CN106654234A - Lithium battery anode material and preparation method thereof - Google Patents
Lithium battery anode material and preparation method thereof Download PDFInfo
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- CN106654234A CN106654234A CN201710065451.7A CN201710065451A CN106654234A CN 106654234 A CN106654234 A CN 106654234A CN 201710065451 A CN201710065451 A CN 201710065451A CN 106654234 A CN106654234 A CN 106654234A
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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
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- 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
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- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- 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
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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
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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
- H01M4/58—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
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
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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
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Abstract
The invention discloses a lithium battery anode material and a preparation method thereof. The lithium battery anode material is prepared from the following main raw materials in parts by weight: 8-12 parts of polypyrrole, 20-30 parts of lithium iron phosphate, 4-10 parts of polyaniline, 1-3 parts of polyvinyl imidazol, 1-3 parts of sodium ethylenesulphonate, and 1-3 parts of N,N'-Bis(4-chlorophenyl)-N,N'-diphenyl-1,4-phenylenediamine. A prepared lithium battery achieves excellent cycle performance, and the capacity remains at above 95% after 1C charge and discharge for 2,000 cycles at a room temperature; a 6C discharge capacity is above 98% of a 1C discharge capacity; the battery doesn't catch fire or explode in a 3C/10V overcharge test; the high-temperature cycle performance is excellent, and the capacity remains at above 93% after 1C charge and discharge for 1,000 cycles at a temperature of 60 DEG C; and good safety performance is achieved, and the battery doesn't explode or catch fire in a puncture test, an extrusion test, an overcharge test, an over-discharge test and other tests.
Description
Technical field
The present invention relates to a kind of cell art, specifically a kind of anode material of lithium battery and preparation method thereof.
Background technology
Commercial lithium-ion batteries positive electrode is mainly cobalt acid lithium and LiMn2O4.But problems are still suffered from, such as electricity
Between the material granule of pole and its between collector loose contact, sheet resistance is big and peel strength is poor, in charge and discharge process
Circulation expansion etc., the problems referred to above have had a strong impact on the cycle life and stability of lithium ion battery.
The content of the invention
It is an object of the invention to provide a kind of anode material of lithium battery and preparation method thereof, to solve above-mentioned background technology
The problem of middle proposition.
For achieving the above object, the present invention provides following technical scheme：
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：It is polypyrrole 8-12 parts, LiFePO4 20-30 parts, poly-
Aniline 4-10 parts, polyvinyl imidazole 1-3 parts, sodium vinyl sulfonate 1-3 parts, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,
4- penylene diamines 1-3 parts.
As further scheme of the invention：The anode material of lithium battery, be according to the primary raw material of weight portion：Poly- pyrrole
Cough up 9-11 parts, LiFePO4 24-27 parts, polyaniline 5-8 parts, polyvinyl imidazole 1-3 parts, sodium vinyl sulfonate 1-3 parts, N, N'-
Double (4- chlorphenyls)-N, N'- diphenyl -1,4- penylene diamines 1-3 parts.
As further scheme of the invention：The anode material of lithium battery, be according to the primary raw material of weight portion：Poly- pyrrole
Cough up 10 parts, 26 parts of LiFePO4,7 parts of polyaniline, 2 parts of polyvinyl imidazole, 2 parts of sodium vinyl sulfonate, N, double (the 4- chlorobenzenes of N'-
Base)-N, 2 parts of N'- diphenyl -1,4- penylenes diamines.
A kind of preparation method of anode material of lithium battery, concretely comprises the following steps：
（1）First, LiFePO4 is immersed in 0.2-0.6mol/L sodium hydroxide solutions, after immersion 2-4h in dustless space
It is ground with polypyrrole and polyaniline, is transferred to after mixing in high temperature furnace, calcining at constant temperature 6-8h at 600-650 DEG C, and with
2-5 DEG C of speed cools to room temperature with the furnace, and semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
As further scheme of the invention：Step（1）In be ground after the uniformity≤1%.
Compared with prior art, the invention has the beneficial effects as follows：
Prepared lithium ion battery has excellent cycle performance, and 1C charge and discharges under normal temperature circulate 2000 capacity and are maintained at 95%
More than；Electric discharge is more than the 98% of 1C capacity under 6C multiplying powers；3C/10V overcharges test, and battery is not on fire does not explode；High temperature circulation is excellent
Different, 1C charge and discharges at 60 DEG C circulate 1000 capacity and are maintained at more than 93%；With good security performance, acupuncture, extrude, overcharge,
Cross put etc. test do not explode, it is not on fire.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：8 parts of polypyrrole, 20 parts of LiFePO4, polyaniline 4
Part, 1 part of polyvinyl imidazole, 1 part of sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylenes diamines 1
Part.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.2mol/L sodium hydroxide solutions, immersion 2h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 6h at 600 DEG C, and with 2 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Embodiment 2
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：9 parts of polypyrrole, 24 parts of LiFePO4, polyaniline 5
Part, 1 part of polyvinyl imidazole, 1 part of sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylenes diamines 1
Part.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.3mol/L sodium hydroxide solutions, immersion 2h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 6h at 617 DEG C, and with 2 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Embodiment 3
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：10 parts of polypyrrole, 26 parts of LiFePO4, polyaniline 7
Part, 2 parts of polyvinyl imidazole, 2 parts of sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylenes diamines 2
Part.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.4mol/L sodium hydroxide solutions, immersion 3h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 7h at 625 DEG C, and with 4 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Embodiment 4
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：11 parts of polypyrrole, 27 parts of LiFePO4, polyaniline 8
Part, 3 parts of polyvinyl imidazole, 3 parts of sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylenes diamines 3
Part.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.5mol/L sodium hydroxide solutions, immersion 4h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 8h at 640 DEG C, and with 4 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Embodiment 5
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：12 parts of polypyrrole, 30 parts of LiFePO4, polyaniline
10 parts, 3 parts of polyvinyl imidazole, 3 parts of sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylene diamines
3 parts.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.6mol/L sodium hydroxide solutions, immersion 4h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 8h at 650 DEG C, and with 5 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Comparative example 1
A kind of anode material of lithium battery, be according to the primary raw material of weight portion：10 parts of polypyrrole, 26 parts of LiFePO4, polyaniline 7
Part, 2 parts of polyvinyl imidazole.
A kind of preparation method of anode material of lithium battery, it is characterised in that concretely comprise the following steps：
（1）First, LiFePO4 is immersed in 0.4mol/L sodium hydroxide solutions, immersion 3h after in dustless space with poly- pyrrole
Cough up and be ground with polyaniline, be transferred to after mixing in high temperature furnace, calcining at constant temperature 7h at 625 DEG C, and with 4 DEG C of speed with stove
Room temperature is cooled to, semi-finished product are obtained；
（2）Finally, semi-finished product are mixed with polyvinyl imidazole and is placed in ball mill and be ground, be subsequently placed at a temperature of 4 DEG C
Vacuum freeze drying, obtains final product.
Wherein：Step（1）In be ground after the uniformity≤1%.
Comparative example 2
Chinese patent " a kind of cell positive material and preparation method thereof "（Authorization Notice No.：CN104538631B）Middle embodiment 3
The positive electrode of preparation.
Comparative example 3
The cobalt acid lithium battery positive electrode of Hunan Shanshan New Materials Co., Ltd's production.
Test experiments：
Lithium electricity positive electrode prepared by embodiment 1-5 and comparative example 1-3 is prepared into 1665132 model lithium-ion-power cells
（The lamination soft-package battery of model H16*W65*L132mm）, compacted density is in 3.0g/cm3More than, volume energy density exists
More than 450Wh/L；Under 3.0V-4.2V voltages, 1C electric discharge gram volumes play more than 120mAh/g to battery core.
Lithium ion battery prepared by the present invention has excellent cycle performance, and 1C charge and discharges under normal temperature circulate 2000 capacity
It is maintained at more than 95%；Electric discharge is more than the 98% of 1C capacity under 6C multiplying powers；3C/10V overcharges test, and battery is not on fire does not explode；It is high
Temperature circulation is excellent, and 1C charge and discharges at 60 DEG C circulate 1000 capacity and are maintained at more than 93%；With good security performance, acupuncture, squeeze
Press, overcharge, cross put etc. test do not explode, it is not on fire.Concrete test result is shown in Table 1:
Table 1
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, the present invention can be in other specific forms realized.Therefore, no matter from which
From the point of view of a bit, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention will by appended right
Ask rather than described above is limited, it is intended that all changes that will fall in the implication and scope of the equivalency of claim
Include in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity those skilled in the art should
Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (5)
1. a kind of anode material of lithium battery, it is characterised in that the primary raw material according to weight portion is：Polypyrrole 8-12 parts, phosphoric acid
Iron lithium 20-30 parts, polyaniline 4-10 parts, polyvinyl imidazole 1-3 parts, sodium vinyl sulfonate 1-3 parts, N, N'- double (4- chlorphenyls)-
N, N'- diphenyl -1,4- penylene diamines 1-3 parts.
2. anode material of lithium battery according to claim 1, it is characterised in that the anode material of lithium battery, according to weight
Amount part primary raw material be：Polypyrrole 9-11 parts, LiFePO4 24-27 parts, polyaniline 5-8 parts, polyvinyl imidazole 1-3 parts, second
Sodium olefin sulfonate 1-3 parts, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl -1,4- penylene diamines 1-3 parts.
3. anode material of lithium battery according to claim 1 and 2, it is characterised in that the anode material of lithium battery, according to
The primary raw material of weight portion is：10 parts of polypyrrole, 26 parts of LiFePO4,7 parts of polyaniline, 2 parts of polyvinyl imidazole, vinyl sulfonic acid
2 parts of sodium, N, double (4- the chlorphenyls)-N of N'-, 2 parts of N'- diphenyl -1,4- penylenes diamines.
4. a kind of preparation method of the anode material of lithium battery as described in claim 1-3 is arbitrary, it is characterised in that concrete steps
For：
（1）First, LiFePO4 is immersed in 0.2-0.6mol/L sodium hydroxide solutions, after immersion 2-4h in dustless space
It is ground with polypyrrole and polyaniline, is transferred to after mixing in high temperature furnace, calcining at constant temperature 6-8h at 600-650 DEG C, and with
2-5 DEG C of speed cools to room temperature with the furnace, and semi-finished product are obtained；
（2）Finally, by semi-finished product and polyvinyl imidazole, sodium vinyl sulfonate, N, double (4- the chlorphenyls)-N of N'-, N'- diphenyl-
Isosorbide-5-Nitrae-penylene diamines mixes and places in ball mill and is ground, and vacuum freeze drying at a temperature of being subsequently placed at 4 DEG C is obtained final product.
5. the preparation method of anode material of lithium battery according to claim 4, it is characterised in that step（1）Middle grinding is mixed
The uniformity≤1% after even.
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| CN201710065451.7A CN106654234A (en) | 2017-02-06 | 2017-02-06 | Lithium battery anode material and preparation method thereof |
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| CN201710065451.7A CN106654234A (en) | 2017-02-06 | 2017-02-06 | Lithium battery anode material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102544505A (en) * | 2011-12-15 | 2012-07-04 | 湖北万润新能源科技发展有限公司 | Surface modification method of lithium iron phosphate cathode material |
| CN102683712A (en) * | 2012-05-25 | 2012-09-19 | 浙江振龙电源股份有限公司 | Lithium ferric phosphate battery adopting compound conductive agent and manufacturing method thereof |
| WO2016088880A1 (en) * | 2014-12-04 | 2016-06-09 | デンカ株式会社 | Conductive composition for electrode, electrode for nonaqueous cell, and nonaqueous cell |
-
2017
- 2017-02-06 CN CN201710065451.7A patent/CN106654234A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102544505A (en) * | 2011-12-15 | 2012-07-04 | 湖北万润新能源科技发展有限公司 | Surface modification method of lithium iron phosphate cathode material |
| CN102683712A (en) * | 2012-05-25 | 2012-09-19 | 浙江振龙电源股份有限公司 | Lithium ferric phosphate battery adopting compound conductive agent and manufacturing method thereof |
| WO2016088880A1 (en) * | 2014-12-04 | 2016-06-09 | デンカ株式会社 | Conductive composition for electrode, electrode for nonaqueous cell, and nonaqueous cell |
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Application publication date: 20170510 |