CN104766998A - A preparing method of a high-power high-energy density lithium ion battery - Google Patents
A preparing method of a high-power high-energy density lithium ion battery Download PDFInfo
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- CN104766998A CN104766998A CN201510128020.1A CN201510128020A CN104766998A CN 104766998 A CN104766998 A CN 104766998A CN 201510128020 A CN201510128020 A CN 201510128020A CN 104766998 A CN104766998 A CN 104766998A
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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
- H01M10/058—Construction or manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
A preparing method of a high-power high-energy density lithium ion battery is provided. According to the lithium ion battery, the cathode material is Li(Ni<0.6>Co<0.2>Mn<0.2>)O2/carbon nanotube composite ternary material, the inner core is hollow, the outer core is of a double-layer structure, the first layer is Li(Ni<0.6>Co<0.2>Mn<0.2>)O2, and the outer layer is carbon nanotubes. The preparing method includes following steps: 1) preparing the cathode material and 2) preparing an anode material. The ternary material prepared by the preparing method is structured and uniform in morphology, large in particles, irregular in morphology, and high in conductivity. A particle gap is reduced, and compaction density and conductivity of the ternary material are improved. By a chemical vapor deposition method, the carbon nanotubes with high conductivity are deposited on the surface of the ternary material, thus further improving conductivity and rate performance of the lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of high power lithium ion battery with high energy density, go out hollow ternary material/carbon nano tube compound material by template synthesis specifically.
Background technology
Lithium ion battery is the green energy-storing battery of a new generation, has that voltage is high, energy density is large, the outstanding advantages such as good cycle, self discharge are little, memory-less effect, has been widely used in the electronic products such as mobile phone, notebook computer, energy storage.Positive electrode is the crucial composition material of lithium ion battery, and the quality of its performance determines the quality of lithium ion battery.
Current positive electrode mainly contains LiFePO4, cobalt acid lithium, LiMn2O4 and ternary material thereof, wherein, cobalt acid lithium is still mainstay material, be mainly used in the small-sized lithium ion battery with high energy density field of high-end electronic product, but cobalt toxicity is larger, scarcity of resources, expensive, and its over-charge safety performance is poor.The LiMn2O4 specific capacity of spinel-type is low, and the shortcoming of high temperature circulation and storge quality difference never solves.LiFePO4 poorly conductive, product batches consistency are poor, poor performance at low temperatures, and the dissolving that there is trace iron may cause the problem of battery short circuit.Above-mentioned shortcoming limits the further application of these materials, therefore finds the emphasis that the better new material of cost performance becomes research.Research finds, with LiNi
1/3co
1/3mn
1/3o
2for the stratiform cobalt nickel oxide manganses series material (abbreviation ternary material) of representative has had both the advantage of above-mentioned material preferably, and compensate its defect to a certain extent, there is the features such as height ratio capacity, stable cycle performance, advantage of lower cost, security performance be better, be considered to the ideal chose for mixed type electrical source of power.The tertiary cathode material mainly solid construction of current preparation, its imbibition ability deviation, such as patent (CN 103872314 A) a kind of lithium ion battery method for pre-oxidizing of nickelic tertiary cathode active material presoma, there is cycle performance difference in its ternary material prepared, rate can differ from and the defect such as imbibition liquid-keeping property difference, limits its demand in hybrid power direction to rate lithium ion battery.
Summary of the invention
The rate that the present invention is directed to the existence of current ternary material can be poor, and the shortcoming of imbibition ability difference, the object of the invention is to provide a kind of hollow-core construction tertiary cathode material by template, to meet the demand of market to high magnification lithium ion battery with high energy density.
Technical scheme of the present invention is achieved in the following ways: a kind of preparation method of lithium ion battery of high power high-energy-density, and its positive electrode is Li (Ni
0.6co
0.2mn
0.2) O
2/ carbon nano-tube complex ternary material, kernel is hollow, and outer core has double-decker, and ground floor is Li (Ni
0.6co
0.2mn
0.2) O
2, skin is carbon nano-tube.Preparation method comprises the following steps: 1) positive electrode, 2) negative material; It is characterized in that:
1) positive electrode: choosing polystyrene colloid particle is microballoon core template, and add in dispersion liquid and stir, add metal salt solution, precipitation reagent afterwards, metal ion is deposited on template surface under the effect of precipitation reagent, organic-inorganic structure composite material is obtained to its filtration, mix with lithium salts, and adopt organic solvent dissolution to remove template, after filtration, obtain Li (Ni
xco
ymn
1-x-y) O
2(being designated as: NCM) material, adopts chemical vapour deposition technique at NCM material surface carbon nano-tube, finally obtains the hollow NCM/ carbon/carbon nano tube compound anode material with nucleocapsid structure.
Described slaine is: the one in the sulfate containing Ni, Co, Mn, nitrate or chlorate; Precipitation reagent is: the one in urea, ammonium carbonate, carbonic hydroammonium; Lithium salts is: the one of lithium hydroxide, lithium carbonate; Described organic solvent is oxolane.
Described chemical vapour deposition technique method is: be placed in reactor by the NCM material of drying, nitrogen is passed in reactor, and heating makes the temperature in reactor reach 500 ~ 1200 DEG C, stop passing into nitrogen, carbon-source gas and ammonia is passed into again in reactor, 20-60 minute is kept, in NCM superficial growth carbon nano-tube at 500 ~ 1200 DEG C; Close carbon-source gas and ammonia afterwards, then pass into hydrogen in reactor, and be cooled to room temperature in a nitrogen atmosphere, be i.e. obtained hollow NCM/ carbon/carbon nano tube compound anode material; Wherein said carbon-source gas is the mist of methane gas, acetylene gas or acetylene and argon gas.
2), negative material: negative material is silicon-carbon cathode, and its particle diameter D50 is 5 ~ 10 μm, and specific area is 2.0 ~ 5.0m
2/ g, gram volume is>=600mAh/g, first efficiency>=88%; Its polystyrene is the mixture be made up of the diameter micron ball that to be the nanosphere of (40 ~ 50) nm and diameter be (1 ~ 2) μm, and its mass ratio is (0.1 ~ 0.5): 1; And prepare flexible packing lithium ion battery in this, as positive and negative pole material.
The present invention, its material morphology prepared is regular, homogeneous, and the irregular pattern of larger particles has better conductivity.Template is owing to utilizing space confinement and the regulating and controlling effect of template, the particle diameter of synthetic material, pattern and structure can be controlled, but it is large to adopt single template can there is spherical space, reduce compacted density and the conductivity of material, therefore the template of different size is adopted to mix, and at surface deposition ternary material, prepare particle size distribution evenly, rational ternary material, thus can particulate interspaces be reduced and improve compacted density and the conductivity of material.By chemical vapour deposition technique, in the carbon nano-tube of ternary material surface deposition high conductivity, conductivity and the high rate performance of lithium ion battery can be improved further.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 prepares anode composite material Li (Ni
0.6co
0.2mn
0.2) O
2/ carbon nano-tube SEM schemes.
Embodiment
embodiment 1:
A preparation method of lithium ion battery for high power high-energy-density, comprises the following steps:
1, positive electrode: to take particle diameter be 50nm polystyrene 30 grams and particle diameter is that 1.5 μm of polystyrene 100 grams add in 1000 grams of second distillation aqueous solvents and stir, and adds 26.2 grams of (0.1mol) NiSO afterwards
46H
2o, 28.1 grams of (0.1mol) C
osO
47H
2o, 19.8 grams of (0.1mol) MnCl
24H
2o, ammonium carbonate 28.8 grams (0.3mol), obtains organic-inorganic structure composite material to its filtration afterwards, mixes afterwards with lithium hydroxide 7.2 grams (0.3mol), and adopt 100 milliliters of oxolane organic solvent dissolution removing templates, obtain Li (Ni after filtration
xco
ymn
1-x-y) O
2(being designated as: NCM) material, afterwards the NCM material of above-mentioned drying is placed in reactor, nitrogen is passed in described reactor, and heating makes the temperature in reactor reach 800 DEG C, stop passing into nitrogen, backward described reactor in pass into methane and ammonia, at 1000 DEG C keep 40 minutes, in NCM superficial growth carbon nano-tube; Close methane and ammonia afterwards, then pass into hydrogen in described reactor, and be cooled to room temperature in a nitrogen atmosphere, be i.e. obtained hollow NCM/ carbon/carbon nano tube compound anode material;
2, negative material: negative material is silicon-carbon cathode, its particle diameter D50 is 8 μm, and specific area is 3m
2/ g, gram volume is 800mAh/g, first efficiency 89%; And prepare flexible packing lithium ion battery in this, as positive and negative pole material.
Embodiment 2:
1, positive electrode: to take particle diameter be 40nm polystyrene 10 grams and particle diameter is that 1.0 μm of polystyrene 40 grams add in 1000 grams of alcohol solvents and stir, and adds 26.2 grams of (0.1mol) NiSO afterwards
46H
2o, 28.1 grams of (0.1mol) C
osO
47H
2o, 19.8 grams of (0.1mol) MnCl
24H
2o, 6.0 grams, urea (0.1mol), obtains organic-inorganic structure composite material to its filtration afterwards, mixes afterwards with lithium carbonate 7.4 grams (0.1mol), and adopt 200 milliliters of oxolane organic solvent dissolution removing templates, obtain Li (Ni after filtration
xco
ymn
1-x-y) O
2(being designated as: NCM) material, afterwards the NCM material of above-mentioned drying is placed in reactor, nitrogen is passed in described reactor, and heating makes the temperature in reactor reach 500 DEG C, stop passing into nitrogen, backward described reactor in pass into acetylene and ammonia, at 8000 DEG C keep 60 minutes, in NCM superficial growth carbon nano-tube; Close acetylene and ammonia afterwards, then pass into hydrogen in described reactor, and be cooled to room temperature in a nitrogen atmosphere, be i.e. obtained hollow NCM/ carbon/carbon nano tube compound anode material;
2, negative material: negative material is silicon-carbon cathode, its particle diameter D50 is 5 μm, and specific area is, 2m
2/ g, gram volume is 900mAh/g, first efficiency 88%; And prepare flexible packing lithium ion battery in this, as positive and negative pole material.
Embodiment 3:
1, positive electrode: to take particle diameter be 50nm polystyrene 10 grams and particle diameter is that 2.0 μm of polystyrene 40 grams add in 1000 grams of alcohol solvents and stir, and adds 26.2 grams of (0.1mol) NiSO afterwards
46H
2o, 28.1 grams of (0.1mol) C
osO
47H
2o, 15.1 grams of (0.1mol) MnSO
430.0 grams, urea (0.5mol), obtains organic-inorganic structure composite material to its filtration afterwards, mixes afterwards with lithium carbonate 37.0 grams (0.5mol), and adopt 400 milliliters of oxolane organic solvent dissolution removing templates, obtain Li (Ni after filtration
xco
ymn
1-x-y) O
2(being designated as: NCM) material, afterwards the NCM material of above-mentioned drying is placed in reactor, nitrogen is passed in described reactor, and heating makes the temperature in reactor reach 1000 DEG C, stop passing into nitrogen, backward described reactor in pass into acetylene and ammonia, at 1200 DEG C keep 20 minutes, in NCM superficial growth carbon nano-tube; Close acetylene and ammonia afterwards, then pass into hydrogen in described reactor, and be cooled to room temperature in a nitrogen atmosphere, be i.e. obtained hollow NCM/ carbon/carbon nano tube compound anode material;
2, negative material: negative material is silicon-carbon cathode, its particle diameter D50 is 5 μm, and specific area is, 2m
2/ g, gram volume is 900mAh/g, first efficiency 88%; And prepare flexible packing lithium ion battery in this, as positive and negative pole material.
Known by Fig. 1, be the SEM figure that embodiment 1 prepares anode composite material, as can be seen from Figure, trielement composite material presents spherical, and forms by size is spherical, and distribution rationally.
1, soft-package battery test: respectively with embodiment 1, embodiment 2, the ternary material that embodiment 3 is prepared, as positive electrode, take Delanium as negative material, adopts LiPF
6/ EC+DEC(volume ratio 1: 1) be electrolyte, Celgard 2400 film is barrier film, prepares 5Ah soft-package battery A1, A2, A3, and the cycle performance testing its soft-package battery;
2, battery as a comparison: purchase unmodified ternary material as positive electrode on market, Delanium is negative material, adopts LiPF
6/ EC+DEC(volume ratio 1: 1) be electrolyte, Celgard 2400 film is barrier film, prepares 2AH soft-package battery B; And be 1.0C/1.0C with multiplying power, voltage is under the condition of 2.7 ~ 4.2V, tests the cycle performance of its battery.Test the high rate performance of its soft-package battery simultaneously.
As can be seen from Table 1, the high rate performance of the battery that embodiment is prepared and cycle performance are obviously better than comparative example, its reason is because the carbon nano-tube of ternary material outer surface has high conductivity and large specific area, thus improve the multiplying power discharging property of battery, hollow ball-shape structure has larger imbibition liquid-keeping property simultaneously, thus improve the structural stability of material and sufficient electrolyte, and therefore improve the cycle performance of battery.
Table 1, embodiment 1-3 compare with the chemical property of comparative example
Claims (3)
1. a preparation method of lithium ion battery for high power high-energy-density, its positive electrode is Li (Ni
0.6co
0.2mn
0.2) O
2/ carbon nano-tube complex ternary material, kernel is hollow, and outer core has double-decker, and ground floor is Li (Ni
0.6co
0.2mn
0.2) O
2, skin is carbon nano-tube;
Preparation method comprises the following steps: 1) positive electrode, 2) negative material; It is characterized in that:
1), positive electrode: choosing polystyrene colloid particle is microballoon core template, and add in dispersion liquid and stir, add metal salt solution, precipitation reagent afterwards, metal ion is deposited on template surface under the effect of precipitation reagent, organic-inorganic structure composite material is obtained to its filtration, mix with lithium salts, and adopt organic solvent dissolution to remove template, after filtration, obtain Li (Ni
xco
ymn
1-x-y) O
2(being designated as: NCM) material, adopts chemical vapour deposition technique at NCM material surface carbon nano-tube, finally obtains the hollow NCM/ carbon/carbon nano tube compound anode material with nucleocapsid structure;
2), negative material: negative material is silicon-carbon cathode, and its particle diameter D50 is 5 ~ 10 μm, and specific area is 2.0 ~ 5.0m
2/ g, gram volume is>=600mAh/g, first efficiency>=88%; Its polystyrene is the mixture be made up of the diameter micron ball that to be the nanosphere of (40 ~ 50) nm and diameter be (1 ~ 2) μm, and its mass ratio is (0.1 ~ 0.5): 1; And prepare flexible packing lithium ion battery in this, as positive and negative pole material.
2. the preparation method of lithium ion battery of a kind of high power high-energy-density according to claim 1, is characterized in that: the slaine in described step 1) is: the one in the sulfate containing Ni, Co, Mn, nitrate or chlorate; Precipitation reagent is: the one in urea, ammonium carbonate, carbonic hydroammonium; Lithium salts is: the one of lithium hydroxide, lithium carbonate; Organic solvent is oxolane.
3. the preparation method of lithium ion battery of a kind of high power high-energy-density according to claim 1, it is characterized in that: the chemical vapour deposition technique method in described step 1) is: the NCM material of drying is placed in reactor, nitrogen is passed in reactor, and heating makes the temperature in reactor reach 500 ~ 1200 DEG C, stop passing into nitrogen, in reactor, pass into carbon-source gas and ammonia again, at 500 ~ 1200 DEG C, keep 20-60 minute, in NCM superficial growth carbon nano-tube; Close carbon-source gas and ammonia afterwards, then pass into hydrogen in reactor, and be cooled to room temperature in a nitrogen atmosphere, be i.e. obtained hollow NCM/ carbon/carbon nano tube compound anode material; Wherein said carbon-source gas is the mist of methane gas, acetylene gas or acetylene and argon gas.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108493406A (en) * | 2018-02-28 | 2018-09-04 | 中航锂电(洛阳)有限公司 | Nickelic tertiary cathode material is as application of the catalyst in terms of preparing carbon nanotube, positive electrode and preparation method thereof, lithium battery |
CN109835956A (en) * | 2019-01-11 | 2019-06-04 | 天津巴莫科技股份有限公司 | A kind of preparation method and applications of anode material for lithium-ion batteries |
CN111564633A (en) * | 2020-05-26 | 2020-08-21 | 大连中比能源科技有限公司 | Positive electrode active material, negative electrode active material, and preparation methods and applications thereof |
CN112310373A (en) * | 2020-10-30 | 2021-02-02 | 合肥国轩高科动力能源有限公司 | Preparation method of ternary cathode material of lithium ion battery |
CN113921789A (en) * | 2021-10-08 | 2022-01-11 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon quantum dot modified NCM ternary cathode material and prepared NCM ternary cathode material |
CN115057488A (en) * | 2022-07-12 | 2022-09-16 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material with special morphology and preparation method and application thereof |
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CN101259401A (en) * | 2004-11-11 | 2008-09-10 | 中国科学院化学研究所 | Method for preparing hollow ball and hollow ball with complex structure by template method |
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CN108493406A (en) * | 2018-02-28 | 2018-09-04 | 中航锂电(洛阳)有限公司 | Nickelic tertiary cathode material is as application of the catalyst in terms of preparing carbon nanotube, positive electrode and preparation method thereof, lithium battery |
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CN111564633A (en) * | 2020-05-26 | 2020-08-21 | 大连中比能源科技有限公司 | Positive electrode active material, negative electrode active material, and preparation methods and applications thereof |
CN112310373A (en) * | 2020-10-30 | 2021-02-02 | 合肥国轩高科动力能源有限公司 | Preparation method of ternary cathode material of lithium ion battery |
CN112310373B (en) * | 2020-10-30 | 2021-10-15 | 合肥国轩高科动力能源有限公司 | Preparation method of ternary cathode material of lithium ion battery |
CN113921789A (en) * | 2021-10-08 | 2022-01-11 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon quantum dot modified NCM ternary cathode material and prepared NCM ternary cathode material |
CN113921789B (en) * | 2021-10-08 | 2022-12-09 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon quantum dot modified NCM ternary cathode material and prepared NCM ternary cathode material |
CN115057488A (en) * | 2022-07-12 | 2022-09-16 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material with special morphology and preparation method and application thereof |
CN115057488B (en) * | 2022-07-12 | 2023-06-23 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material with special morphology, and preparation method and application thereof |
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