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WO2023050806A1 - Matériau d'électrode positive à base de phosphate ferrique de sodium dopé, son procédé de préparation et son application - Google Patents

Matériau d'électrode positive à base de phosphate ferrique de sodium dopé, son procédé de préparation et son application Download PDF

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Publication number
WO2023050806A1
WO2023050806A1 PCT/CN2022/090072 CN2022090072W WO2023050806A1 WO 2023050806 A1 WO2023050806 A1 WO 2023050806A1 CN 2022090072 W CN2022090072 W CN 2022090072W WO 2023050806 A1 WO2023050806 A1 WO 2023050806A1
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Prior art keywords
sodium
phosphate
nickel
cobalt
preparation
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PCT/CN2022/090072
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English (en)
Chinese (zh)
Inventor
余海军
钟应声
李爱霞
谢英豪
张学梅
李长东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
Original Assignee
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Priority to DE112022003502.1T priority Critical patent/DE112022003502T5/de
Priority to GB2310302.1A priority patent/GB2618695A/en
Priority to ES202390248A priority patent/ES2977204R1/es
Publication of WO2023050806A1 publication Critical patent/WO2023050806A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H01M4/58—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
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/582—Halogenides
    • 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 invention belongs to the technical field of battery materials, and in particular relates to a doped sodium iron phosphate cathode material and a preparation method and application thereof.
  • LIBs lithium-ion batteries
  • NIBs sodium-ion batteries
  • the cathode material is the key to the technology of sodium-ion batteries. It is difficult for the existing cathode active materials to achieve stable deintercalation of sodium ions, which limits the engineering application of sodium-ion batteries.
  • the present invention aims to solve at least one of the technical problems in the above-mentioned prior art.
  • the present invention provides a doped sodium iron phosphate positive electrode material and its preparation method and application.
  • the doped sodium iron phosphate positive electrode material introduces nickel and cobalt to dope sodium iron phosphate.
  • the ratio improves the phase transition in the process of sodium ion deintercalation, and plays a role in improving the cycle stability of the sodium iron phosphate crystal structure.
  • the present invention adopts the following technical solutions:
  • a doped sodium iron phosphate cathode material the chemical formula is xAlF 3 -MPO 4 , M is NaNi a Co b Fe, 0 ⁇ x ⁇ 0.2, 0 ⁇ a ⁇ 1, 0 ⁇ b ⁇ 0.5.
  • a preparation method of a doped sodium iron phosphate positive electrode material comprising the following steps:
  • the ferrous nickel mixed hydroxide is mixed with phosphate-containing substances, sodium source, cobalt source, dispersant, aluminum fluoride, ball milled, and roasted to obtain a doped sodium iron phosphate positive electrode material.
  • the preparation step of the aluminum fluoride is: using ammonium hexafluoroaluminate to decompose by heating.
  • ammonium hexafluoroaluminate can be prepared by reacting aluminum chloride and ammonium fluoride in the presence of water.
  • ammonium hexafluoroaluminate is prepared from aluminum powder recovered from waste lithium batteries as an aluminum source.
  • the preparation process of the ammonium hexafluoroaluminate can specifically be: add hydrochloric acid to the aluminum powder, react to obtain an aluminum chloride solution, add ammonium fluoride to obtain ammonium hexafluoroaluminate, heat and decompose it to obtain fluorine Aluminum.
  • the aluminum powder is obtained by crushing and sieving waste lithium batteries.
  • the aluminum powder and hydrochloric acid are reacted at a molar ratio of Al to HCl of 10:(30-100).
  • the molar ratio of aluminum chloride and ammonium fluoride is 10:(40-150).
  • the method further includes evaporating the ammonium hexafluoroaluminate before heating and decomposing, and the evaporation temperature is 90-120°C.
  • the thermal decomposition temperature is 200-380°C, and the thermal decomposition time is 0.5h-6h.
  • the decomposition reaction formula of ammonium hexafluoroaluminate is: (NH 4 ) 3 AlF 6 ⁇ AlF 3 +3HF+3NH 3 .
  • the nickel-containing alloy is ground into powder by adding a grinding aid before acid leaching;
  • the grinding aid is one of sodium sulfate, sodium chloride or sodium phosphate.
  • the nickel-containing alloy is one of nickel-iron and nickel-containing pig iron.
  • the nickel content in ferronickel is ⁇ 15.0%.
  • the nickel content in the nickel-containing pig iron is ⁇ 4.0%.
  • the acid is at least one of phosphoric acid, sulfuric acid, hydrochloric acid or nitric acid.
  • the solid-to-liquid ratio of the nickel-containing alloy to the acid is 1: (3-30) g/ml.
  • the H + content in the acid is 2-15 mol/L.
  • step (1) further comprising evaporating the leaching solution obtained after acid leaching to remove acid, and the evaporation temperature is 100-400°C.
  • adding water for dissolution is also included after the evaporation to obtain a ferronickel salt solution.
  • the solid-to-liquid ratio of the nickel-iron salt and water is (1-10): (30-100) kg/L.
  • the reducing agent is one of iron powder, iron sulfite and sodium sulfite.
  • the alkali is an aqueous solution of alkali metal and alkaline earth metal.
  • the alkali metal is one of lithium, sodium and potassium; the alkaline earth metal is one of calcium and magnesium.
  • the aqueous solution of alkali metal is sodium hydroxide, and the concentration of sodium hydroxide is 0.1-10 mol/L.
  • step (1) the pH is adjusted to 7.0-9.0 to recover ferrous nickel hydroxide.
  • the pH is adjusted to 7.5-8.0.
  • the phosphate-containing substance is phosphoric acid, pyrophosphoric acid, metaphosphoric acid, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, iron phosphate, nickel phosphate, lithium phosphate, ammonium phosphate, At least one of ammonium dihydrogen phosphate or ammonium hydrogen phosphate.
  • the phosphate-containing substance is at least one of ammonium phosphate, ammonium dihydrogen phosphate or ammonium hydrogen phosphate.
  • the sodium source is sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium acetate, sodium oxalate, sodium formate, sodium citrate, coke At least one of sodium phosphate or sodium metaphosphate.
  • the sodium source is sodium phosphate.
  • the cobalt source is at least one of cobalt hydroxide, cobalt oxalate, cobalt phosphate or cobalt carbonate.
  • the dispersant is at least one of polyalkylene oxide, phenolic resin, polyvinylpyrrolidone, N-methylpyrrolidone, methanol, ethanol, polyol or polyolamine.
  • the general chemical formula of the polyol is C n H 2n+2-x (OH) x (X>2).
  • the polyol is polypropylene glycol.
  • the polymeric alcohol amine is triethanolamine.
  • the dispersant is at least one of polyalkylene oxide, methanol, ethanol or polypropylene glycol.
  • step (2) mixture A is obtained after mixing the ferrous nickel mixed hydroxide with phosphate-containing substances, sodium source, and cobalt source, and in the mixture A, sodium, ferrous, nickel, cobalt
  • the molar ratio is (0.01 ⁇ 150):(0.01 ⁇ 150):(0 ⁇ 100):(0 ⁇ 50).
  • the mass ratio of the mixture A, dispersant, and aluminum fluoride is 100:(10-200):(0-20).
  • the particle size of the ball mill output is ⁇ 20 ⁇ m, and the ball mill is performed at 100-1200 r/min for 1-12 hours.
  • the firing atmosphere is one of nitrogen atmosphere, neon atmosphere, argon atmosphere, and helium atmosphere.
  • the temperature of the calcination is 500-1000° C., and the calcination time is 1-24 hours.
  • the present invention also provides a sodium ion battery, comprising the doped sodium iron phosphate cathode material.
  • the doped sodium iron phosphate positive electrode material prepared by the present invention introduces nickel and cobalt to dope sodium iron phosphate, which can improve the phase transition in the process of sodium ion deintercalation by increasing the ratio of nickel and cobalt, and improve the crystallinity of sodium iron phosphate.
  • the role of structural cycle stability by coating aluminum fluoride on the surface of doped sodium iron phosphate, it can reduce the surface loss of sodium ion deintercalation during charge and discharge, inhibit the growth of Na dendrites, improve the cycle stability of the surface of sodium iron phosphate, and improve the performance of sodium iron phosphate.
  • the electrical conductivity of the surface enhances the electrochemical performance of sodium iron phosphate.
  • the present invention utilizes nickel-containing alloys, solves the problem of selecting iron and doping metals in sodium iron phosphate, and achieves the purpose of synthesizing nickel-cobalt-doped sodium iron phosphate.
  • nickel-containing alloys iron accounts for the largest proportion, followed by nickel. Therefore, iron is separated to synthesize ferrous phosphate, nickel and cobalt are separated to synthesize nickel-cobalt phosphate, and nickel-cobalt is introduced for doping.
  • the present invention can be improved by adjusting the ratio of nickel-cobalt phosphate
  • the phase transition during the deintercalation of sodium ions plays a role in improving the cycle stability of the sodium iron phosphate crystal structure.
  • aluminum recovered from waste lithium batteries is used for secondary utilization to prepare aluminum fluoride, and aluminum fluoride enhances the electrical properties of sodium iron phosphate.
  • the by-product aluminum recovered from waste lithium batteries is prepared as aluminum powder, and the aluminum powder is dissolved in acid and ammonium fluoride is added to prepare ammonium hexafluoroaluminate.
  • the aluminum fluoride obtained by thermal decomposition of ammonium hexafluoroaluminate has high stability and Good conductivity, coating aluminum fluoride on the surface of sodium iron phosphate can reduce the surface loss of sodium ion deintercalation during charge and discharge, improve the cycle stability of the surface of sodium iron phosphate, and lead to the reduction of iron-based phosphate on the surface The resistance is improved and the electrochemical performance of sodium iron phosphate is enhanced.
  • Fig. 1 is the SEM figure of the doped type sodium iron phosphate cathode material prepared in embodiment 1;
  • the doped sodium iron phosphate cathode material in this embodiment has a chemical formula of 0.015AlF 3 -NaNi 0.089 Co 0.064 FePO 4 .
  • Nickel-containing pig iron (Ni content 11.7%, iron content 82.6%) dissolution: crush 0.382kg of nickel-containing pig iron, add 7.2g of sodium sulfate to grind into nickel-containing pig iron powder, and send the nickel-containing pig iron powder to the airtight
  • Fig. 1 is the SEM figure of the nickel-cobalt-doped type sodium iron phosphate coated with positive electrode material aluminum fluoride prepared in Example 1
  • Fig. 2 is the SEM figure of the nickel-cobalt-doped type sodium iron phosphate prepared in Comparative Example 1
  • the nickel-cobalt-doped type in Example 1 is basically covered by aluminum fluoride, and there is a coating layer>10nm on the outside, so the overall is relatively blurred, while the nickel-cobalt-doped sodium iron phosphate prepared in Comparative Example 1
  • the exterior is clear with no cladding visible.
  • the doped sodium iron phosphate cathode material in this example has a chemical formula of 0.011AlF 3 -NaNi 0.087 Co 0.066 FePO 4 .
  • the doped sodium iron phosphate cathode material in this example has a chemical formula of 0.043AlF 3 -NaNi 0.38 Co 0.087 FePO 4 .
  • the preparation method of the sodium iron phosphate cathode material of this comparative example comprises the following concrete steps:
  • Sodium citrate and ferrous phosphate are mixed at a molar ratio of 1:1, then mixed with 320mL of ethanol by ultrasound, ball milled for 7h14min, then roasted in an argon atmosphere and a tube furnace at 730°C for 8h7min, and the temperature is lowered to obtain ferric phosphate Sodium NaFePO 4 cathode material.
  • the preparation method of the sodium iron phosphate cathode material of this comparative example comprises the following specific steps:
  • Sodium citrate and ferrous phosphate were mixed at a molar ratio of 1:1, and then mixed with 320mL of ethanol by ultrasound, ball milled for 6h49min, then roasted in an argon atmosphere and a tube furnace at 780°C for 8h7min, and cooled to obtain NaFePO 4 Cathode material.
  • Embodiment 1-3 and comparative example 1-2 analyze:
  • Doped sodium iron phosphate, conductive agent, and polytetrafluoroethylene were formulated into a slurry at a mass ratio of 85:10:5, and then coated on copper foil, and the pole pieces were dried in a drying oven at 80°C for 6 hours.
  • the die is stamped into a disc. Cut the sodium sheet into an electrode pole piece with a diameter of about 6mm, add 1.5mol/L sodium hexafluorophosphate to propylene carbonate to prepare the electrolyte, use Celgard2400 as the separator, and assemble the battery in a vacuum glove box under an argon atmosphere.
  • the cycle performance is tested with an electrochemical workstation, the charge and discharge range is 1.5-3.0V, and the test is performed at a rate of 2C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention se rapporte au domaine technique des matériaux de batterie. L'invention concerne un matériau d'électrode positive à base de phosphate ferrique de sodium dopé, son procédé de préparation et son application. La formule chimique du matériau d'électrode positive est xAlF3-MPO4, avec M représentant NaNiaCobFe, 0 ≤ x ≤ 0,2 ; 0 ≤ a ≤ 1 ; et 0 ≤ b ≤ 0,5. Dans le matériau d'électrode positive à base de phosphate ferrique de sodium dopé préparé par la présente invention, le nickel et le cobalt sont introduits pour doper le phosphate ferrique de sodium, la transformation de phase dans un processus de désintercalation des ions sodium peut être améliorée par ajustement de la proportion de phosphate de nickel et de cobalt, et l'effet d'amélioration de la stabilité de cycle d'une structure cristalline de phosphate ferrique de sodium est obtenu. Le fluorure d'aluminium est déposé sur la surface du phosphate ferrique de sodium dopé, réduisant ainsi la perte en surface de la désintercalation des ions sodium pendant la charge et la décharge, améliorant la stabilité de cycle de la surface du phosphate ferrique de sodium, améliorant la résistance du phosphate à base de fer réduit en surface, et améliorant les performances électrochimiques du phosphate ferrique de sodium.
PCT/CN2022/090072 2021-09-30 2022-04-28 Matériau d'électrode positive à base de phosphate ferrique de sodium dopé, son procédé de préparation et son application Ceased WO2023050806A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE112022003502.1T DE112022003502T5 (de) 2021-09-30 2022-04-28 Dotiertes natriumeisen(iii)phosphatmaterial für die positive elektrode, verfahren zu dessen herstellung und dessen verwendung
GB2310302.1A GB2618695A (en) 2021-09-30 2022-04-28 Doped sodium ferric phosphate positive electrode material, preparation method therefor and application thereof
ES202390248A ES2977204R1 (es) 2021-09-30 2022-04-28 Material de electrodo positivo fosfato férrico de sodio dopado, método de preparación para el mismo y aplicación del mismo

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CN202111161800.8A CN113948697B (zh) 2021-09-30 2021-09-30 掺杂型磷酸铁钠正极材料及其制备方法和应用
CN202111161800.8 2021-09-30

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DE (1) DE112022003502T5 (fr)
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WO (1) WO2023050806A1 (fr)

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CN117923452A (zh) * 2024-01-19 2024-04-26 贲安能源科技江苏有限公司 一种规模化制备复合型磷酸焦磷酸铁钠材料的方法
CN119812287A (zh) * 2025-02-27 2025-04-11 中国科学院宁波材料技术与工程研究所 一种铁基磷酸盐正极材料及其制备方法和应用
WO2025077148A1 (fr) * 2023-10-09 2025-04-17 荆门市格林美新材料有限公司 Matériau d'électrode positive au sulfate de sodium-fer-aluminium-titane dopé au carbone et son procédé de préparation

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CN113948697A (zh) * 2021-09-30 2022-01-18 广东邦普循环科技有限公司 掺杂型磷酸铁钠正极材料及其制备方法和应用

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CN117756078A (zh) * 2023-12-08 2024-03-26 深圳珈钠能源科技有限公司 空气稳定性好的铁基焦磷酸类二次电池正极材料制备方法
CN117756078B (zh) * 2023-12-08 2025-11-04 深圳珈钠能源科技有限公司 空气稳定性好的铁基焦磷酸类二次电池正极材料制备方法
CN117923452A (zh) * 2024-01-19 2024-04-26 贲安能源科技江苏有限公司 一种规模化制备复合型磷酸焦磷酸铁钠材料的方法
CN119812287A (zh) * 2025-02-27 2025-04-11 中国科学院宁波材料技术与工程研究所 一种铁基磷酸盐正极材料及其制备方法和应用

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