WO2014077662A1 - Procédé permettant de produire un précurseur de matière active d'anode pour batterie secondaire au sodium en utilisant une technique de coprécipitation et précurseur de matière active d'anode pour batterie secondaire au sodium produite ainsi - Google Patents
Procédé permettant de produire un précurseur de matière active d'anode pour batterie secondaire au sodium en utilisant une technique de coprécipitation et précurseur de matière active d'anode pour batterie secondaire au sodium produite ainsi Download PDFInfo
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- WO2014077662A1 WO2014077662A1 PCT/KR2013/010520 KR2013010520W WO2014077662A1 WO 2014077662 A1 WO2014077662 A1 WO 2014077662A1 KR 2013010520 W KR2013010520 W KR 2013010520W WO 2014077662 A1 WO2014077662 A1 WO 2014077662A1
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- secondary battery
- active material
- sodium secondary
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
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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
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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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
- C01P2006/40—Electric properties
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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 relates to a method for producing a cathode active material precursor for a sodium secondary battery using a coprecipitation method and a cathode active material precursor for a sodium secondary battery produced thereby.
- a lithium ion secondary battery using a nonaqueous electrolyte solution in which an electrolyte salt is dissolved in a nonaqueous solvent and moving lithium ions between a positive electrode and a negative electrode so that charge and discharge is performed is widely used.
- Lithium ion batteries using an intercalation reaction of lithium ions using lithium transition metal oxides are commercially available as positive electrode materials.
- lithium included in the lithium ion battery is expensive, there is a need for a battery having a lower cost and a higher capacity.
- Japanese Unexamined Patent Application Publication No. 2007-287661 has a positive electrode made of a composite metal oxide obtained by firing a raw material having a composition ratio of Na, Mn and Co (Na: Mn: Co) of 0.7: 0.5: 0.5 and a negative electrode made of sodium metal. Secondary batteries are described in detail. Further, Japanese Patent Laid-Open No. 2005-317511 discloses ⁇ -NaFeO 2 having a hexagonal crystal (layered rock salt) crystal structure as a sum metal oxide, specifically, by mixing Na 2 O 2 and Fe 3 O 4 . This composite metal oxide was obtained by baking at 600-700 degreeC in air. However, the conventional sodium secondary battery cannot be said to have sufficient lifespan characteristics, that is, a discharge capacity retention rate when repeated charging and discharging.
- the most common manufacturing method for producing a cathode active material of a lithium secondary battery or a sodium secondary battery is a solid phase reaction method, which is performed by mixing and firing powders of the carbonate or hydroxide of each element several times.
- the solid-phase reaction method has a disadvantage in that it is difficult to form a solid solution of solid phases and inflow of impurities during mixing, it is difficult to control the size of the particles uniformly, and high temperature and manufacturing time are long in manufacturing.
- the coprecipitation method of wet method has the advantage that the element can be controlled to the atomic range, and the spherical metal composite carbonate can be produced.
- a solid state reaction method was mainly applied, and a method of manufacturing a cathode active material of a sodium secondary battery by applying a coprecipitation method has not been studied.
- An object of the present invention is to provide a method for producing a cathode active material precursor for sodium secondary batteries using a coprecipitation method in order to solve the problems of the prior art as described above.
- Another object of the present invention is to provide a cathode active material precursor for a sodium secondary battery of a novel composition prepared by the manufacturing method of the present invention and having improved life characteristics.
- the present invention to solve the above problems
- It provides a method for producing a cathode active material precursor for a sodium secondary battery using a coprecipitation method comprising a.
- the first pH adjusting agent in the step (a) is characterized in that the aqueous ammonia solution or ammonium sulfate solution.
- the second pH adjusting agent in step (b) is characterized in that selected from the group consisting of ammonium oxalate, KOH, and NaOH.
- the pH in the reactor is adjusted to 9 to 11 when KOH or NaOH is added as the second pH adjusting agent.
- the pH in the reactor is adjusted to 6.5 to 11.
- the nickel salt in the step (c) is selected from the group consisting of nickel sulfate, nickel nitrate, nickel chloride, nickel fluoride, nickel acetate and nickel hydroxide.
- the iron salt is selected from the group consisting of iron sulfate, iron nitrate, iron chloride, iron fluoride, iron acetate, and iron hydroxide
- the manganese salt is manganese sulfate, manganese nitrate, manganese chloride, manganese fluoride, manganese acetate, and manganese hydroxide It is characterized by being selected from the group consisting of.
- the complexing agent in the step (c) is an aqueous ammonia solution (NH 4 OH), ammonium sulfate ((NH 4 ) 2 SO 4 ), ammonium nitrate ( NH 4 NO 3 ) and first ammonium phosphate ((NH 4 ) 2 HPO 4 ).
- the ratio of the concentration of the complexing agent in the step (c) and the concentration of the aqueous solution of the transition metal compound is characterized in that 0.8 to 1.2.
- the present invention also provides a cathode active material precursor for a sodium secondary battery, which is prepared by the production method of the present invention, and has a spherical particle size of 5 to 15 ⁇ m and a particle size distribution of a monodisperse type.
- the positive electrode active material precursor according to the invention is characterized by represented by Ni x Fe y Mn 1-xy (OH) 2 (0.1 ⁇ x ⁇ 0.3, 0.2 ⁇ y ⁇ 0.7, 0.1 ⁇ 1-xy ⁇ 0.5) do.
- the positive electrode active material precursor according to the invention is characterized by represented by Ni x Fe y Mn 1-xy C 2 O 4 (0.1 ⁇ x ⁇ 0.3, 0.2 ⁇ y ⁇ 0.7, 0.1 ⁇ 1-xy ⁇ 0.5) do.
- the positive electrode active material precursor according to the invention is characterized in that which is represented by [Ni x Fe y Mn 1- xy] 3 O 4 (0.1 ⁇ x ⁇ 0.3, 0.2 ⁇ y ⁇ 0.7, 0.1 ⁇ 1-xy ⁇ 0.5) It is done.
- the present invention also provides a cathode active material for sodium secondary battery prepared using the cathode active material precursor for sodium secondary battery according to the present invention and a sodium secondary battery comprising the same.
- the method for preparing a cathode active material precursor for a sodium secondary battery using the coprecipitation method according to the present invention may provide a cathode active material precursor for a sodium secondary battery having a new composition having improved life characteristics by appropriately adjusting the type and pH of the complexing agent while using the coprecipitation method. Can be.
- 1 to 4 show SEM pictures of the precursor prepared in the embodiment of the present invention.
- 5 to 8 show the results of measuring the particle size distribution of the precursor prepared in the embodiment of the present invention.
- Figure 11 shows the results of measuring the particle size distribution of the precursor prepared in the embodiment of the present invention.
- 16 to 21 show the results of XRD measurements on the positive electrode active material prepared in one embodiment of the present invention.
- NiSO 4 ⁇ 6H 2 O, FeSO 4 ⁇ 7H 2 O, MnSO 4 ⁇ 5H 2 O as an aqueous solution of a transition metal compound were mixed in an equivalent ratio, and introduced into the reactor together with NH 4 OH as a complexing agent, as shown in Table 1 below.
- a precursor of the composition was prepared.
- Example 1 Ni 0.25 Fe 0.25 Mn 0.5 (OH) 2
- Example 2 Ni 0.25 Fe 0.35 Mn 0.4 (OH) 2
- Example 3 Ni 0.25 Fe 0.5 Mn 0.25 (OH) 2
- Example 4 Ni 0.15 Fe 0.35 Mn 0.5 (OH) 2
- Example 5 Ni 0.25 Fe 0.5 Mn 0.25 C 2 O 4
- Example 6 Ni 0.2 Fe 0.6 Mn 0.2 C 2 O 4
- Example 7 Ni 0.17 Fe 0.66 Mn 0.17 C 2 O 4
- Example 8 Ni 0.2 Fe 0.55 Mn 0.25 C 2 O 4
- Example 9 Ni 0.3 Fe 0.45 Mn 0.25 C 2 O 4
- Example 10 Ni 0.35 Fe 0.4 Mn 0.25 C 2 O 4
- Example 11 Ni 0.4 Fe 0.35 Mn 0.25 C 2 O 4
- Example 12 Ni 0.45 Fe 0.3 Mn 0.25 C 2 O 4, Example 13 (Ni 0.25 Fe 0.5 Mn 0.25 ) 3 O 4
- Example 14 (Ni 0.25 Fe 0.25 Mn 0.5 ) 3 O 4
- the particle size distribution of the precursors prepared in Examples 1 to 4 was measured and shown in FIGS. 5 to 8. 5 to 8 it can be seen that the particle size distribution of the precursor particles prepared according to the embodiment of the present invention is monodisperse.
- Example 1 As in Example 1, except that the pH inside the reactor was adjusted to 7 using an aqueous ammonia solution as the first pH adjusting agent, and the pH inside the reactor was adjusted to 7 using an aqueous 0.5M ammonium oxalate solution as the second pH adjusting agent.
- Example 1 To prepare a precursor of Examples 5 to 12 of the composition as shown in Table 1.
- XRDs of the precursors prepared in Examples 5 to 7 were measured and shown in FIG. 9.
- XRD of the precursors prepared in Examples 5 and 8 to 12 were measured and shown in FIG. 10.
- Particle size distribution of the precursors prepared in Examples 5 to 7 was measured and shown in FIG. 11.
- Example 13 As in Example 1, except that the pH inside the reactor was adjusted to 7 using an aqueous ammonia solution as the first pH regulator, and the pH inside the reactor was adjusted to 9.2 by adding 4 M NaOH as the second pH regulator (The precursors of Examples 13 and 14 represented by Ni 0.25 Fe 0.5 Mn 0.25 ) 3 O 4 and (Ni 0.25 Fe 0.25 Mn 0.5 ) 3 O 4 were prepared.
- Particle size distribution of the precursors prepared in Examples 8 and 9 were measured and shown in FIGS. 14 and 15. It can be seen from FIG. 14 and FIG. 15 that the particle size distribution is monodisperse.
- FIGS. 16 to 21 XRD of the cathode active materials prepared in Examples 15 to 28 is shown in FIGS. 16 to 21.
- FIG. 22 shows XRD results of the cathode active materials prepared in Examples 19 and 22 to 26.
- the composite metal oxide and acetylene black are sufficiently mixed with an agate mortar, and N-methyl-2-pyrrolidone (NMP: manufactured by Tokyo Kasei Kogyo Co., Ltd.) is appropriately added to the mixture, followed by addition.
- PVDF was added to the mixture to make it uniform and slurryed.
- FEC Fluoro Ethylene Carbonate
- a polypropylene porous membrane thinness 20 ⁇ m
- Table 2 shows the results of measuring the charge and discharge characteristics of the sodium secondary battery including the active material of Examples 15 to 22 made of the precursors of Examples 1 to 8.
- Example 15 Ni 0.25 Fe 0.25 Mn 0.5 (OH) 2 Precursor / Na 95%, sintered at 970 ° C / 24h, 4.3V 155.5 mAh / g 94.1%
- Example 2 Ni 0.25 Fe 0.35 Mn 0.4 (OH) 2 Precursor / Na 98%, 900 ° C / 24h Sintered, 4.3V 180.1 mAh / g 101.2% Ni 0.25 Fe 0.35 Mn 0.4 (OH) 2 Precursor / Na 98%, 930 ° C / 24h Sintered, 4.3V 176.3 mAh / g 100.9% Ni 0.25 Fe 0.35 Mn 0.4 (OH) 2 Precursor / Na 98%, Sintered at 970 ° C / 24h, 4.3V 166.2 mAh / g 95.4%
- Example 3 Example 17 Ni 0.25 Fe 0.5 Mn 0.25 (OH) 2 Precursor / Na 95%, sintered at 970 ° C / 24h, 4.3V 166.2 mAh
- the battery containing the active material prepared using the sodium battery cathode active material precursor prepared according to the present invention can be seen that the initial charge and discharge efficiency is 90% or more.
- Table 3 shows the results of measuring the charge and discharge characteristics of the sodium secondary battery including the active materials of Examples 15 to 18 and Example 22 prepared by using the precursors prepared in Examples 1 to 4, and Example 8.
- Example 15 155.5 mAh / g 130.2 mAh / g 83.7% 106.9 mAh / g 96.0 mAh / g 89.8%
- Example 2 Example 16 180.1 mAh / g 141.3 mAh / g 78.5% 125.6 mAh / g 117.5 mAh / g 93.6% 176.3 mAh / g 140.5 mAh / g 76.7% 125.9 mAh / g 117.8 mAh / g 93.6% 166.2 mAh / g 124.6 mAh / g 75.0% 107.7 mAh / g 95.1 mAh / g 88.3%
- Example 3 Example 17 130.7 mAh / g 122.0 mAh / g 93.3% 114.3 mAh / g 105.4 mAh / g 92
- the method for preparing a cathode active material precursor for a sodium secondary battery using the coprecipitation method according to the present invention may provide a cathode active material precursor for a sodium secondary battery having a new composition having improved life characteristics by appropriately adjusting the type and pH of the complexing agent while using the coprecipitation method. Can be.
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Abstract
La présente invention concerne un procédé permettant de produire un précurseur de matière active d'anode pour une batterie secondaire au sodium en utilisant une technique de coprécipitation et un précurseur de matière active d'anode pour une batterie secondaire au sodium produite ainsi. Le procédé permettant de produire un précurseur de matière active d'anode pour une batterie secondaire au sodium en utilisant une technique de coprécipitation selon la présente invention peut fournir un précurseur de matière active d'anode, présentant des caractéristiques de durée de vie améliorées et une nouvelle composition, pour une batterie secondaire au sodium en adaptant de manière appropriée les types d'agents complexants tout en utilisant une technique de coprécipitation.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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CN201380068776.0A CN104885265B (zh) | 2012-11-19 | 2013-11-19 | 利用共沉淀法的钠二次电池用正极活性材料前驱体的制备方法及由此制备的钠二次电池用正极活性材料前驱体 |
US14/716,362 US20150333325A1 (en) | 2012-11-19 | 2015-05-19 | Manufacturing method of positive active material precursor for sodium rechargeable batteries, positive active material precursor for sodium rechargeable batteries made by the same, and manufacturing method of positive active material for sodium rechargeable batteries, positive active material for sodium rechargeable batteries made by the same |
US15/993,174 US10781110B2 (en) | 2012-11-19 | 2018-05-30 | Manufacturing method of positive active material precursor for sodium rechargeable batteries, positive active material precursor for sodium rechargeable batteries made by the same, and manufacturing method of positive active material for sodium rechargeable batteries, positive active material for sodium rechargeable batteries made by the same |
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KR20120130824 | 2012-11-19 | ||
KR10-2012-0130824 | 2012-11-19 | ||
KR10-2013-0140907 | 2013-11-19 | ||
KR1020130140907A KR101570125B1 (ko) | 2012-11-19 | 2013-11-19 | 공침법을 이용한 나트륨 이차전지용 양극활물질 전구체의 제조 방법 및 이에 의하여 제조된 나트륨 이차전지용 양극활물질 전구체 |
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PCT/KR2013/010521 Continuation-In-Part WO2014077663A1 (fr) | 2012-11-19 | 2013-11-19 | Matériau actif d'anode pour pile secondaire au sodium et son procédé de fabrication |
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US14/716,362 Continuation-In-Part US20150333325A1 (en) | 2012-11-19 | 2015-05-19 | Manufacturing method of positive active material precursor for sodium rechargeable batteries, positive active material precursor for sodium rechargeable batteries made by the same, and manufacturing method of positive active material for sodium rechargeable batteries, positive active material for sodium rechargeable batteries made by the same |
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Cited By (8)
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---|---|---|---|---|
WO2017017944A1 (fr) * | 2015-07-24 | 2017-02-02 | Sharp Kabushiki Kaisha | Composés d'oxydes de métaux de transition à base de sodium pour batteries na-ion |
US10781110B2 (en) | 2012-11-19 | 2020-09-22 | Iucf-Hyu(Industry-University Cooperation Foundation Hanyang University) | Manufacturing method of positive active material precursor for sodium rechargeable batteries, positive active material precursor for sodium rechargeable batteries made by the same, and manufacturing method of positive active material for sodium rechargeable batteries, positive active material for sodium rechargeable batteries made by the same |
CN114920306A (zh) * | 2022-06-29 | 2022-08-19 | 荆门市格林美新材料有限公司 | 正极材料前驱体、正极材料、其制备方法和钠离子电池 |
CN114956202A (zh) * | 2022-04-28 | 2022-08-30 | 南通金通储能动力新材料有限公司 | 一种钠离子正极材料的前驱体、制备方法及正极材料 |
CN115196691A (zh) * | 2022-07-18 | 2022-10-18 | 宿迁市翔鹰新能源科技有限公司 | 一种钠离子电池用镍铁锰三元前驱体及其制备方法和应用 |
CN116102078A (zh) * | 2022-11-11 | 2023-05-12 | 泾河新城陕煤技术研究院新能源材料有限公司 | 高振实钠电前驱体的制备方法 |
CN116375111A (zh) * | 2023-06-06 | 2023-07-04 | 宜宾锂宝新材料有限公司 | 一种钠离子电池及其正极材料与前驱体和制备方法 |
CN116621234A (zh) * | 2023-07-20 | 2023-08-22 | 宜宾光原锂电材料有限公司 | 一种钠离子正极材料前驱体及制备方法和正极材料 |
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10781110B2 (en) | 2012-11-19 | 2020-09-22 | Iucf-Hyu(Industry-University Cooperation Foundation Hanyang University) | Manufacturing method of positive active material precursor for sodium rechargeable batteries, positive active material precursor for sodium rechargeable batteries made by the same, and manufacturing method of positive active material for sodium rechargeable batteries, positive active material for sodium rechargeable batteries made by the same |
WO2017017944A1 (fr) * | 2015-07-24 | 2017-02-02 | Sharp Kabushiki Kaisha | Composés d'oxydes de métaux de transition à base de sodium pour batteries na-ion |
CN114956202B (zh) * | 2022-04-28 | 2023-11-14 | 南通金通储能动力新材料有限公司 | 一种钠离子正极材料的前驱体、制备方法及正极材料 |
CN114956202A (zh) * | 2022-04-28 | 2022-08-30 | 南通金通储能动力新材料有限公司 | 一种钠离子正极材料的前驱体、制备方法及正极材料 |
CN114920306A (zh) * | 2022-06-29 | 2022-08-19 | 荆门市格林美新材料有限公司 | 正极材料前驱体、正极材料、其制备方法和钠离子电池 |
CN114920306B (zh) * | 2022-06-29 | 2024-03-26 | 荆门市格林美新材料有限公司 | 正极材料前驱体、正极材料、其制备方法和钠离子电池 |
CN115196691A (zh) * | 2022-07-18 | 2022-10-18 | 宿迁市翔鹰新能源科技有限公司 | 一种钠离子电池用镍铁锰三元前驱体及其制备方法和应用 |
CN116102078A (zh) * | 2022-11-11 | 2023-05-12 | 泾河新城陕煤技术研究院新能源材料有限公司 | 高振实钠电前驱体的制备方法 |
CN116102078B (zh) * | 2022-11-11 | 2023-08-18 | 泾河新城陕煤技术研究院新能源材料有限公司 | 高振实钠电前驱体的制备方法 |
CN116375111A (zh) * | 2023-06-06 | 2023-07-04 | 宜宾锂宝新材料有限公司 | 一种钠离子电池及其正极材料与前驱体和制备方法 |
CN116375111B (zh) * | 2023-06-06 | 2023-09-01 | 宜宾锂宝新材料有限公司 | 一种钠离子电池及其正极材料与前驱体和制备方法 |
CN116621234B (zh) * | 2023-07-20 | 2023-11-07 | 宜宾光原锂电材料有限公司 | 一种钠离子正极材料前驱体及制备方法和正极材料 |
CN116621234A (zh) * | 2023-07-20 | 2023-08-22 | 宜宾光原锂电材料有限公司 | 一种钠离子正极材料前驱体及制备方法和正极材料 |
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