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WO2023024584A1 - Carbonate de cobalt dopé au nickel, son procédé de préparation et son utilisation - Google Patents

Carbonate de cobalt dopé au nickel, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2023024584A1
WO2023024584A1 PCT/CN2022/092471 CN2022092471W WO2023024584A1 WO 2023024584 A1 WO2023024584 A1 WO 2023024584A1 CN 2022092471 W CN2022092471 W CN 2022092471W WO 2023024584 A1 WO2023024584 A1 WO 2023024584A1
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nickel
carbonate
solution
cobalt
doped cobalt
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Chinese (zh)
Inventor
卢星华
李长东
阮丁山
刘更好
李斌
蔡勇
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Priority to GB2310283.3A priority Critical patent/GB2618694A/en
Publication of WO2023024584A1 publication Critical patent/WO2023024584A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/06—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Complex oxides containing cobalt and at least one other metal element
    • C01G51/42—Complex oxides containing cobalt and at least one other metal element containing alkali metals, e.g. LiCoO2
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C01P2006/80—Compositional purity
    • 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 precursors of positive electrode materials for lithium-ion batteries, and in particular relates to a nickel-doped cobalt carbonate and its preparation method and application.
  • Lithium cobaltate cathode material is mainly used in the 3C field due to its high energy density. With the popularization of 5G mobile phones, the requirements for lithium-ion battery life and volume continue to increase. Tricobalt tetroxide is used as the precursor of lithium cobaltate cathode material. It is prepared by thermal decomposition of cobalt carbonate.
  • Doping nickel in the cobalt carbonate precursor is beneficial to improve the discharge specific capacity of high-voltage materials (4.45V and above); since the solubility product of nickel carbonate is much larger than that of cobalt carbonate, In the process of synthesizing nickel-doped cobalt carbonate by co-precipitation method, due to the low precipitation rate of nickel in the medium, the nickel content in the supernatant is high, which increases the cost of wastewater treatment and is difficult to realize industrial production.
  • the present invention aims to solve at least one of the technical problems in the above-mentioned prior art. Therefore, the present invention proposes a nickel-doped cobalt carbonate and its preparation method and application.
  • a kind of preparation method of nickel-doped cobalt carbonate comprising the following steps:
  • S1 Mix the first carbonate solution and the nickel salt solution for reaction, and control the temperature and pH to obtain nickel carbonate seeds, and the first carbonate is one or both of sodium carbonate or potassium carbonate;
  • step S1 the specific process of step S1 is: first add the second carbonate solution as the bottom liquid, and simultaneously add the first carbonate solution and the nickel salt solution to the bottom liquid The reaction is carried out, and the temperature and pH are controlled to obtain nickel carbonate seed crystals; the second carbonate is one or both of sodium carbonate and potassium carbonate.
  • the concentration of the bottom liquid is 0.5-1.5 mol/L; preferably, the pH of the bottom liquid is 8.5-9.5.
  • step S1 the temperature of the reaction is 38-42° C., and the pH is 8.0-9.0.
  • the more specific process of step S1 is: first add the second carbonate solution to the reactor as the bottom liquid, control the temperature at 38-42°C, and add Nickel salt solution and sodium carbonate solution, the pH of the reaction is maintained at 8.0-9.0 by controlling the flow of the sodium carbonate solution, and when the particle size grows to the target value, the nickel carbonate seed crystals are obtained.
  • the particle size of nickel carbonate seeds can be controlled by different pH of the bottom solution, the temperature and time of seed crystal synthesis, and then the content of nickel element in the finished sample can be controlled.
  • the nickel salt is one or both of nickel chloride or nickel sulfate.
  • the concentration of nickel ions in the nickel salt solution is 1.5-2.0 mol/L, and the concentration of the first carbonate solution is 1.5-2.5 mol/L.
  • the flow rate of the nickel salt solution is 2-3L/h, and the co-current time is 10-20h.
  • the cobalt salt is one or both of cobalt chloride or cobalt sulfate.
  • step S2 the temperature of the reaction is 45-55° C., and the pH is 7.0-7.5.
  • the specific process of step S2 is: add cobalt salt solution and ammonium bicarbonate solution in parallel to the reactor containing nickel carbonate seeds, control the temperature at 45-55°C, and control the temperature by controlling the hydrogen carbonate
  • the flow rate of the ammonium solution maintains the pH of the reaction at 7.0-7.5.
  • the concentration is started.
  • the cobalt salt solution and ammonium bicarbonate solution are continuously fed in and the liquid level in the kettle is kept relatively stable until the particle size grows to the target. value, namely the described nickel-doped cobalt carbonate slurry.
  • the synthesis of nickel carbonate seed crystals and the growth of cobalt carbonate can be completed in the same reactor, and the reaction temperature is low, the energy consumption is low, and the synthesis efficiency is improved through the concentration process.
  • step S1 the particle size D50 of the nickel carbonate seed crystal is 2-5 ⁇ m, and in step S3, the particle size D50 of the nickel-doped cobalt carbonate is 8-20 ⁇ m. Further, the mass fraction of nickel in the nickel-doped cobalt carbonate is 0.1-2%.
  • the concentration of cobalt ions in the cobalt salt solution is 1.6-2.4mol/L, and the concentration of the ammonium bicarbonate solution is 2.0-3.0mol/L; preferably, The flow rate of the cobalt salt solution is 2-3L/h.
  • step S3 the washing is performed with hot pure water at 70-80°C for 10-30 minutes; preferably, the drying temperature is 100-110°C. Further, the moisture content of the dried material is lower than 1%.
  • step S3 sieving is performed after drying, and the mesh size of the sieve is 300-400.
  • the invention also provides a nickel-doped cobalt carbonate prepared by the preparation method.
  • the present invention also provides tricobalt tetroxide, which is prepared by thermal decomposition of the nickel-doped cobalt carbonate.
  • the thermal decomposition temperature is 600-800° C. and the time is 3-5 hours.
  • the present invention uses nickel salt and sodium carbonate to prepare spherical nickel carbonate crystal seed earlier, then adds cobalt salt and ammonium bicarbonate and prepares cobalt carbonate, finally obtained nickel-doped cobalt carbonate, and its advantage is: (1) avoids in carbonic acid During the co-precipitation of nickel and cobalt in the acid salt system, because the solubility product of nickel carbonate is much greater than that of cobalt carbonate, the precipitation of nickel is not complete, resulting in the loss of nickel in the supernatant; (2) sodium carbonate is used as the Precipitant, because sodium carbonate is a strong base and weak acid salt, it provides CO for the reaction 3 2- at the same time, it can also ensure that the system has a higher pH value, which is conducive to the uniform nucleation of nickel carbonate particles and the complete precipitation of nickel; (3 ) In the seed crystal growth stage, cobalt salt and ammonium bicarbonate are used as precipitants to ensure that the reaction proceeds smoothly, so that cobalt
  • the nickel-doped cobalt carbonate of the present invention can make the internal nickel element migrate outward after thermal decomposition, and obtain a precursor material of tricobalt tetroxide with uniform distribution of nickel element.
  • Fig. 1 is the SEM figure of 10000 times of nickel-doped cobalt carbonate of the embodiment of the present invention
  • Fig. 2 is the SEM picture of 20,000 times of nickel-doped cobalt carbonate in Example 1 of the present invention
  • Fig. 3 is the SEM picture of 10000 times of nickel-doped cobalt carbonate of embodiment 2 of the present invention.
  • Fig. 4 is the SEM picture of 20,000 times of nickel-doped cobalt carbonate in Example 2 of the present invention.
  • Fig. 5 is the SEM picture of 50,000 times of nickel-doped cobalt carbonate in Example 3 of the present invention.
  • Fig. 6 is the SEM picture of 10000 times of nickel-doped cobalt carbonate of embodiment 3 of the present invention.
  • Fig. 7 is the SEM picture of 50,000 times of nickel-doped cobalt carbonate in Example 4 of the present invention.
  • Fig. 8 is the SEM picture of 10,000 times of nickel-doped cobalt carbonate in Example 4 of the present invention.
  • Fig. 9 is the SEM figure of comparative example 1 cobalt carbonate 10000 times of the present invention.
  • Figure 10 is a cross-sectional view of nickel-doped cobalt tetroxide in Example 1 of the present invention.
  • Fig. 11 is a cross-sectional view of nickel-doped cobalt tetroxide in Example 2 of the present invention.
  • the present embodiment has prepared a kind of nickel-doped cobalt carbonate, and concrete process is:
  • Step 1 Preparation of solutions: 2.4 mol/L cobalt sulfate solution, 2.0 mol/L nickel sulfate solution, 3 mol/L ammonium bicarbonate solution, and 2.5 mol/L sodium carbonate solution were respectively prepared.
  • Preparation of spherical nickel carbonate seed crystals add pure water and sodium carbonate solution as the bottom liquid in the reaction kettle, the concentration of sodium carbonate in the bottom liquid is 0.5mol/L, the volume of the bottom liquid is based on submerging the bottom layer and stirring, the pH of the bottom liquid The value is 8.5, the temperature is 42°C, under the condition of high-speed stirring, add nickel sulfate solution and sodium carbonate solution concurrently, the flow rate of nickel sulfate solution is 3L/h, adjust the flow rate of sodium carbonate solution through the PLC control system to maintain the pH of the seed crystal synthesis stage The value is 8.0, co-flow for 20h, when the particle size grows to 5 ⁇ m, stop feeding, and obtain spherical nickel carbonate seeds.
  • Seed crystal growth the reaction temperature is raised to 55°C, and cobalt sulfate solution and ammonium bicarbonate solution are added in flow, wherein the flow rate of cobalt sulfate solution is 3L/h, and the flow rate of ammonium bicarbonate solution is regulated and maintained by the PLC control system to maintain the seed crystal
  • the pH is 7.0
  • the concentration is started, and the cobalt sulfate solution and ammonium bicarbonate solution are continuously introduced and the liquid level in the kettle is kept stable at 70-80% of the total volume until the particle size grows to 18.5 ⁇ m to obtain a nickel-doped cobalt carbonate slurry.
  • Step 3 Washing, drying, and screening of nickel-doped cobalt carbonate: put the slurry in the reaction kettle into a centrifuge for filtration, wash with 80°C hot pure water for 30 minutes, take the filter cake and dry it at 100°C until the moisture content is 0.3%. , passed through a 300-mesh vibrating sieve, and packed to obtain a nickel-doped cobalt carbonate finished product.
  • the particle size D50 of the nickel-doped cobalt carbonate finished product is 18.5 ⁇ m, and the mass fraction of nickel element is 1%.
  • Figures 1 and 2 are SEM images of 10,000 times and 20,000 times the nickel-doped cobalt carbonate prepared in this example, respectively. From the figures, it can be seen that the surface of the particles is piled up in the form of powder particles without fine powder.
  • the nickel-doped cobalt carbonate prepared in this example was finally fired into a lithium cobalt oxide positive electrode material, and the metal lithium sheet was used as the negative electrode.
  • the charge and discharge test of the button battery was carried out. When the charge and discharge voltage range was 3.0-4.55V, at a rate of 0.1C
  • the first discharge specific capacity is 213.2mAg/g, and the capacity retention rate after 50 cycles at 0.5C rate is 94.6%.
  • the present embodiment has prepared a kind of nickel-doped cobalt carbonate, and concrete process is:
  • Step 1 Preparation of solutions: 2.0 mol/L cobalt chloride solution, 1.8 mol/L nickel sulfate solution, 2.6 mol/L ammonium bicarbonate solution, and 2.0 mol/L sodium carbonate solution were respectively prepared.
  • Step 3 Washing, drying, and screening of nickel-doped cobalt carbonate: put the slurry in the reaction kettle into a centrifuge for filtration, wash with 80°C hot pure water for 30 minutes, take the filter cake and dry it at 105°C until the moisture content is 0.24%. , pass through a 350-mesh vibrating sieve, and get the nickel-doped cobalt carbonate finished product after packaging.
  • the particle size D50 of the nickel-doped cobalt carbonate finished product is 16.3 ⁇ m, and the mass fraction of nickel element is 0.8%.
  • Figures 3 and 4 are SEM images of 20,000 times and 10,000 times the nickel-doped cobalt carbonate prepared in this example, respectively. It can be seen from the figures that the surface of the particles is piled up in the form of powder, without fine powder.
  • the nickel-doped cobalt carbonate prepared in this example was finally fired into a lithium cobalt oxide positive electrode material, and the metal lithium sheet was used as the negative electrode.
  • the charge and discharge test of the button battery was carried out. When the charge and discharge voltage range was 3.0-4.55V, at a rate of 0.1C
  • the first discharge specific capacity is 212.8mAg/g, and the capacity retention rate after 50 cycles at 0.5C rate is 93.7%.
  • the present embodiment has prepared a kind of nickel-doped cobalt carbonate, and concrete process is:
  • Step 1 Preparation of solutions: 1.8 mol/L cobalt sulfate solution, 1.6 mol/L nickel chloride solution, 2.2 mol/L ammonium bicarbonate solution, and 1.8 mol/L sodium carbonate solution were respectively prepared.
  • Spherical nickel carbonate seed crystal preparation add pure water and sodium carbonate solution as the bottom liquid in the reaction kettle, the concentration of sodium carbonate in the bottom liquid is 1.0mol/L, the volume of the bottom liquid is based on submerging the bottom layer and stirring, the pH of the bottom liquid The value is 9.0, the temperature is 40°C, under the condition of high-speed stirring, nickel chloride solution and sodium carbonate solution are added in parallel, the flow rate of nickel chloride solution is 2.4L/h, and the flow rate of sodium carbonate solution is adjusted through the PLC control system to maintain the seed crystal In the synthesis stage, the pH value was 8.6, and the co-flow was 14 hours. When the particle size grew to 3 ⁇ m, the feeding was stopped to obtain spherical nickel carbonate seeds.
  • Seed crystal growth the reaction temperature is raised to 48°C, and cobalt sulfate solution and ammonium bicarbonate solution are added, wherein the cobalt sulfate solution flow rate is 2.4L/h, and the ammonium bicarbonate solution flow rate is regulated and maintained by the PLC control system.
  • the pH of the seed growth stage was 7.4.
  • the concentration is started, and the cobalt sulfate solution and the ammonium bicarbonate solution are continuously introduced to keep the liquid level in the kettle stable at 70-80% of the total volume until the particle size grows to 12 ⁇ m to obtain nickel-doped Cobalt Carbonate Slurry.
  • Step 3 Washing, drying, and screening of nickel-doped cobalt carbonate: put the slurry in the reaction kettle into a centrifuge for filtration, wash with hot pure water at 75°C for 20 minutes, take the filter cake and dry it at 110°C until the moisture content is 0.58% , pass through a 400-mesh vibrating sieve, and get the nickel-doped cobalt carbonate finished product after packaging.
  • the particle size D50 of the nickel-doped cobalt carbonate finished product is 12 ⁇ m, and the mass fraction of nickel element is 0.5%.
  • Figures 5 and 6 are SEM images of 50,000 times and 10,000 times the nickel-doped cobalt carbonate prepared in this example, respectively. It can be seen from the figures that the surface of the particles is piled up in blocks without fine powder.
  • the present embodiment has prepared a kind of nickel-doped cobalt carbonate, and concrete process is:
  • Step 1 Preparation of solutions: 1.6 mol/L cobalt chloride solution, 1.5 mol/L nickel chloride solution, 2.0 mol/L ammonium bicarbonate solution, and 1.5 mol/L sodium carbonate solution were respectively prepared.
  • Spherical nickel carbonate seed crystal preparation add pure water and sodium carbonate solution as the bottom liquid in the reaction kettle, the sodium carbonate concentration of the bottom liquid is 1.5mol/L, the volume of the bottom liquid is based on submerging the bottom layer and stirring, the pH of the bottom liquid The value is 9.5, the temperature is 38°C, under the condition of high-speed stirring, nickel chloride solution and sodium carbonate solution are added in parallel, the flow rate of nickel chloride solution is 2.0L/h, and the flow rate of sodium carbonate solution is adjusted through the PLC control system to maintain the seed crystal In the synthesis stage, the pH value is 8.8, and the co-flow is 10 hours. When the particle size grows to 2 ⁇ m, the feeding is stopped to obtain spherical nickel carbonate seeds.
  • Step 3 Washing, drying, and screening of nickel-doped cobalt carbonate: put the slurry in the reaction kettle into a centrifuge for filtration, wash with hot pure water at 75°C for 20 minutes, take the filter cake and dry it at 110°C until the moisture content is 0.84% , pass through a 400-mesh vibrating sieve, and get the nickel-doped cobalt carbonate finished product after packaging.
  • the particle size D50 of the nickel-doped cobalt carbonate product is 8 ⁇ m, and the mass fraction of nickel element is 1.2%.
  • Figures 7 and 8 are SEM images of 50,000 times and 10,000 times the nickel-doped cobalt carbonate prepared in this example, respectively. It can be seen from the figures that the SEM shows that the surface of the particles is piled up in blocks without fine powder.
  • This comparative example has prepared a kind of cobalt carbonate, and the seed crystal prepared by this comparative example is cobalt carbonate crystal seed, and concrete process is:
  • Step 1 Preparation of solutions: prepare 2.0 mol/L cobalt chloride solution and 3 mol/L ammonium bicarbonate solution respectively.
  • Cobalt carbonate seed crystal growth the reaction temperature is raised to 55°C, and cobalt chloride solution and ammonium bicarbonate solution are added in flow, wherein the cobalt chloride solution flow rate is 3L/h, and the ammonium bicarbonate solution flow rate is regulated by the PLC control system And maintain the pH of the seed crystal growth stage at 7.0, when the liquid level in the kettle reaches 70-80% of the total volume, the concentration is started, the cobalt chloride solution and the ammonium bicarbonate solution are continuously fed and the liquid level in the kettle is kept stable at 70-80% of the total volume %. Until the particle size grows to 18.5 ⁇ m, cobalt carbonate slurry is obtained.
  • Step 3 cobalt carbonate washing, drying, and sieving: filter the slurry in the reaction kettle to a centrifuge, wash with 80°C hot pure water for 30 minutes, take the filter cake and dry it at 100°C to a moisture content of 0.2%, and pass 400-mesh vibrating sieve, and the cobalt carbonate finished product is obtained after packaging.
  • the particle size D50 of the finished cobalt carbonate is 18.4 ⁇ m.
  • Fig. 9 is the SEM picture of 10000 times of the cobalt carbonate prepared in this comparative example, it can be seen from the picture that the surface of the particles is fine block accumulation.
  • the cobalt carbonate prepared in this comparative example is finally fired into a lithium cobalt oxide positive electrode material, and the metal lithium sheet is used as the negative electrode.
  • the charge and discharge test of the button battery is carried out. When the charge and discharge voltage range is 3.0-4.55V, the first discharge is performed at a rate of 0.1C The specific capacity is only 199.1mAg/g, and the capacity retention rate is 86.5% after 50 cycles at a rate of 0.5C.
  • Example 1-2 and Comparative Example 1 were calcined at 680°C for 4 hours to obtain tricobalt tetroxide, which was then made into a lithium cobalt oxide positive electrode material, and the metal lithium sheet was used as the negative electrode.
  • the charge and discharge test of the button battery was carried out.
  • the charge and discharge voltage range It is 3.0-4.55V, and its electrochemical performance is shown in Table 1.
  • the first discharge specific capacity at 0.1C rate is 213.2mAh/g, and the capacity retention rate after 50 cycles at 0.5C rate is 94.6%.
  • Figure 10 is a cross-sectional view of nickel-doped cobalt tetroxide in Example 1.
  • the five rectangular areas of the cross-section were scanned by EDS, and the corresponding test results are shown in Table 2. The results show that the nickel element is uniformly distributed inside the particles.
  • Figure 11 is a cross-sectional view of nickel-doped cobalt tetroxide in Example 2.
  • the five rectangular areas of the cross-section were scanned by EDS, and the corresponding test results are shown in Table 3. The results show that the nickel element is uniformly distributed inside the particles.

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Abstract

Un carbonate de cobalt dopé au nickel, son procédé de préparation et son utilisation sont divulgués dans la présente invention. Le procédé consiste à : mélanger une première solution de carbonate et une solution de sel de nickel pour les faire réagir, et commander la température et le pH pour obtenir un germe de carbonate de nickel, le premier carbonate étant un ou deux parmi le carbonate de sodium ou le carbonate de potassium ; mélanger le germe de carbonate de nickel, une solution de sel de cobalt et une solution de bicarbonate d'ammonium pour les faire réagir, et commander la température et le pH pour obtenir une bouillie de carbonate de cobalt dopé au nickel ; et soumettre la bouillie de carbonate de cobalt dopé au nickel à une séparation solide-liquide, et la laver et sécher pour obtenir un carbonate de cobalt dopé au nickel. Selon la présente invention, un germe de carbonate de nickel est d'abord préparé en utilisant un sel de nickel et du carbonate de sodium, un sel de cobalt et du bicarbonate d'ammonium sont ensuite ajoutés à celui-ci pour préparer du carbonate de cobalt, et le carbonate de cobalt dopé au nickel est finalement obtenu ; et lorsque le carbonate de cobalt dopé au nickel est soumis à une décomposition thermique, le nickel interne peut migrer vers l'extérieur de façon à obtenir un matériau précurseur d'oxyde cobaltosique avec du nickel uniformément distribué à l'intérieur de celui-ci.
PCT/CN2022/092471 2021-08-26 2022-05-12 Carbonate de cobalt dopé au nickel, son procédé de préparation et son utilisation Ceased WO2023024584A1 (fr)

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