CN106025207A - Preparation method for carbon-coated manganese-based positive electrode material - Google Patents
Preparation method for carbon-coated manganese-based positive electrode material Download PDFInfo
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- CN106025207A CN106025207A CN201610387170.9A CN201610387170A CN106025207A CN 106025207 A CN106025207 A CN 106025207A CN 201610387170 A CN201610387170 A CN 201610387170A CN 106025207 A CN106025207 A CN 106025207A
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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
- 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
- H01M4/485—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
- H01M4/50—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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- 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
- H01M4/62—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
- 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
Abstract
The invention relates to a preparation method for a carbon-coated manganese-based positive electrode material. The base material component of the manganese-based positive electrode material is Li[Ni<0.3-x>Li<0.13>Mn<0.57>Al<x>]O<2>, wherein x is equal to 0.05-0.15. According to the carbon-coated manganese-based positive electrode material prepared by the method, nickel ions are placed by a certain amount of aluminum ions, so that the mixing degree of lithium and nick is reduced; meanwhile, the thermal stability of the battery is improved; 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 manganese-based anode 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.
In recent years, a series of lithium-rich material Li [LixG1-x]O2(G=Ni, Co, Mn, Al, Zn), being considered the next generation widely most has desired lithium ion anode material.Specific discharge capacity when material is charged to 4.8V can more than 200mAh/g, but to there is also irreversible capacity first higher for lithium-rich material, the shortcomings such as high rate performance is relatively low, poor safety performance.
Summary of the invention
The present invention provides the preparation method of a kind of carbon cladding manganese-based anode 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 manganese-based anode material, and the matrix material ingredients of this manganese-based anode material is: Li [Ni0.3-xLi0.13Mn0.57Alx]O2, wherein X=0.05-0.15, the method comprises the steps:
(1) use hydroxide coprecipitation step method in following ratio synthetic material, first take the nickel sulfate hexahydrate (NiSO of certain mol proportion4·6H2And manganese sulfate monohydrate (MnSO O)4·H2O); put in the large beaker that capacity is 500ML; and in beaker, add the high-purity deionized water of 100ML; beaker is placed in constant temperature blender with magnetic force and is stirred; and under the protection of nitrogen, stir at a temperature of keeping 60 DEG C, when effects of ion mix homogeneously, in solution, gradually drip ammonia and the alkali liquor of potassium hydroxide configuration; note dripping too fast, in case reacting uneven；
(2) when the pH=11 of solution, dropping alkali liquor is stopped; naked eyes can find out that solution is light blue clearly; continue solution to stop after constant temperature 60 DEG C stirs 12 hours under nitrogen protection; see after 12 hours; the color of solution is almost without significantly change occurs; solution is used deionized water centrifuge washing, and tests with pH tester, until stopping washing after pH value is constant；
(3) washed precipitation being placed on after puts in beaker, is put into by beaker in 120 DEG C of baking ovens, dries and probably has 12 hours, when material is the driest, is thus made for presoma Ni0.3-xMn0.57(OH)1.74-2x, then by certain mol proportion, lithium carbonate, aluminium oxide, presoma are placed in clean mortar after mix homogeneously, with the ball mill grinding that rotating speed is 300rad/min 4 hours；
After hands grinds nearly one hour again, material balance measurement quality once, the circular slice, thin piece of about 2mm it is pressed into after being uniformly divided into several parts, thin and thick circular slice, thin piece uniformly 450 DEG C of heat treatments after 5 hours in Muffle furnace will be pressed into, after room temperature, take out circular slice, thin piece mortar tabletting again, carry out 800 DEG C during it puts into Muffle furnace the most again and calcine 15 hours, after cooling, pulverize, obtain matrix material Li [Ni0.3-xLi0.13Mn0.57Alx]O2；
(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 manganese-based anode material.
Carbon of the present invention cladding manganese-based anode material, a certain amount of aluminium ion replaces nickel ion can reduce lithium nickel mixing degree, improves the heat stability of battery simultaneously；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
The matrix material ingredients of the aluminum doped with manganese base anode material of the present embodiment is: Li [Ni0.25Li0.13Mn0.57Al0.05]O2。
Use hydroxide coprecipitation step method in following ratio synthetic material, first take the nickel sulfate hexahydrate (NiSO of certain mol proportion4·6H2And manganese sulfate monohydrate (MnSO O)4·H2O); put in the large beaker that capacity is 500ML; and in beaker, add the high-purity deionized water of 100ML; beaker is placed in constant temperature blender with magnetic force and is stirred; and under the protection of nitrogen, stir at a temperature of keeping 60 DEG C, when effects of ion mix homogeneously, in solution, gradually drip ammonia and the alkali liquor of potassium hydroxide configuration; note dripping too fast, in case reacting uneven.
Dropping alkali liquor is stopped when the pH=11 of solution; naked eyes can find out that solution is light blue clearly; continue solution to stop after constant temperature 60 DEG C stirs 12 hours under nitrogen protection; see after 12 hours; the color of solution is almost without significantly change occurs; solution is used deionized water centrifuge washing, and tests with pH tester, until stopping washing after pH value is constant.
Washed precipitation being placed on afterwards puts in beaker, is put into by beaker in 120 DEG C of baking ovens, dries and probably has 12 hours, when material is the driest, is thus made for presoma Ni0.25Mn0.57(OH)1.64, then by certain mol proportion, lithium carbonate, aluminium oxide, presoma are placed in clean mortar after mix homogeneously, with the ball mill grinding that rotating speed is 300rad/min 4 hours.
After hands grinds nearly one hour again, material balance measurement quality once, the circular slice, thin piece of about 2mm it is pressed into after being uniformly divided into several parts, thin and thick circular slice, thin piece uniformly 450 DEG C of heat treatments after 5 hours in Muffle furnace will be pressed into, after room temperature, take out circular slice, thin piece mortar tabletting again, carry out 800 DEG C during it puts into Muffle furnace the most again and calcine 15 hours, after cooling, pulverize, obtain matrix material Li [Ni0.25Li0.13Mn0.57Al0.05]O2。
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 manganese-based anode material.
Embodiment two
The matrix material ingredients of the aluminum doped with manganese base anode material of the present embodiment is: Li [Ni0.15Li0.13Mn0.57Al0.15]O2。
Use hydroxide coprecipitation step method in following ratio synthetic material, first take the nickel sulfate hexahydrate (NiSO of certain mol proportion4·6H2And manganese sulfate monohydrate (MnSO O)4·H2O); put in the large beaker that capacity is 500ML; and in beaker, add the high-purity deionized water of 100ML; beaker is placed in constant temperature blender with magnetic force and is stirred; and under the protection of nitrogen, stir at a temperature of keeping 60 DEG C, when effects of ion mix homogeneously, in solution, gradually drip ammonia and the alkali liquor of potassium hydroxide configuration; note dripping too fast, in case reacting uneven.
Dropping alkali liquor is stopped when the pH=11 of solution; naked eyes can find out that solution is light blue clearly; continue solution to stop after constant temperature 60 DEG C stirs 12 hours under nitrogen protection; see after 12 hours; the color of solution is almost without significantly change occurs; solution is used deionized water centrifuge washing, and tests with pH tester, until stopping washing after pH value is constant.
Washed precipitation being placed on afterwards puts in beaker, is put into by beaker in 120 DEG C of baking ovens, dries and probably has 12 hours, when material is the driest, is thus made for presoma Ni0.15Mn0.57(OH)1.44, then by certain mol proportion, lithium carbonate, aluminium oxide, presoma are placed in clean mortar after mix homogeneously, with the ball mill grinding that rotating speed is 300rad/min 4 hours.
After hands grinds nearly one hour again, material balance measurement quality once, the circular slice, thin piece of about 2mm it is pressed into after being uniformly divided into several parts, thin and thick circular slice, thin piece uniformly 450 DEG C of heat treatments after 5 hours in Muffle furnace will be pressed into, after room temperature, take out circular slice, thin piece mortar tabletting again, carry out 800 DEG C during it puts into Muffle furnace the most again and calcine 15 hours, after cooling, pulverize, obtain matrix material Li [Ni0.15Li0.13Mn0.57Al0.15]O2。
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 manganese-based anode 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 17-19%, brings up to more than 25% service life.
Claims (1)
1. a preparation method for carbon cladding manganese-based anode material, the matrix material ingredients of this manganese-based anode material is: Li [Ni0.3-xLi0.13Mn0.57Alx]O2, wherein X=0.05-0.15, the method comprises the steps:
(1) use hydroxide coprecipitation step method in following ratio synthetic material; first nickel sulfate hexahydrate and the manganese sulfate monohydrate of certain mol proportion are taken; put in the large beaker that capacity is 500ML; and in beaker, add the high-purity deionized water of 100ML; beaker is placed in constant temperature blender with magnetic force and is stirred; and under the protection of nitrogen; stir at a temperature of keeping 60 DEG C; in solution, ammonia and the alkali liquor of potassium hydroxide configuration is gradually dripped when effects of ion mix homogeneously; note dripping too fast, in case reacting uneven；
(2) when the pH=11 of solution, dropping alkali liquor is stopped; naked eyes can find out that solution is light blue clearly; continue solution to stop after constant temperature 60 DEG C stirs 12 hours under nitrogen protection; see after 12 hours; the color of solution is almost without significantly change occurs; solution is used deionized water centrifuge washing, and tests with pH tester, until stopping washing after pH value is constant；
(3) washed precipitation being placed on after puts in beaker, is put into by beaker in 120 DEG C of baking ovens, dries and probably has 12 hours, when material is the driest, is thus made for presoma Ni0.3-xMn0.57(OH)1.74-2x, then by certain mol proportion, lithium carbonate, aluminium oxide, presoma are placed in clean mortar after mix homogeneously, with the ball mill grinding that rotating speed is 300rad/min 4 hours；
After hands grinds nearly one hour again, material balance measurement quality once, the circular slice, thin piece of about 2mm it is pressed into after being uniformly divided into several parts, thin and thick circular slice, thin piece uniformly 450 DEG C of heat treatments after 5 hours in Muffle furnace will be pressed into, after room temperature, take out circular slice, thin piece mortar tabletting again, carry out 800 DEG C during it puts into Muffle furnace the most again and calcine 15 hours, after cooling, pulverize, obtain matrix material Li [Ni0.3-xLi0.13Mn0.57Alx]O2；
(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 manganese-based anode material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394156A (en) * | 2017-07-19 | 2017-11-24 | 长沙矿冶研究院有限责任公司 | A kind of method of modifying and its modified anode material of the lithium-rich manganese-based anode material for lithium-ion batteries based on organic matter ammoniacal liquor |
| 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 |
Citations (1)
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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 |
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- 2016-06-04 CN CN201610387170.9A patent/CN106025207A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Non-Patent Citations (1)
| Title |
|---|
| 杨丽丽: ""Zn2+掺杂的富锂层状正极材料Li[Ni0.3Li0.13Mn0.57]O2的合成与性质研究"", 《中国优秀硕士学位论文全文数据库（工程科技II辑）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394156A (en) * | 2017-07-19 | 2017-11-24 | 长沙矿冶研究院有限责任公司 | A kind of method of modifying and its modified anode material of the lithium-rich manganese-based anode material for lithium-ion batteries based on organic matter ammoniacal liquor |
| 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 |
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Application publication date: 20161012 |