CN106025208A - Preparation method for carbon-coated ternary positive electrode material - Google Patents
Preparation method for carbon-coated ternary positive electrode material Download PDFInfo
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- CN106025208A CN106025208A CN201610387492.3A CN201610387492A CN106025208A CN 106025208 A CN106025208 A CN 106025208A CN 201610387492 A CN201610387492 A CN 201610387492A CN 106025208 A CN106025208 A CN 106025208A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- 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
Abstract
The invention relates to a preparation method for a carbon-coated ternary positive electrode material. According to the carbon-coated ternary positive electrode material, a precursor wet co-deposition coating technology is combined with a high-temperature solid-phase multi-step sintering technology; meanwhile, the melting point of the material is reduced by adding a fluxing agent; the precursor and the lithium salt are put in a melting environment so as to accelerate the metal ion diffusion and to enable the crystal particles to be grown at a relatively low temperature; the rate capability of the composite material can be remarkably improved due to the carbon coating; the high energy density of the lithium ion battery prepared by the positive electrode material can be ensured, and the power density can be increased as well; and in addition, the production cost is lowered.
Description
Technical field
The present invention relates to technical field of lithium batteries, be specifically related to the preparation method of a kind of carbon cladding tertiary cathode material.
Background technology
Lithium ion battery has the plurality of advantages such as energy density is high, power density is high, have extended cycle life, and is widely used in the electronic equipment such as mobile phone, notebook computer.Along with the application of lithium ion battery is more and more extensive, particularly in hybrid-power electric vehicle, pure electric vehicle and the application at aspects such as intelligent grids, people are more and more higher to the requirement of the chemical property of lithium ion battery.
Current business-like lithium ion anode material is mainly based on LiFePO4 (LiFePO4), ternary material (nickel-cobalt-manganese ternary material NCM, nickel cobalt aluminum ternary material NCA) and LiMn2O4 (LiMn2O4) etc., wherein lithium manganate battery cycle life is short and under hot environment cycle life worse, and there is safety issue as electrokinetic cell in ternary material.LiFePO4 cost of material is low, and theoretical capacity is big, has extended cycle life, and is the most promising product generally acknowledged of lithium battery.
Polynary transiting metal nickel bores manganese composite lithium-inserting oxide LiNi1-x-yCoxAlyO2(also referred to as ternary material), with LiNiO2And LiCoO2Structure is similar, has a-NaFeO2Layer structure, due to the cooperative effect between transition metal, the chemical property of multielement ma-terial is better than arbitrary single component oxide LiNiO2And LiCoO2；With LiCoO2Compare, the Ni-based tertiary cathode material LiNi of Co and Al doping1-x-yCoxAlyO2There is the advantages such as specific capacity is high, cheap, be generally considered and most possibly substitute LiCoO2Positive electrode, therefore become current anode material for lithium-ion batteries research focus.Existing market high-volume uses multielement ma-terial main specifications to be 111,424 and 523 specifications.But universal along with digital mobile product, market is increasingly stronger to the demand of the lithium ion battery of high power capacity, and the capacity of existing material all ratios are relatively low, is difficult to meet the requirement that people are the highest to aspects such as the high power capacity of lithium ion battery, high-energy-densities.
Summary of the invention
The present invention provides the preparation method of a kind of carbon cladding tertiary cathode material, the positive electrode using the method to prepare, and has preferable electric conductivity and cycle performance, has higher specific capacity and higher security performance.
To achieve these goals, the present invention provides the preparation method of a kind of carbon cladding tertiary cathode material, and the method comprises the steps:
(1) it is 60:20:20 mix homogeneously by nickel sulfate solution, cobalt sulfate solution and manganese sulfate solution by Ni:Co:Al mol ratio, then in solution, adds NaOH or KOH solution neutralizes, produce the hydroxide Ni of ternary system by controlling crystallization process0.6Co0.2Al0.2(OH)2Precipitation, then the precipitation that obtain is filtered, after washing, is dried 4-8h at 100-150 DEG C；
(2) in atmosphere furnace, it is passed through oxygen or air, heat treatment natural cooling after 10-12 hour will be carried out at step (1) products therefrom is at 300-600 DEG C, obtain oxide；
(3) by mixing by mol ratio 1:1-1.15 of the metal cation in oxide with Li ion in step (2) gained oxide and lithium salts, being simultaneously introduced flux in mixed process, its quality added is lithium salts and the 5-10% of oxide gross mass；Fully after mixing, by reactant point double sintering in air stream or oxygen stream, first sinter 6-8 hour under the airflow conditions of 700-800 DEG C, then sintering temperature is risen to 850-950 DEG C, sinter 10-12 hour in oxygen stream again, furnace cooling after sintering, obtain composite oxides；Carry out the composite oxides obtained pulverizing, classification, cross 300 mesh sieves, obtain ternary system composite oxides LiNi0.6Co0.2Al0.2O2Matrix material；
(4) by during in step (3), the matrix material of gained joins the aqueous sucrose solution that weight percentage is 0.2-0.3%, and stirring is made into uniform suspension, above-mentioned suspension is spray-dried by spray dryer under being continuously agitated, obtain dried powder, inlet temperature is 150-180 DEG C, whirlwind index 100%, charging rate is 10-15ml/min-1, dried powder is incorporated in the reactor having been heated to 350-400 DEG C by the atmospheric carrier air that flow velocity is 10-15L/min, outlet temperature 100-150 DEG C, collects and obtains carbon cladding tertiary cathode material.
Carbon of the present invention cladding tertiary cathode material, presoma wet method co-precipitation coating technology and high temperature solid-state multi-steps sintering technology are combined, use the method adding flux to reduce the fusing point of material simultaneously, presoma and lithium salts is made to be in a melted environment, accelerate the diffusion of metal ion, make crystal grain start growth promoter at a lower temperature；Carbon cladding is i.e. remarkably improved the high rate performance of composite, both can guarantee that the high-energy-density of lithium ion battery prepared by positive electrode, and can improve again its power density, and reduce production cost.
Detailed description of the invention
Embodiment one
It is 60:20:20 mix homogeneously by nickel sulfate solution, cobalt sulfate solution and manganese sulfate solution by Ni:Co:Al mol ratio, then in solution, adds NaOH or KOH solution neutralizes, produce the hydroxide Ni of ternary system by controlling crystallization process0.6Co0.2Al0.2(OH)2Precipitation, then the precipitation that obtain is filtered, after washing, is dried 4h at 100 DEG C.
In atmosphere furnace, it is passed through oxygen or air, products therefrom is carried out at 300 DEG C heat treatment natural cooling after 10 hours, obtains oxide.
Gained oxide and lithium salts being mixed by mol ratio 1:1 of the metal cation in oxide with Li ion, be simultaneously introduced flux in mixed process, its quality added is lithium salts and the 5% of oxide gross mass；Fully after mixing, by reactant point double sintering in air stream or oxygen stream, first sinter 6 hours under the airflow conditions of 700 DEG C, then sintering temperature is risen to 850 DEG C, sinter 10 hours in oxygen stream again, furnace cooling after sintering, obtain composite oxides；Carry out the composite oxides obtained pulverizing, classification, cross 300 mesh sieves, obtain ternary system composite oxides LiNi0.6Co0.2Al0.2O2Matrix material.
The matrix material of gained is joined in the aqueous sucrose solution that weight percentage is 0.2%, and stirring is made into uniform suspension, above-mentioned suspension is spray-dried by spray dryer under being continuously agitated, obtain dried powder, inlet temperature is 150 DEG C, whirlwind index 100%, charging rate is 10ml/min-1, dried powder is incorporated in the reactor having been heated to 350 DEG C by the atmospheric carrier air that flow velocity is 10L/min, outlet temperature 100 DEG C, collects and obtains carbon cladding tertiary cathode material.
Embodiment two
It is 60:20:20 mix homogeneously by nickel sulfate solution, cobalt sulfate solution and manganese sulfate solution by Ni:Co:Al mol ratio, then in solution, adds NaOH or KOH solution neutralizes, produce the hydroxide Ni of ternary system by controlling crystallization process0.6Co0.2Al0.2(OH)2Precipitation, then the precipitation that obtain is filtered, after washing, is dried 8h at 150 DEG C.
In atmosphere furnace, it is passed through oxygen or air, products therefrom is carried out at 600 DEG C heat treatment natural cooling after 12 hours, obtains oxide.
Gained oxide and lithium salts being mixed by mol ratio 1:1.15 of the metal cation in oxide with Li ion, be simultaneously introduced flux in mixed process, its quality added is lithium salts and the 10% of oxide gross mass；Fully after mixing, by reactant point double sintering in air stream or oxygen stream, first sinter 8 hours under the airflow conditions of 800 DEG C, then sintering temperature is risen to 950 DEG C, sinter 12 hours in oxygen stream again, furnace cooling after sintering, obtain composite oxides；Carry out the composite oxides obtained pulverizing, classification, cross 300 mesh sieves, obtain ternary system composite oxides LiNi0.6Co0.2Al0.2O2Matrix material.
The matrix material of gained is joined in the aqueous sucrose solution that weight percentage is 0.3%, and stirring is made into uniform suspension, above-mentioned suspension is spray-dried by spray dryer under being continuously agitated, obtain dried powder, inlet temperature is 180 DEG C, whirlwind index 100%, charging rate is 15ml/min-1, dried powder is incorporated in the reactor having been heated to 400 DEG C by the atmospheric carrier air that flow velocity is 15L/min, outlet temperature 150 DEG C, collects and obtains carbon cladding tertiary cathode material.
Comparative example
Commercially available lithium iron phosphate positive material.
Above-described embodiment one, two and comparative example products therefrom are used NMP as solvent, by active substance: be configured to slurry that solid content be 70% at SP: PVDF=90: 5: 5 is evenly applied on Al paper tinsel, makes positive pole.Negative pole selects the metal lithium sheet of diameter 14mm, 1mol LiFP6 (EC:DMC:EMC=1:1:1 selected by electrolyte, v/v), being packaged by battery with the order of negative electrode casing shell fragment pad lithium sheet electrolyte barrier film positive plate pad anode cover, whole process all completes in the glove box be filled with argon.Be at 25 DEG C, to carry out electric performance test in test temperature, after tested this embodiment one with two material compared with the product of comparative example, first charge-discharge reversible capacity improves 22-27%, brings up to more than 25% service life.
Claims (1)
1. a preparation method for carbon cladding tertiary cathode material, the method comprises the steps:
(1) it is 60:20:20 mix homogeneously by nickel sulfate solution, cobalt sulfate solution and manganese sulfate solution by Ni:Co:Al mol ratio, then in solution, adds NaOH or KOH solution neutralizes, produce the hydroxide Ni of ternary system by controlling crystallization process0.6Co0.2Al0.2(OH)2Precipitation, then the precipitation that obtain is filtered, after washing, is dried 4-8h at 100-150 DEG C；
(2) in atmosphere furnace, it is passed through oxygen or air, heat treatment natural cooling after 10-12 hour will be carried out at step (1) products therefrom is at 300-600 DEG C, obtain oxide；
(3) by mixing by mol ratio 1:1-1.15 of the metal cation in oxide with Li ion in step (2) gained oxide and lithium salts, being simultaneously introduced flux in mixed process, its quality added is lithium salts and the 5-10% of oxide gross mass；Fully after mixing, by reactant point double sintering in air stream or oxygen stream, first sinter 6-8 hour under the airflow conditions of 700-800 DEG C, then sintering temperature is risen to 850-950 DEG C, sinter 10-12 hour in oxygen stream again, furnace cooling after sintering, obtain composite oxides；Carry out the composite oxides obtained pulverizing, classification, cross 300 mesh sieves, obtain ternary system composite oxides LiNi0.6Co0.2Al0.2O2Matrix material；
(4) by during in step (3), the matrix material of gained joins the aqueous sucrose solution that weight percentage is 0.2-0.3%, and stirring is made into uniform suspension, above-mentioned suspension is spray-dried by spray dryer under being continuously agitated, obtain dried powder, inlet temperature is 150-180 DEG C, whirlwind index 100%, charging rate is 10-15ml/min-1, dried powder is incorporated in the reactor having been heated to 350-400 DEG C by the atmospheric carrier air that flow velocity is 10-15L/min, outlet temperature 100-150 DEG C, collects and obtains carbon cladding tertiary cathode material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106848183A (en) * | 2017-02-24 | 2017-06-13 | 中国科学院新疆理化技术研究所 | A kind of method for improving ternary cathode material of lithium ion battery high rate performance |
| CN108878828A (en) * | 2018-06-26 | 2018-11-23 | 浙江天能能源科技股份有限公司 | Carbon-coated nickelic tertiary cathode material of one kind and preparation method thereof |
| CN108963210A (en) * | 2018-06-26 | 2018-12-07 | 桑顿新能源科技有限公司 | A kind of preparation method of carbon coating monocrystalline tertiary cathode material |
| CN108987742A (en) * | 2018-07-23 | 2018-12-11 | 内蒙古华夏新材料科技有限公司 | A kind of nickelic positive electrode of lithium ion battery and preparation method thereof |
| CN109728277A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The method and product and battery be surface-treated to nickelic tertiary cathode material |
| CN109728279A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The surface treatment method and product and battery of a kind of nickelic tertiary cathode material |
| CN113443659A (en) * | 2021-06-25 | 2021-09-28 | 浙江帕瓦新能源股份有限公司 | Wet-method doping and carbon-coating co-modified quaternary anode material and preparation method thereof |
| CN114899381A (en) * | 2022-05-23 | 2022-08-12 | 广西科技大学 | Nickel cobalt lithium manganate lithium battery positive electrode material and preparation method and application thereof |
| CN114899399A (en) * | 2022-05-07 | 2022-08-12 | 武汉楚能新能源有限公司 | Carbon coating method of ternary cathode material with PVDF (polyvinylidene fluoride) as carbon source |
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| CN103000874A (en) * | 2012-11-07 | 2013-03-27 | 彩虹集团公司 | Preparation method of carbon-coated ternary positive electrode material |
| CN104157854A (en) * | 2014-07-31 | 2014-11-19 | 山东玉皇新能源科技有限公司 | Preparation method for ternary positive electrode material of graphene composite lithium ion battery |
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| CN102173465A (en) * | 2010-12-31 | 2011-09-07 | 国光电器股份有限公司 | Method for preparing lithium nickel cobalt aluminum oxides serving as lithium ion battery positive electrode material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106848183A (en) * | 2017-02-24 | 2017-06-13 | 中国科学院新疆理化技术研究所 | A kind of method for improving ternary cathode material of lithium ion battery high rate performance |
| CN108878828A (en) * | 2018-06-26 | 2018-11-23 | 浙江天能能源科技股份有限公司 | Carbon-coated nickelic tertiary cathode material of one kind and preparation method thereof |
| CN108963210A (en) * | 2018-06-26 | 2018-12-07 | 桑顿新能源科技有限公司 | A kind of preparation method of carbon coating monocrystalline tertiary cathode material |
| CN108987742A (en) * | 2018-07-23 | 2018-12-11 | 内蒙古华夏新材料科技有限公司 | A kind of nickelic positive electrode of lithium ion battery and preparation method thereof |
| CN109728277A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The method and product and battery be surface-treated to nickelic tertiary cathode material |
| CN109728279A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The surface treatment method and product and battery of a kind of nickelic tertiary cathode material |
| CN113443659A (en) * | 2021-06-25 | 2021-09-28 | 浙江帕瓦新能源股份有限公司 | Wet-method doping and carbon-coating co-modified quaternary anode material and preparation method thereof |
| CN113443659B (en) * | 2021-06-25 | 2022-05-03 | 浙江帕瓦新能源股份有限公司 | Wet-method doping and carbon-coating co-modified quaternary anode material and preparation method thereof |
| CN114899399A (en) * | 2022-05-07 | 2022-08-12 | 武汉楚能新能源有限公司 | Carbon coating method of ternary cathode material with PVDF (polyvinylidene fluoride) as carbon source |
| CN114899399B (en) * | 2022-05-07 | 2023-02-07 | 武汉楚能新能源有限公司 | Carbon coating method of ternary cathode material with PVDF (polyvinylidene fluoride) as carbon source |
| CN114899381A (en) * | 2022-05-23 | 2022-08-12 | 广西科技大学 | Nickel cobalt lithium manganate lithium battery positive electrode material and preparation method and application thereof |
| CN114899381B (en) * | 2022-05-23 | 2024-02-02 | 广西科技大学 | Nickel cobalt lithium manganate battery positive electrode material, and preparation method and application thereof |
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