CN105047917A - Preparation method of lithium iron phosphate battery cathode material - Google Patents
Preparation method of lithium iron phosphate battery cathode material Download PDFInfo
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- CN105047917A CN105047917A CN201510382321.7A CN201510382321A CN105047917A CN 105047917 A CN105047917 A CN 105047917A CN 201510382321 A CN201510382321 A CN 201510382321A CN 105047917 A CN105047917 A CN 105047917A
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- 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
- 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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- H—ELECTRICITY
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- 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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a preparation method of a lithium iron phosphate battery cathode material. The method comprises the following steps: (1), preparing a lithium iron phosphate/carbon nanotube compound in a high-energy ball milling manner; (2), pelleting the lithium iron phosphate/carbon nanotube compound to obtain 1-10[mu]m particles; and (3), coating the compound with graphene nanosheets by a powder mixer, and then mixing a compound electrode material with a binder to obtain a lithium battery cathode material. The cathode material prepared by the method provided by the invention is good in electrical conductivity, high in tap density, simple in preparation technology and good in controllability; a high-capacity battery can be prepared; and the requirements of large-scale production can be met.
Description
Technical field
The present invention relates to a kind of dynamic lithium battery material, be specifically related to a kind of preparation method of lithium iron phosphate battery positive material.
Background technology
The performance of lithium ion battery depends primarily on positive and negative pole material, LiFePO4 is a kind of novel anode material for lithium-ion batteries, its security performance and cycle life are that other battery material is incomparable, meet the needs of the frequent discharge and recharge of electric motor car, and be that the high capacity lithium ion battery of positive electrode is more easily connected use with LiFePO4, higher power can be provided for electric motor car.In addition, LiFePO4 has the advantages such as nontoxic, pollution-free, security performance is good, raw material sources is extensive, low price, and the life-span is long, is the desirable positive electrode of power lithium-ion battery of new generation.
LiFePO4 bulk density is low hinders its practical application with shortcoming that is poorly conductive.Researchers, in order to improve conductivity, mix the material with carbon elements such as electrically conductive graphite in the material, and this significantly reduces again the bulk density of material, and the tap density of carbon dope LiFePO4 generally only has 1.0 ~ 1.2g/cm
3, and the tap density of commodity cobalt acid lithium is generally 2.0 ~ 2.4g/cm
3, so low bulk density makes the volume and capacity ratio of LiFePO4 mutually far short of what is expected with cobalt acid lithium, and the battery volume made is comparatively large, is difficult to be applied to reality; In addition, the electrically conductive graphite of doping is generally spherical, forms point cantact with LiFePO4, and in order to form good path, doping is comparatively large, thus causes the volume of lithium iron phosphate positive material larger.
How while guarantee lithium iron phosphate positive material electric conductivity, improving its tap density, being the capacitance effectively improving lithium battery, is the key technology that its practical application lays the foundation.
Summary of the invention
There is provided herein a kind of preparation method of lithium iron phosphate battery positive material, solve the problem of the low and poorly conductive of the tap density of LiFePO4, for the further raising of lithium battery performance lays the foundation.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: LiFePO4 is mixed with carbon nano-tube, high-energy ball milling 3 ~ 20h;
2) compound granulation: by step 1) gained compound and binding agent mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with graphene nanometer sheet, obtains through mixed powder 5 ~ 30h the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with binding agent, homogenate and drying, then high-temperature vacuum process at 180 ~ 220 DEG C.
First optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, step 1) mass ratio that mixes with carbon nano-tube of described LiFePO4 is 100: 1 ~ 1: 1.
Second optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, step 1) mass ratio that mixes with carbon nano-tube of described LiFePO4 is 20: 1.
3rd optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, step 1) ratio of grinding media to material of described high-energy ball milling is 11: 1 ~ 10: 1.
4th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, described binding agent is sodium alginate, shitosan, sodium cellulose glycolate or polyacrylic acid.
5th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, step 2) mass ratio 1: 1 ~ 1: 50 of LiFePO4 in described binding agent and compound.
6th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, in composite particles described in step a, the mass ratio of LiFePO4 and graphene nanometer sheet is 100: 1 ~ 1: 1.
7th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, in composite particles described in step a, the mass ratio of LiFePO4 and graphene nanometer sheet is 20: 1.
8th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, the mass ratio 1: 1 ~ 1: 50 of LiFePO4 in binding agent described in step b and compound.
9th optimal technical scheme of the preparation method of described lithium iron phosphate battery positive material, vacuum treated temperature described in step b is 200 DEG C.
With immediate prior art ratio, tool of the present invention has the following advantages:
1) in the positive electrode prepared of the present invention inner mutual become the carbon nano-tube of conductive network and surface coated graphene nanometer sheet greatly can improve the conductivity of positive electrode, improve power density and the charge/discharge rates of battery, the capacitance of the lithium battery that can effectively improve, specific discharge capacity is up to 169.2mAhg
-1, after 1000 circulations of 10C multiplying power, specific capacity conservation rate is greater than 92%;
2) compound of the inventive method to LiFePO4 and carbon nano-tube adopts the preparation technology of granulation, improves its tap density, reduce the volume of conductive carbon material while guarantee positive electrode conductivity.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further.
Embodiment 1
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 5g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 10h;
2) compound granulation: by step 1) gained compound and 10g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with 5g graphene nanometer sheet, and in mixed powder machine, mixed powder 20h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 200 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Embodiment 2
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 10g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 15h;
2) compound granulation: by step 1) gained compound and 15g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with 8g graphene nanometer sheet, and in mixed powder machine, mixed powder 25h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 180 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Embodiment 3
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 80g lithium iron phosphate nano powder, 5g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 8h;
2) compound granulation: by step 1) gained compound and 6g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with 4g graphene nanometer sheet, and in mixed powder machine, mixed powder 15h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 200 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Embodiment 4
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 6g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 15h;
2) compound granulation: by step 1) gained compound and 8g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with 6g graphene nanometer sheet, and in mixed powder machine, mixed powder 20h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 200 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Embodiment 5
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 10g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 20h;
2) compound granulation: by step 1) gained compound and 15g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with 10g graphene nanometer sheet, and in mixed powder machine, mixed powder 30h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 8g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 210 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Comparative example 1
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 5g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 10h;
2) compound granulation: by step 1) gained compound and 10g polyacrylic acid mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
Lithium iron phosphate/carbon nanotube composite particles is mixed with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 200 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Comparative example 2
A preparation method for lithium iron phosphate battery positive material, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: take 100g lithium iron phosphate nano powder, 5g carbon nano-tube mixes in rear loading stainless steel jar mill, high-energy ball milling 10h;
2) preparation of anode material of lithium battery
A. by step 1) gained compound mixes with 5g graphene nanometer sheet, and in mixed powder machine, mixed powder 20h obtains the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with 5g polyacrylic acid, stirs and make slurry, be applied in aluminum foil current collector, after to be dried, carry out 200 DEG C of high-temperature vacuum process, namely can be used as electrode material of lithium battery application.
Gained positive electrode is assembled into 2025 button cells, and at its discharge capacity of 2.5 ~ 4.2V voltage range build-in test and cycle performance, result is as shown in table 1, and in embodiment, the specific discharge capacity of products obtained therefrom is up to 169.2mAhg
-1after 1000 circulations of 10C multiplying power, specific capacity conservation rate is greater than 92%, the acting in conjunction of carbon nano-tube and Graphene is conducive to the raising (comparative example 1 and comparative example 1) of positive electrode performance, adopts prilling to improve capacity and the cycle performance (comparative example 1 and comparative example 2) of positive electrode.
Table 1
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent to replace, these do not depart from any amendment of spirit and scope of the invention or equivalently to replace within the claims that all awaits the reply in application.
Claims (10)
1. a preparation method for lithium iron phosphate battery positive material, is characterized in that, the method comprises the steps:
1) preparation of lithium iron phosphate/carbon nanotube complex: LiFePO4 is mixed with carbon nano-tube, high-energy ball milling 3 ~ 20h;
2) compound granulation: by step 1) gained compound and binding agent mix, and granulation obtains the lithium iron phosphate/carbon nanotube composite particles of 1 ~ 10 μm of particle diameter;
3) preparation of anode material of lithium battery
A. by step 2) gained composite particles mixes with graphene nanometer sheet, obtains through mixed powder 5 ~ 30h the lithium iron phosphate/carbon nanotube complex that Surface coating has graphene nanometer sheet;
B. lithium iron phosphate/carbon nanotube complex step a gained being coated with graphene nanometer sheet mixes with binding agent, homogenate and drying, then high-temperature vacuum process at 180 ~ 220 DEG C.
2. the preparation method of lithium iron phosphate battery positive material according to claim 1, is characterized in that, step 1) mass ratio that mixes with carbon nano-tube of described LiFePO4 is 100: 1 ~ 1: 1.
3. the preparation method of lithium iron phosphate battery positive material according to claim 2, is characterized in that, step 1) mass ratio that mixes with carbon nano-tube of described LiFePO4 is 20: 1.
4. the preparation method of lithium iron phosphate battery positive material according to claim 1, is characterized in that, step 1) ratio of grinding media to material of described high-energy ball milling is 11: 1 ~ 10: 1.
5. the preparation method of lithium iron phosphate battery positive material according to claim 1, it is characterized in that, described binding agent is sodium alginate, shitosan, sodium cellulose glycolate or polyacrylic acid.
6. the preparation method of lithium iron phosphate battery positive material according to claim 1, is characterized in that, step 2) mass ratio 1: 1 ~ 1: 50 of LiFePO4 in described binding agent and compound.
7. the preparation method of lithium iron phosphate battery positive material according to claim 1, it is characterized in that, in composite particles described in step a, the mass ratio of LiFePO4 and graphene nanometer sheet is 100: 1 ~ 1: 1.
8. the preparation method of lithium iron phosphate battery positive material according to claim 7, it is characterized in that, in composite particles described in step a, the mass ratio of LiFePO4 and graphene nanometer sheet is 20: 1.
9. the preparation method of lithium iron phosphate battery positive material according to claim 1, is characterized in that, the mass ratio 1: 1 ~ 1: 50 of LiFePO4 in binding agent described in step b and compound.
10. the preparation method of lithium iron phosphate battery positive material according to claim 1, it is characterized in that, vacuum treated temperature described in step b is 200 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532108A (en) * | 2016-12-22 | 2017-03-22 | 复旦大学 | Porous-structured lithium iron phosphate/carbon nanotube composite microsphere and preparation method therefor |
| CN107275606A (en) * | 2017-06-13 | 2017-10-20 | 山东大学 | A kind of carbon coating spinel lithium manganate nano composite material and preparation method and application |
| CN109904387A (en) * | 2019-02-25 | 2019-06-18 | 天津艾克凯胜石墨烯科技有限公司 | A kind of high-performance lithium anode piece preparation method |
| CN110380020A (en) * | 2019-06-18 | 2019-10-25 | 清华大学深圳研究生院 | Carbon-coated composite ferric lithium phosphate material, preparation method and application |
| JP2020508541A (en) * | 2017-02-27 | 2020-03-19 | ノースウェスタン ユニヴァーシティＮｏｒｔｈｗｅｓｔｅｒｎ Ｕｎｉｖｅｒｓｉｔｙ | Nanostructured lithium-ion battery electrode composites with conformal graphene dispersion |
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| CN101714627A (en) * | 2008-10-08 | 2010-05-26 | 中国科学院金属研究所 | Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof |
| CN103872287A (en) * | 2014-03-20 | 2014-06-18 | 重庆工商大学 | Composite positive electrode material of graphene and lithium iron phosphate battery and preparation method thereof |
| CN103887512A (en) * | 2014-04-09 | 2014-06-25 | 江苏天泽纳米科技有限公司 | Method for preparing lithium ion battery by using carbon nanotube as conductive agent |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532108A (en) * | 2016-12-22 | 2017-03-22 | 复旦大学 | Porous-structured lithium iron phosphate/carbon nanotube composite microsphere and preparation method therefor |
| CN106532108B (en) * | 2016-12-22 | 2019-07-05 | 复旦大学 | Lithium iron phosphate/carbon nanotube complex microsphere with porous structure and preparation method thereof |
| JP2020508541A (en) * | 2017-02-27 | 2020-03-19 | ノースウェスタン ユニヴァーシティＮｏｒｔｈｗｅｓｔｅｒｎ Ｕｎｉｖｅｒｓｉｔｙ | Nanostructured lithium-ion battery electrode composites with conformal graphene dispersion |
| JP7262392B2 (en) | 2017-02-27 | 2023-04-21 | ノースウェスタン ユニヴァーシティ | Nanostructured Lithium-ion Battery Electrode Composites by Conformal Graphene Dispersion |
| CN107275606A (en) * | 2017-06-13 | 2017-10-20 | 山东大学 | A kind of carbon coating spinel lithium manganate nano composite material and preparation method and application |
| CN107275606B (en) * | 2017-06-13 | 2020-03-17 | 山东大学 | Carbon-coated spinel lithium manganate nanocomposite and preparation method and application thereof |
| CN109904387A (en) * | 2019-02-25 | 2019-06-18 | 天津艾克凯胜石墨烯科技有限公司 | A kind of high-performance lithium anode piece preparation method |
| CN109904387B (en) * | 2019-02-25 | 2021-07-13 | 天津艾克凯胜石墨烯科技有限公司 | Preparation method of high-performance lithium battery positive plate |
| CN110380020A (en) * | 2019-06-18 | 2019-10-25 | 清华大学深圳研究生院 | Carbon-coated composite ferric lithium phosphate material, preparation method and application |
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