WO2010139125A1 - 一种纳米级锂电池正极材料及其制备方法 - Google Patents
一种纳米级锂电池正极材料及其制备方法 Download PDFInfo
- Publication number
- WO2010139125A1 WO2010139125A1 PCT/CN2009/072394 CN2009072394W WO2010139125A1 WO 2010139125 A1 WO2010139125 A1 WO 2010139125A1 CN 2009072394 W CN2009072394 W CN 2009072394W WO 2010139125 A1 WO2010139125 A1 WO 2010139125A1
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- Prior art keywords
- powder
- positive electrode
- lithium battery
- electrode material
- nano
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Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
- H01M4/5825—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- Nano-scale lithium battery cathode material and preparation method thereof are nano-scale lithium battery cathode material and preparation method thereof.
- the present invention relates to a nano-scale lithium battery positive electrode material and a preparation method thereof for use in a polymer, a colloidal and a liquid lithium ion battery, and is particularly suitable for producing a high-powered power battery.
- Lithium cobaltate and lithium nickel cobaltate are oxides of a hexagonal layered rock salt structure.
- the electrons in lithium ions move in the octahedral gap formed by 0-Co-0, which has high conductivity and lithium ion deintercalation. / Embedding reversibility.
- Lithium manganate is an oxide of three-dimensional structure of spinel. Electrons in lithium ions move in an octahedral cubic channel composed of 0-Mn-0, and also have high electrical conductivity and lithium ion deintercalation/embedded reversibility.
- lithium cobaltate and lithium nickel cobaltate are expensive to manufacture and have poor safety.
- lithium manganate is cheaper and safer, it has a small capacitance and a poor cycle life under high temperature conditions (above 55 °C). Even after doping and surface chemical treatment, the cycle life of lithium manganate batteries cannot meet the actual requirements. Therefore, the lithium battery industry, especially high-power lithium batteries, urgently needs a cathode material that is low in cost, environmentally friendly, large in capacity, and safe.
- lithium iron phosphate polycrystal When 1 mole of lithium ions are deintercalated from the structure, the theoretical discharge capacity of the lithium iron phosphate polycrystal can reach 170 mAh/g. Due to the abundant reserves of lithium and iron, the production cost of lithium iron phosphate is low. This paper predicts that lithium iron phosphate materials may have broad application prospects in the battery industry due to their low cost, environmental protection, high performance and safety. However, very low electrical conductivity of lithium iron phosphate (10- 9 S / cm) at room temperature under normal discharge current (lO ⁇ mA / cm 2) conditions of actual discharge capacity of lithium iron phosphate is only a theoretical value ( 10% of 170 mAh/g). Therefore, its application in the battery is limited.
- the object of the present invention is to provide a nano-scale lithium battery cathode material with lithium iron phosphate as a base material, which is further doped with conductive doping ions and pressurized doping ions, and a preparation method thereof, to overcome the above-mentioned problems existing in the prior art. defect.
- the above-mentioned nano-sized lithium battery positive electrode material has a particle diameter of 40 to 80 nm.
- the invention also provides a preparation method of a nano-scale lithium battery positive electrode material, the method adopting a solid phase reaction, comprising the following steps:
- a lithium dihydrogen phosphate, ferrous ferrous sulfate, glucose and a conductive dopant and a pressurized dopant are uniformly mixed and then pulverized into powder;
- the temperature is raised to 200 to 400 ° C in an inert gas atmosphere for 2 to 3 hours;
- the temperature is raised to 500 to 780 ° C in an inert gas atmosphere for 15 20 hours;
- step e The powder obtained in step e is subjected to ultrafine gas flow pulverization and classification.
- the conductive dopant is Mg 2+ , Ca 2+ , Sr 2+ , Ti 2+ , Al 3+ , B 3+ , Ce 3+ , C 4+ , Si 4+ , Ge 4+ or P 5+ A compound or a combination of any two or more.
- the conductive dopant is added in an amount of:
- the number of moles of the conductive dopant ions is 4 to 10% of the sum of the number of moles of lithium ions and the number of moles of conductive dopant ions.
- the pressurized dopant is an oxide, carbonate, sulfide or oxide of Ti 2+ , V 5+ , Co 3+ , Ni 3+ , Mn 2+ , Cr 3+ , Cu 2+ or Mo 4+ Phosphate or a combination of any two or more.
- the amount of the pressurized dopant added is:
- the number of moles of the pressurized dopant ions is 3 to 7% of the sum of the number of moles of iron ions and the number of moles of pressurized dopant ions.
- the nanometer lithium battery positive electrode material provided by the invention adds a positive ion having a small atomic weight and a high polarizability as a conductive doping ion, and the conductivity of the lithium iron phosphate positive electrode material is from 3 l (r 9 S/cm).
- the present invention also provides a preparation method of the above-mentioned nano-scale lithium battery positive electrode material, which has low production cost, simple operation method, and no production. Characteristics of high pollution and yield ( > 99%).
- Figure 1 Scanning electron micrograph of the nano-scale lithium battery cathode material, magnification: 10,000 times; scale: 2.0 ⁇ .
- the material has a particle diameter of 40 to 80 nm.
- Figure 2 Charging and discharging characteristics of a lithium battery made of a nano-scale lithium battery cathode material.
- Figure 3 X-ray diffraction pattern of a nano-scale lithium battery cathode material.
- the powder prepared in the first step is granulated, placed in an alumina ceramic crucible, heated to 200-300 ° C in a nitrogen furnace, and sintered at a constant temperature for 3 hours;
- the third step after cooling to room temperature, take out, ball-mill into powder, and mix evenly;
- the temperature is raised to 500 to 600 ° C in a nitrogen furnace, and the temperature is sintered for 18 to 20 hours to form a doped lithium iron phosphate crystal, which naturally falls to room temperature;
- the crystal particles are crushed into a powder form;
- the powder prepared in the fifth step is crushed and classified on a superfine jet mill to prepare a nano-scale lithium battery positive electrode material having a particle diameter of 40 to 80 nm.
- the conductivity of the ordinary lithium iron phosphate positive electrode material is 3 x 10 - 9 S / cm, and the room temperature discharge voltage is 3.2 V; and the room temperature conductivity and the room temperature discharge voltage of the nano-scale lithium battery positive electrode material provided in this embodiment are respectively 1.30 X l (r 2 S/cm and 4.0 V, respectively increased by 10 7 times and 25%.
- Example 2
- the powder prepared in the first step is granulated, placed in an alumina ceramic crucible, heated to 300-400 ° C in a nitrogen furnace, and heated at a constant temperature for 1.5-2.5 hours;
- the third step after cooling to room temperature, take out, ball-mill into powder, and stir evenly;
- the temperature is further increased to 700-800 ° C in a nitrogen furnace, and the temperature is sintered for 15 16 hours to form a doped lithium iron phosphate crystal, which is naturally cooled to room temperature;
- the crystal particles are crushed into a powder form
- the powder prepared in the fifth step is crushed and classified on a superfine jet mill to form a solid powder for the positive electrode of the lithium battery, and the powder particles have a diameter of 40 to 80 nm.
- the conductivity of the ordinary lithium iron phosphate positive electrode material is 3 x 10 - 9 S / cm, and the room temperature discharge voltage is 3.2 V; and the room temperature conductivity and the room temperature discharge voltage of the nano-scale lithium battery positive electrode material provided in this embodiment are respectively It is 1.75 X 10" 2 S/cm and 3.85V, which is increased by 10 7 times and 20%, respectively.
- the powder prepared in the first step is granulated, placed in an alumina ceramic crucible, heated to 200-300 ° C in a nitrogen furnace, and sintered at a constant temperature for 2 to 3 hours;
- the third step after cooling to room temperature, take out, ball-mill into powder, and stir evenly;
- the fourth step after the powder obtained in the third step is granulated, the temperature is further increased to 650-750 ° C in a nitrogen furnace, and the temperature is sintered for 16 17 hours to form a doped nano lithium iron phosphate crystal, which is naturally cooled to room temperature;
- the crystal particles are crushed into a powder form
- the powder prepared in the fifth step is crushed and classified on a superfine jet mill to form a solid powder of a nano-scale lithium battery positive electrode material, and the particle diameter is 40 to 80 nm.
- the conductivity of the ordinary lithium iron phosphate positive electrode material is 3 x 10 - 9 S / cm, and the room temperature discharge voltage is 3.2 V; and the room temperature conductivity and the room temperature discharge voltage of the nano-scale lithium battery positive electrode material provided in this embodiment are respectively The ratio of 1.35 X 10" 2 S/cm and 3.90 V is increased by 10 7 times and 22%, respectively.
- the nano-scale lithium battery positive electrode materials provided in Examples 1, 2 and 3 of the present invention can be rapidly charged and discharged at a rate of 1 C 9C.
- the present invention includes, but is not limited to, the above embodiments. The specific embodiments described above are only for understanding the essence of the present invention, and the modifications made to the present invention according to the prior art without departing from the essence of the present invention are still within the scope of protection of the present invention. .
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2009347499A AU2009347499B2 (en) | 2009-06-02 | 2009-06-23 | Nano-Positive Electrode Material Of Lithium Cell And Method For Preparation Thereof |
EP09838542.0A EP2287944B1 (en) | 2009-06-02 | 2009-06-23 | Nanometer-level positive electrode material for lithium battery and method for making the same |
JP2011537823A JP5347031B2 (ja) | 2009-06-02 | 2009-06-23 | リチウム電池用ナノ正極材料及びその製造方法 |
US12/865,357 US8470207B2 (en) | 2009-06-02 | 2009-06-23 | Nano-positive electrode material of lithium cell and method for preparation thereof |
RU2011126090/07A RU2477908C2 (ru) | 2009-06-02 | 2009-06-23 | Наноматериал положительного электрода литиевого элемента и способ его получения |
HK11103875.1A HK1150096A1 (zh) | 2009-06-02 | 2011-04-18 | 種納米級鋰電池正極材料及其製備方法 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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CN200910143905.3 | 2009-06-02 | ||
CN2009101439053A CN101567449B (zh) | 2009-06-02 | 2009-06-02 | 一种纳米级锂电池正极材料及其制备方法 |
Publications (1)
Publication Number | Publication Date |
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WO2010139125A1 true WO2010139125A1 (zh) | 2010-12-09 |
Family
ID=41283507
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Application Number | Title | Priority Date | Filing Date |
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PCT/CN2009/072394 WO2010139125A1 (zh) | 2009-06-02 | 2009-06-23 | 一种纳米级锂电池正极材料及其制备方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US8470207B2 (zh) |
EP (1) | EP2287944B1 (zh) |
JP (1) | JP5347031B2 (zh) |
CN (1) | CN101567449B (zh) |
AU (1) | AU2009347499B2 (zh) |
HK (1) | HK1150096A1 (zh) |
RU (1) | RU2477908C2 (zh) |
WO (1) | WO2010139125A1 (zh) |
Cited By (2)
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CN109665508A (zh) * | 2017-10-16 | 2019-04-23 | 中天新兴材料有限公司 | 正极材料磷酸铁锂及其制备方法 |
CN115417394A (zh) * | 2022-09-20 | 2022-12-02 | 广西自贸区量孚新能源科技有限公司 | 一种磷酸铁锂材料及其制备工艺和应用 |
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CN101567449B (zh) * | 2009-06-02 | 2012-06-27 | 徐瑞松 | 一种纳米级锂电池正极材料及其制备方法 |
JPWO2011138964A1 (ja) * | 2010-05-06 | 2013-07-22 | 旭硝子株式会社 | ケイ酸−リン酸化合物、二次電池用正極、および二次電池の製造方法 |
CN101841027A (zh) * | 2010-05-13 | 2010-09-22 | 湘西自治州矿产与新材料技术创新服务中心 | 锂离子电池锂位稀土掺杂磷酸氧钒锂正极材料的制备方法 |
US20120003139A1 (en) * | 2010-06-30 | 2012-01-05 | Semiconductor Energy Laboratory Co., Ltd. | Method for manufacturing power storage device |
KR101965016B1 (ko) * | 2011-07-25 | 2019-04-02 | 에이일이삼 시스템즈, 엘엘씨 | 블렌딩된 캐소드 물질 |
CN102364733B (zh) * | 2011-10-26 | 2013-02-13 | 黄景诚 | 锑、钡活化磷酸铁锂正极材料制备方法 |
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RU2623212C1 (ru) * | 2016-07-12 | 2017-06-23 | Федеральное государственное бюджетное учреждение науки Институт общей и неорганической химии им. Н.С. Курнакова Российской академии наук (ИОНХ РАН) | Композиционный катодный материал |
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CN112088897B (zh) * | 2020-09-23 | 2021-10-22 | 大连海事大学 | 一种纳米氧化镁无机抗菌剂及其制备方法 |
CN116101990B (zh) * | 2022-09-07 | 2024-05-10 | 浙江华友钴业股份有限公司 | 磷酸铁和磷酸铁锂及其制备方法、电极及电池 |
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- 2009-06-02 CN CN2009101439053A patent/CN101567449B/zh active Active
- 2009-06-23 WO PCT/CN2009/072394 patent/WO2010139125A1/zh active Application Filing
- 2009-06-23 US US12/865,357 patent/US8470207B2/en not_active Expired - Fee Related
- 2009-06-23 JP JP2011537823A patent/JP5347031B2/ja active Active
- 2009-06-23 AU AU2009347499A patent/AU2009347499B2/en active Active
- 2009-06-23 EP EP09838542.0A patent/EP2287944B1/en active Active
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109665508A (zh) * | 2017-10-16 | 2019-04-23 | 中天新兴材料有限公司 | 正极材料磷酸铁锂及其制备方法 |
CN115417394A (zh) * | 2022-09-20 | 2022-12-02 | 广西自贸区量孚新能源科技有限公司 | 一种磷酸铁锂材料及其制备工艺和应用 |
CN115417394B (zh) * | 2022-09-20 | 2023-12-12 | 上海量孚新能源科技有限公司 | 一种磷酸铁锂材料及其制备工艺和应用 |
Also Published As
Publication number | Publication date |
---|---|
JP5347031B2 (ja) | 2013-11-20 |
EP2287944A4 (en) | 2014-04-23 |
US8470207B2 (en) | 2013-06-25 |
CN101567449B (zh) | 2012-06-27 |
HK1150096A1 (zh) | 2011-10-28 |
US20110114899A1 (en) | 2011-05-19 |
CN101567449A (zh) | 2009-10-28 |
RU2477908C2 (ru) | 2013-03-20 |
AU2009347499B2 (en) | 2012-07-26 |
EP2287944A1 (en) | 2011-02-23 |
AU2009347499A1 (en) | 2010-12-09 |
JP2012510140A (ja) | 2012-04-26 |
EP2287944B1 (en) | 2016-04-06 |
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