during use of a battery incorporating the structure at the cathode.
  • Figure 1 shows a configuration diagram of the Continuous Hydrothermal Flow Synthesis (CHFS) used to produce Example 1 (NMC532) and Example 2 (NCA) precursor powders.
  • CHFS Continuous Hydrothermal Flow Synthesis
  • Figure 2 shows the tabulated values for Example 1 (NMC532) and Example 2 (NCA) cycled at C/10 (‘low’ rate, charge or discharge in 10 hours);
  • Figure 3 shows the tabulated values for Example 1 (NMC532) and Example 2 (NCA) cycled at 10C (‘high’ rate, charge or discharge in 6 min);
  • Figure 4 shows a comparison of gravimetric capacity of Example 1 (NMC532) and Example 2 (NCA) to Comparative Example 1 (commercial NCA-powder) and Comparative Example 2 (commercial NCA-sheet).
  • the precursor powder was synthesised according to the following method using a Continuous Hydrothermal Flow Synthesis (CHFS) reactor, utilising a Confined Jet Mixer (CJM).
  • CHFS Continuous Hydrothermal Flow Synthesis
  • CJM Confined Jet Mixer
  • a third pump ( Figure 1 , pump P1) was used to pump ambient temperature deionised water under pressure (240 bar) at a rate of 400 mL min -1 into a heat exchanger at 450°C which produced a supercritical water flow.
  • the combined P2 and P3 flow (iii) was mixed in the CJM with the supercritical water flow at a mixing temperature of about 335°C, whereupon precipitation and crystallisation occurred to produce a slurry.
  • the slurry was cooled to 40°C using a pipe-in-pipe heat exchanger. The cooled slurry product was then collected at the exit of the CHFS process at about 50°C.
  • the collected slurry was then centrifuged at 4000 rpm (using model Sigma 6-16S, Sigma Aldrich, Dorset, UK) until the solid content settled and the liquid was removed by pouring.
  • the remaining wet solids were cleaned by dialysis in Visking Dialysis Membrane (Medicell Membranes Ltd) using deionised water until a conductivity value below 100 pS was achieved.
  • the cleaned slurry was then centrifuged at 4000 rpm for 30 minutes (using model Sigma 6-16S, Sigma Aldrich, Dorset, UK) into a thick paste and any remaining bulk water poured off.
  • the freeze dried precursor powder was then mixed with a lithium source. 167.85 g of LiOH’F was dissolved in 800 mL deionised water for 30 minutes to produce a 5M LiOH aqueous solution.
  • the LiOH aqueous solution (LiOH «H2O) was then added (80 mL min -1 ) to 200 g of the precursor powder under continuous stirring using a high shear mixer (IKA, T18 digital package S2, Ultra-turrax) for 20 minutes (10 minutes at 12000 rpm followed by 10 minutes at 16000 rpm) to obtain a composite material.
  • the resulting solid dry mixture was then placed into an alumina crucible before being slowly fed into a pre-heated tube furnace, at the desired temperature (typically, “slowly” means over about 1 or 2 minutes to avoid thermal shock).
  • the crucible was maintained in the furnace at the temperature for the desired time and subsequently removed and allowed to cool to room temperature.
  • the heating process referred to is a flash heat treatment.
  • Example 1 (NMC532 - nickel manganese cobalt) was synthesised and processed according to the above methodology.
  • the aqueous solution containing a mixture of metals in (i) was as follows: - 0.556M total metal concentration solution comprised of 0.266M Ni(NO 3 )2'6H2O; 0.15M Mn(NO 3 )2'4H 2 O and 0.14M Co(N0 3 ) 2 '6H 2 0.
  • a 2M KOH was used as the base feed (ii).
  • the formed solid dry mixture of NMC532 was heated in a furnace at 1090, 1100, 1110 and 1120°C for 0.5, 1 , 1.5, 2, 2.5, 3, 3.5, 4, 4.5 and 5 minutes to prepare a library of Example 1 samples (i.e. 40 different materials).
  • Example 2 (NCA - nickel cobalt aluminium) was synthesised and processed according to the above methodology.
  • the aqueous solution containing a mixture of metals in (i) was as follows: - 0.5M total metal concentration solution comprised of 0.4M Ni(NO3)2'6H2O, 0.025M AI(NC>3)3'9H2O and 0.075M Co(NC>3)2'6H20.
  • a 1 ,5M KOH was used as the base feed (ii).
  • Figure 2 shows the tabulated values for Example 1 (NMC532) and Example 2 (NCA) cycled at C/10 (‘low’ rate, charge or discharge in 10 hours). It can be seen from the results that the performance is dependent on the time and temperature conditions. The optimum time was lower, and temperature higher for Example 1 (NMC532) with a best performance at a time range of 4.0 to 4.5 minutes at 1090°C, compared to Example 2 (NCA) with a best performance at a time range 8 to 10 minutes at 850°C.
  • Figure 3 shows the tabulated values for NMC532 and NCA cycled at 10C (‘high’ rate, charge or discharge in 6 minutes) where a similar relationship to the low-rate data between time, temperature and gravimetric capacity is observed.
  • Figure 4 shows the capacities achieved for Example 1 (NMC52) and Example 2 (NCA) compared to the capacity of commercial cathodes Comparative Example 1 (NCA powder - Lithium Nickel Cobalt Aluminium Oxide (LiNiCoAI02)) and Comparative Example 2 (NCA sheet - Lithium Nickel Cobalt Aluminium Oxide (LiNiCoAI02)). Comparative Example 1 (NCA powder) and Comparative Example 2 (NCA sheet) are cathodes that are commercially available from Targray, Canada.

Abstract

L'invention concerne un procédé de production d'un matériau de cathode pour une batterie rechargeable au lithium (Li) et/ou au sodium (Na)-ion. Le procédé comprend les étapes consistant à : - a. préparer un mélange précurseur non calciné d'un ou de plusieurs composés métalliques appropriés pour former une structure pouvant être intercalée avec Li-ion et/ou Na-ion lors d'un traitement thermique à l'état solide ; b. mélanger le mélange précurseur non calciné produit à l'étape a. avec une source de Li et/ou Na-ion ; c. sécher le mélange contenant du Li et/ou du Na-ion produit à l'étape b. ; et d. réaliser un chauffage instantané du mélange contenant du Li et/ou du Na-ion non calciné produit à l'étape c. pour produire une structure pouvant être intercalée avec un composé métallique avec des ions Li et/ou Na intercalés, la structure pouvant être intercalée étant défectueuse. Le procédé se poursuit par la trempe de la structure pouvant être intercalée produite à l'étape d. Le chauffage instantané et le taux de trempe qu'il s'agisse d'un chauffage ou d'un refroidissement est de 2400 à 100°C par minute.
PCT/GB2023/051425 2022-05-30 2023-05-30 Procédé de production d'un matériau de cathode pour batteries rechargeables au lithium et/ou au sodium-ion WO2023233144A1 (fr)

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GB2207971.9 2022-05-30
GBGB2207971.9A GB202207971D0 (en) 2022-05-30 2022-05-30 Process for the production of a cathode material for rechargeable lithium and/or sodium-ion batteries

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US20120130694A1 (en) * 2008-12-12 2012-05-24 Nanoexa Corporation Simulated X-Ray Diffraction Spectra for Analysis of Crystalline Materials
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