CN101826614A - Preparation method of modified cathode material of lithium ion battery and battery applying same - Google Patents
Preparation method of modified cathode material of lithium ion battery and battery applying same Download PDFInfo
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- CN101826614A CN101826614A CN200910213790A CN200910213790A CN101826614A CN 101826614 A CN101826614 A CN 101826614A CN 200910213790 A CN200910213790 A CN 200910213790A CN 200910213790 A CN200910213790 A CN 200910213790A CN 101826614 A CN101826614 A CN 101826614A
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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 discloses a preparation method of a modified cathode material of a lithium ion battery and a battery applying the same. The invention is mainly characterized by taking lithium metal oxide which can be represented by using the general formula LiAl-xBxO2 of a molecular formula and has a laminar structure as a matrix of the modified cathode material. The surface of the matrix of the cathode material is coated with a layer of porous organic polymer for modification, and the organic polymer is a copolymer of vinylidene fluoride and hexafluoropropylene, or/and a homopolymer or a copolymer of ethylene oxide and propylene oxide. The modified cathode material in the lithium ion battery generates a reaction with a solvent in electrolyte or under the action of an additive to form a gelatinous dielectric layer. The modified cathode material is suitable for various lithium ion batteries and is especially suitable for polymer type lithium ion batteries.
Description
Technical field:
The invention belongs to lithium ion battery in new energy materials and the new energy field, more specifically relate to the preparation of cathode material for lithium ion battery and use the battery of this modification cathode material.
Technical background:
Lithium ion battery since realizing commercialization because its energy density height, in light weight, the life-span long and memoryless property is widely used.Business-like lithium ion battery mainly is to adopt LiCoO at present
2And LiNi
1-x-yCo
xMn
yO
2Cathode material, and these materials are under degree of depth charge status, structural stability and security performance have the open defect of existence.Along with mobile phone, notebook computer, digital camera, MP4﹠amp; 5, popularizing of means of communication such as palmtop PC, bluetooth earphone and digital electronic goods, the market demand of lithium ion battery is advanced by leaps and bounds, and to 2008, the annual requirement of global lithium ion battery was about 2,700,000,000.Incidents such as following lithium electrician industry high speed development and battery volume of production and marketing is that the potential safety hazard of lithium battery highlights day by day, and battery of mobile phone blast, Notebook Battery are on fire happen occasionally.The security performance of lithium ion battery and critical material thereof is improved, chemical property promotes and paid much attention to gradually.
At present, the method for modifying of industry inner cathode material mainly contains and mixes and surface coating two classes, and wherein mainly in order to improve the chemical property of material, the surface coats the chemical property that then not only can promote material in doping, can also improve the security performance of material.Method for coating of having reported and material mainly contain lithium carbonate, aluminium oxide, aluminum phosphate, magnesium oxide, zirconia, tin oxide, silica, titanium oxide, carbon, lithium tetraborate, composite oxides, other cathode materials etc., and do not see the report that uses organic substance to carry out coating modification.The method of modifying of a kind of cathode material for lithium ion battery disclosed by the invention and use the battery of this modification cathode material, use organic substance target material matrix to carry out coating modification, cathode material after modification can with solvent in the electrolyte under the effect of additive, cross-linking reaction takes place, form gel conduction matter, significantly improve the security performance and the cycle performance of material and battery, be applicable to various types of lithium ion batteries, be specially adapted to polymer Li-ion battery.
Summary of the invention:
The invention discloses a kind of preparation method of lithium ion battery modification cathode material and use the battery of this modification cathode material.The present invention is applicable to that all have the cathode material for lithium ion battery of layer structure, and material is applicable to various types of lithium ion batteries after modification, be specially adapted to polymer Li-ion battery.After the stratiform cathode material of routine carried out surface coating modification, the modification cathode material and use this modification cathode material battery security performance and chemical property obviously promoted.
Technical scheme of the present invention has following feature:
The conventional layered cathode material that the present invention uses the traditional industry method to make is matrix, and this matrix is useful molecules formula general formula LiA
1-xB
xThe lithium metal oxide with layer structure of O2 (0≤x≤0.1) expression.Wherein A is a transition metal, be one or more the combination in nickel, cobalt, the manganese, B is the divalence no variable valency metal element of above (containing divalence), is one or more the combination in magnesium, calcium, copper, aluminium, chromium, zirconium, titanium, zinc, yttrium, niobium, the gallium.
The present invention coats one deck porous organo polysilica compound at the cathode material matrix surface and carries out modification, preparation modification cathode material.At first organic polymer is dissolved in the organic solvent; Then, under 30～80 ℃ reaction temperature, the cathode material matrix is added, and be aided with stirring 0.5～3 hour; Refilter, the material slag is removed organic solvent 80～150 ℃ of oven dry, obtains the modification cathode material.
The organic polymer that the present invention is used to be coated on the cathode material matrix surface is a copolymer from vinylidene fluoride and hexafluoropropylene, or/and the homopolymers of oxirane, expoxy propane or copolymer, wherein the molecular weight that all occupies thing or copolymer of oxirane, expoxy propane is 5000-50000.The solvent that is used to be dissolved with organic polymer is the mixture of following one or more: acetone, methylethylketone ketones solvent, methyl formate, Ethyl formate, ethyl acetate esters solvent, ethylene carbonate, propene carbonate carbonates solvent, the tetrafluoro hydrogen heterocyclic compound solvent of muttering.
Among the present invention, use the battery of modification cathode material as cathode active material, also comprise: aluminum plastic film, aluminum hull, box hat with different shape are that housing is used to pack naked electric core, can carry out material with carbon element, alloy material or metal oxide that lithium embeds/deviate from is active material of positive electrode, the microporous membrane that with the polyolefin is basic material is a barrier film, electrolyte also contains additive except that containing lithium salts, chain and cyclic carbonate kind solvent.Additive in the electrolyte is plasticizer and initator two classes, plasticizer is one or more a mixture in dibutyl phthalate, o-phthalic acid dibutyl ester, the n-octyl n-decyl adipate (NODA), and initator is a kind of in azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), cumyl peroxide, the benzoyl peroxide.
Among the present invention, the battery of applying modified cathode material, in 60-110 ℃ temperature and 800-2000kPa scope, in electrolyte under the initiation and plasticization of additive, solvent generation cross-linking reaction in surface coated organic polymer of modification cathode material and the electrolyte forms gel-like electrolyte.
Adopt technical scheme of the present invention, the battery of applying modified cathode material uses the battery of unmodified cathode material matrix and uses the battery of the cathode material of existing public technology modification to have following notable feature and beneficial effect: 1) adopt organic polymer target material matrix to carry out coating modification; 2) the Promethean employing organic polymer that can form gel electrolyte with electrolyte solvent generation cross-linking reaction carries out coating modification; 3) modification cathode material surface coating layer can reduce the side reaction generation, helps material and keep Stability Analysis of Structures in charge and discharge process; 4) use the battery of modification cathode material, security performance and cycle performance be improved significantly.
Description of drawings
Fig. 1 uses the loop test figure of the material modified battery of cobalt acid lithium basis material or the modification of cobalt acid lithium
Fig. 2 uses LiNi
1/3Co
1/3Mn
1/3O
2Basis material or modification LiNi
1/3Co
1/3Mn
1/3O
2The loop test figure of material modified battery
Fig. 3 uses LiNi
0.75Co
0.20Al
0.05O
2Basis material or LiNi
0.75Co
0.20Al
0.05O
2The loop test figure of material modified battery
Embodiment
Below by specific embodiment content of the present invention is further set forth and explanation.But embodiment just in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, the some simple deduction or replace of making all should be considered as belonging to protection scope of the present invention.
Embodiment 1:
Copolymer from vinylidene fluoride and hexafluoropropylene is dissolved in the acetone, and to keep temperature be 40 ℃, then industrial conventional cobalt acid lithium basis material added, and stirring 1h, carry out Separation of Solid and Liquid again, solid formation toasts 12h in 100 ℃ baking oven, obtains cobalt acid lithium modification cathode material.
With the performance of the polymer battery test material of 053450 model, material modified with conventional cobalt acid lithium and cobalt acid lithium respectively is cathode active material, and anode adopts the needle-like Delanium, and electrolyte adopts three layers of microporous barrier of PE/PP/PE, and electrolyte adopts 1MLiPF
6/ EC: EMC: DEC=1: 1: 1 system and add therein dibutyl phthalate as plasticizer, azodiisobutyronitrile as initator.After the battery Vacuum Package of applying modified cathode material, be that 80 ℃, pressure are under the condition of 800kPa, make the solvent in material coating layer and the electrolyte under the effect of additive, crosslinked action take place, form gel-like electrolyte in temperature.
The battery mark of using cobalt acid lithium basis material is battery-A, the battery mark of using cobalt acid lithium modification cathode material is battery-B, the test result of overcharging of battery-A and battery-B is as shown in table 1,85 ℃/4h high-temperature storage test result is as shown in table 2, and the loop test result as shown in Figure 1.
Overcharge data test as seen from table 1, and cobalt acid lithium basis material and forms gel electrolyte with the electrolyte solvent reaction in battery after being coated with the organic polymer modification, make battery the anti-over-charging performance be improved significantly, can overcharge test by 3C5V7h.High-temperature storage test result from table 2 as seen, the size and the internal resistance of using the material modified battery of cobalt acid lithium are slightly larger than the battery of using cobalt acid lithium basis material because of the formation of gel layer, capacity is also a little less than the latter, but after carrying out the test of 85 ℃/4h high-temperature storage, use the material modified battery of cobalt acid lithium and on several Key Performance Indicators such as residual capacity, recovery capacity, internal resistance and size, all be better than the latter.Fig. 1 loop test result shows, both cycle performance basically identicals in early stage, but along with the increasing of cycle-index, the cycle performance of quoting the material modified battery of cobalt acid lithium is better than using the battery of cobalt acid lithium basis material gradually.
Table 1
Table 2
Embodiment 2:
With molecular weight is that 30000 oxirane, the homopolymers of expoxy propane are dissolved in the Ethyl formate, and to keep temperature be 50 ℃, then with industrial conventional LiNi
1/3Co
1/3Mn
1/3O
2Basis material adds, and stirs 2h, carries out Separation of Solid and Liquid again, and solid formation toasts 12h in 110 ℃ baking oven, obtain LiNi
1/3Co
1/3Mn
1/3O
2The modification cathode material.
With the performance of the polymer battery test material of 053450 model, respectively with conventional LiNi
1/3Co
1/3Mn
1/3O
2And LiNi
1/3Co
1/3Mn
1/3O
2Material modified is cathode active material, and anode adopts the needle-like Delanium, and electrolyte adopts three layers of microporous barrier of PE/PP/PE, and electrolyte adopts 1MLiPF
6/ EC: EMC: DEC=1: 1: 1 system and add therein o-phthalic acid dibutyl ester as plasticizer, cumyl peroxide as initator, cyclohexylbenzene functional additive.After the battery Vacuum Package of applying modified cathode material, be that 85 ℃, pressure are under the condition of 500kPa, make the solvent in material coating layer and the electrolyte under the effect of additive, crosslinked action take place, form gel-like electrolyte in temperature.
Use LiNi
1/3Co
1/3Mn
1/3O
2The battery mark of basis material is battery-C, uses LiNi
1/3Co
1/3Mn
1/3O
2The battery mark of modification cathode material is battery-D, and the test result of overcharging of battery-C and battery-D is as shown in table 3, and 85 ℃/4h high-temperature storage test result is as shown in table 4, and the loop test result as shown in Figure 2.
Table 3
Table 4
From table 3, overcharge data test as seen, LiNi
1/3Co
1/3Mn
1/3O
2Basis material and forms gel electrolyte with electrolyte solvent reaction in battery after being coated with the organic polymer modification, make battery the anti-over-charging performance be improved significantly, can overcharge test by 3C10V7h.As seen high-temperature storage test result from table 4 uses LiNi
1/3Co
1/3Mn
1/3O
2The size of material modified battery and internal resistance are slightly larger than because of the formation of gel layer uses LiNi
1/3Co
1/3Mn
1/3O
2The battery of basis material, capacity be also a little less than the latter, but after carrying out the test of 85 ℃/4h high-temperature storage, use LiNi
1/3Co
1/3Mn
1/3O
2Material modified battery all is better than the latter on several Key Performance Indicators such as residual capacity, recovery capacity, internal resistance and size.Fig. 2 loop test result shows, both cycle performance basically identicals in early stage, but, quote LiNi along with the increasing of cycle-index
1/3Co
1/3Mn
1/3O
2The cycle performance of material modified battery is better than using LiNi gradually
1/3Co
1/3Mn
1/3O
2The battery of basis material.
Embodiment 3:
With copolymer from vinylidene fluoride and hexafluoropropylene, and molecular weight be that the copolymer of 30000 oxirane, expoxy propane is dissolved in during tetrafluoro hydrogen mutters, and to keep temperature be 60 ℃, then with industrial conventional LiNi
0.75Co
0.20Al
0.05O
2Basis material adds, and stirs 1h, carries out Separation of Solid and Liquid again, and solid formation toasts 12h in 100 ℃ baking oven, obtain LiNi
0.75Co
0.20Al
0.05O
2The modification cathode material.
With the performance of the polymer battery test material of 053450 model, respectively with conventional LiNi
0.75Co
0.20Al
0.05O
2And LiNi
0.75Co
0.20Al
0.05O
2Material modified is cathode active material, and anode adopts the needle-like Delanium, and electrolyte adopts three layers of microporous barrier of PE/PP/PE, and electrolyte adopts 1MLiPF
6/ EC: EMC: DEC=1: 1: 1 system and add therein n-octyl n-decyl adipate (NODA) as plasticizer, azodiisobutyronitrile as initator.After the battery Vacuum Package of applying modified cathode material, be that 80 ℃, pressure are under the condition of 1000kPa, make the solvent in material coating layer and the electrolyte under the effect of additive, crosslinked action take place, form gel-like electrolyte in temperature.
Use LiNi
0.75Co
0.20Al
0.05O
2The battery mark of basis material is battery-E, uses LiNi
0.75Co
0.20Al
0.05O
2The battery mark of modification cathode material is battery-F, and the 85 ℃/4h high-temperature storage test result of battery-E and battery-F is as shown in table 5, and the loop test result as shown in Figure 3.
As seen 85 ℃/4h high-temperature storage test result from table 5 uses LiNi
0.75Co
0.20Al
0.05O
2The size of material modified battery and internal resistance are slightly larger than because of the formation of gel layer uses LiNi
0.75Co
0.20Al
0.05O
2The battery of basis material, capacity be also a little less than the latter, but after the high-temperature storage, use LiNi
0.75Co
0.20Al
0.05O
2Material modified battery all is better than the latter on several Key Performance Indicators such as residual capacity, recovery capacity, internal resistance and size.Both cycle performance test results in the comparison diagram 3 after 300 circulations, are used LiNi
0.75Co
0.20Al
0.05O
2The capability retention of material modified battery is used LiNi
0.75Co
0.20Al
0.05O
2The battery of basis material is high by 3%.
Table 5
Claims (9)
1. the preparation method of a lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: the modification cathode material makes by coat one deck porous organo polysilica compound at the cathode material matrix surface.With the modification cathode material is the battery of cathode active material, also comprise: can carry out material with carbon element, alloy material or metal oxide that lithium embeds/deviate from is active material of positive electrode, the microporous membrane that with the polyolefin is basic material is a barrier film, electrolyte also contains additive except that containing lithium salts, carbonates solvent.
2. the preparation method of a kind of lithium ion battery modification cathode material according to claim 1 and use the battery of this modification cathode material, it is characterized in that: the cathode material matrix is molecular formula general formula LiA
1-xB
xThe lithium metal oxide with layer structure of O2 (0≤x≤0.1) expression.Wherein A is a transition metal, is one or more the combination in nickel, cobalt, the manganese, and B is the above no variable valency metal element of divalence, is one or more the combination in magnesium, calcium, copper, aluminium, chromium, zirconium, titanium, zinc, yttrium, niobium, the gallium.
3. the preparation method of a kind of lithium ion battery modification cathode material according to claim 1 and use the battery of this modification cathode material, it is characterized in that: the surface coated porous organo polysilica compound of cathode material is a copolymer from vinylidene fluoride and hexafluoropropylene.
4. according to the preparation method of claims 1 described a kind of lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: homopolymers or copolymer that the surface coated porous organo polysilica compound of cathode material is oxirane, expoxy propane, and its molecular weight is between 5000-50000.
5. according to the preparation method of claims 1 described a kind of lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: the surface coated porous organo polysilica compound of cathode material is the homopolymers or the copolymer of copolymer from vinylidene fluoride and hexafluoropropylene and oxirane, expoxy propane.
6. according to the preparation method of claims 1,3,4,5 described a kind of lithium ion battery modification cathode materials and use the battery of this modification cathode material, it is characterized in that: at first organic polymer is dissolved in the organic solvent; Then the cathode material matrix is added, and be aided with stirring 0.5-3 hour; Refilter, the material slag is removed organic solvent 80-150 ℃ of oven dry, obtains the modification cathode material.
7. according to the preparation method of claims 1 described a kind of lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: the solvent that is used to be dissolved with organic polymer is the mixture of following one or more: acetone, methylethylketone ketones solvent, methyl formate, Ethyl formate, ethyl acetate esters solvent, ethylene carbonate, propene carbonate carbonates solvent, the tetrafluoro hydrogen heterocyclic compound solvent of muttering.
8. according to the preparation method of claims 1 described a kind of lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: the additive in the electrolyte is plasticizer and initator two classes, plasticizer is one or more a mixture in dibutyl phthalate, o-phthalic acid dibutyl ester, the n-octyl n-decyl adipate (NODA), and initator is a kind of in azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), cumyl peroxide, the benzoyl peroxide.
9. according to the preparation method of claims 1 described a kind of lithium ion battery modification cathode material and use the battery of this modification cathode material, it is characterized in that: the battery of applying modified cathode material, in 60-110 ℃ temperature and 800-2000kPa scope, in electrolyte under the initiation and plasticization of additive, solvent in surface coated organic polymer of modification cathode material and the electrolyte reacts, and forms gel-like electrolyte.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102097622A (en) * | 2011-01-18 | 2011-06-15 | 中国人民解放军国防科学技术大学 | Sulfur-containing composite anode material, anode plate and Li-S (lithium-sulfur) secondary battery and preparation method thereof |
| CN103078081A (en) * | 2013-01-15 | 2013-05-01 | 宁德新能源科技有限公司 | Surface coated lithium ion battery positive electrode active material particle and preparation method thereof |
| CN104037449A (en) * | 2013-03-08 | 2014-09-10 | 台湾塑胶工业股份有限公司 | Additive for lithium battery electrolyte and lithium battery electrolyte using same |
| CN104681782A (en) * | 2015-01-29 | 2015-06-03 | 北大先行科技产业有限公司 | Lithium ion secondary battery composite positive material and preparation method thereof |
| CN104701489A (en) * | 2015-03-25 | 2015-06-10 | 宁德新能源科技有限公司 | Lithium ion battery negative pole active material and preparation method and application thereof |
| CN106803575A (en) * | 2016-12-26 | 2017-06-06 | 宁波中车新能源科技有限公司 | A kind of anode material for lithium-ion batteries and its preparation method and application |
| CN109817910A (en) * | 2019-01-09 | 2019-05-28 | 蜂巢能源科技有限公司 | Positive electrode and preparation method thereof for solid lithium ion battery |
| CN109888381A (en) * | 2019-03-12 | 2019-06-14 | 清华大学 | Lithium anode protects liquid, lithium anode method for protecting surface, cathode pole piece, lithium battery and lithium-air battery |
| CN110265717A (en) * | 2019-06-15 | 2019-09-20 | 松山湖材料实验室 | High-voltage lithium ion battery electrolyte and its battery |
| CN111883765A (en) * | 2020-07-23 | 2020-11-03 | 松山湖材料实验室 | Lithium battery positive active material, preparation method thereof and lithium battery |
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| CN102097622A (en) * | 2011-01-18 | 2011-06-15 | 中国人民解放军国防科学技术大学 | Sulfur-containing composite anode material, anode plate and Li-S (lithium-sulfur) secondary battery and preparation method thereof |
| CN103078081A (en) * | 2013-01-15 | 2013-05-01 | 宁德新能源科技有限公司 | Surface coated lithium ion battery positive electrode active material particle and preparation method thereof |
| CN103078081B (en) * | 2013-01-15 | 2016-04-06 | 宁德新能源科技有限公司 | Surface coated anode active material of lithium ion battery particle and preparation method thereof |
| CN104037449A (en) * | 2013-03-08 | 2014-09-10 | 台湾塑胶工业股份有限公司 | Additive for lithium battery electrolyte and lithium battery electrolyte using same |
| CN104037449B (en) * | 2013-03-08 | 2017-03-01 | 台湾塑胶工业股份有限公司 | Additive for lithium battery electrolyte and lithium battery electrolyte using same |
| CN104681782A (en) * | 2015-01-29 | 2015-06-03 | 北大先行科技产业有限公司 | Lithium ion secondary battery composite positive material and preparation method thereof |
| CN104701489A (en) * | 2015-03-25 | 2015-06-10 | 宁德新能源科技有限公司 | Lithium ion battery negative pole active material and preparation method and application thereof |
| CN106803575B (en) * | 2016-12-26 | 2020-05-22 | 宁波中车新能源科技有限公司 | Lithium ion battery positive electrode material and preparation method and application thereof |
| CN106803575A (en) * | 2016-12-26 | 2017-06-06 | 宁波中车新能源科技有限公司 | A kind of anode material for lithium-ion batteries and its preparation method and application |
| CN109817910A (en) * | 2019-01-09 | 2019-05-28 | 蜂巢能源科技有限公司 | Positive electrode and preparation method thereof for solid lithium ion battery |
| CN109888381A (en) * | 2019-03-12 | 2019-06-14 | 清华大学 | Lithium anode protects liquid, lithium anode method for protecting surface, cathode pole piece, lithium battery and lithium-air battery |
| CN109888381B (en) * | 2019-03-12 | 2020-11-13 | 清华大学 | Metal lithium negative electrode protection solution, metal lithium negative electrode surface protection method, negative electrode plate, lithium battery and lithium-air battery |
| CN110265717A (en) * | 2019-06-15 | 2019-09-20 | 松山湖材料实验室 | High-voltage lithium ion battery electrolyte and its battery |
| CN111883765A (en) * | 2020-07-23 | 2020-11-03 | 松山湖材料实验室 | Lithium battery positive active material, preparation method thereof and lithium battery |
| CN113437300A (en) * | 2021-06-28 | 2021-09-24 | 山东大学 | Polyvinylidene fluoride modified lithium manganate positive electrode material and preparation method thereof |
| CN113437300B (en) * | 2021-06-28 | 2022-04-26 | 山东大学 | Polyvinylidene fluoride modified lithium manganate positive electrode material and preparation method thereof |
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