CN102664268A - Composite electrode active particle and preparation method and application thereof - Google Patents
Composite electrode active particle and preparation method and application thereof Download PDFInfo
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- CN102664268A CN102664268A CN2012101409613A CN201210140961A CN102664268A CN 102664268 A CN102664268 A CN 102664268A CN 2012101409613 A CN2012101409613 A CN 2012101409613A CN 201210140961 A CN201210140961 A CN 201210140961A CN 102664268 A CN102664268 A CN 102664268A
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Abstract
The invention discloses a composite electrode active particle and a preparation method and application thereof and belongs to the field of chemical energy storage batteries. The composite electrode active particle consists of a polymer adhesive, a conductive material and lithium-de-intercalated electrode active particles, wherein the conductive material is dispersed in the polymer adhesive; and the lithium-de-intercalated electrode active particles are dispersed in the polymer adhesive or attached to the surface of the polymer adhesive. The invention has the advantages that by compositing the electrode active particles, the conductive material and the polymer adhesive together, the density of an electrode active material can be effectively reduced, the electrode active particles can be suspended in an electrolyte solution, and the deposition speed rate of the electrode active material is reduced, so the flowing performance and conductive performance of electrode suspending liquid can be improved.
Description
Technical field
The invention belongs to chemical energy-storage battery field, relate in particular to a kind of combination electrode active particle and preparation method thereof and electrode suspension that utilizes this combination electrode active particle and lithium ion flow battery.
Background technology
The lithium ion flow battery is a kind of chemical cell technology that latest development is got up, and it combines the advantage of lithium ion battery and flow battery, is that a kind of power output and stored energy capacitance are independently of one another, energy density is big, lower-cost novel rechargeable battery.The lithium ion flow battery has boundless market prospects at aspects such as wind power generation, photovoltaic generation, peak load regulation network, distribution power station, municipal traffics.
The lithium ion flow battery is made up of anodal pool of suspension, negative pole pool of suspension, cell reaction device, closed conduit, liquid pump or other power set.Wherein, anodal pool of suspension holds the mixture of positive electrode active materials particle, conductive agent particle and electrolyte, and the negative pole pool of suspension holds the mixture of negative active core-shell material particle, conductive agent particle and electrolyte.During the work of lithium ion flow battery, electrode suspension is flowing between electrode pool of suspension and cell reaction device through closed conduit under liquid pump or other powered, and flow velocity can be regulated according to suspension concentration and ambient temperature.Wherein, anodal suspension is accomplished the reaction back and is returned anodal pool of suspension by anodal liquid outlet through closed conduit by the anodal reaction chamber of anodal inlet entering cell reaction device.Meanwhile, negative pole suspension is accomplished the reaction back and is returned the negative pole pool of suspension by the negative pole liquid outlet through closed conduit by the negative reaction chamber of negative pole inlet entering cell reaction device.Between anodal reaction chamber and the negative reaction chamber the nonconducting porous septum of electronics is arranged; Positive electrode active materials particle in the anodal suspension and the negative active core-shell material particle in the negative pole suspension are spaced from each other, avoid the both positive and negative polarity active material particle directly to contact the short circuit that causes inside battery.Anodal suspension in the anodal reaction chamber and the negative pole suspension in the negative reaction chamber can carry out lithium ion exchange transmission through the electrolyte in the porous septum.
The conductive agent particle average grain diameter that comprises in the existing electrode suspension is little, density is low, and therefore tiny conductive agent particle passes through the hole of barrier film probably, causes battery short circuit, causes the security incident of battery.Simultaneously; The density of electrode active material particles is generally all bigger, in suspension, is easy to take place sedimentation, is trapped in the cell reaction device; Electrode active material in the electrode suspension is lost activity, thereby influence the charge/discharge capacity and the efficient of lithium ion flow battery.
Summary of the invention
For solving the problems referred to above that the lithium ion flow battery exists, the present invention provides a kind of combination electrode active particle and preparation method thereof, and is applied to electrode suspension and lithium ion flow battery.
The present invention adopts following technical scheme:
But a kind of combination electrode active particle provided by the invention is made up of the electrode activity particle of low-density polymeric adhesive, electric conducting material and removal lithium embedded.Electric conducting material is scattered in the polymer adhesive, but the electrode activity particle of removal lithium embedded also is scattered in the polymer adhesive or is attached to the surface of polymer adhesive.
In the above-mentioned combination electrode active particle, polymer adhesive: electric conducting material: but the mass ratio of the electrode activity particle of removal lithium embedded is 5%～40%:1%～30%:40%～94%.The average grain diameter of above-mentioned combination electrode active particle is greater than 1 micron.
But the electrode activity particle of above-mentioned removal lithium embedded can be anodal active particle, also can be the negative electrode active particle.When but the electrode activity particle of above-mentioned removal lithium embedded was anodal active particle, the combination electrode active particle was the anode composite active particle; When but the electrode activity particle of above-mentioned removal lithium embedded was the negative electrode active particle, the combination electrode active particle was the composite negative pole active particle.
But above-mentioned anodal active particle is one or more mixtures of LiFePO 4, lithium manganese phosphate, lithium metasilicate, ferric metasilicate lithium, sulphate cpd, titanium sulphur compound, molybdenum sulfur compound, iron sulphur compound, doped lithium manganese oxide, lithium and cobalt oxides, Li-Ti oxide, lithium-barium oxide, Li, Ni, Mn oxide, lithium-nickel-cobalt-oxygen thing, lithium-nickel-manganese-cobalt oxidation thing and other removal lithium embedded compound.
One or more mixtures of the acieral that above-mentioned negative electrode active particle is reversible embedding lithium, silicon-base alloy, kamash alloy, lithium-barium oxide, Li-Ti oxide, material with carbon element.
Above-mentioned polymer adhesive is one or more mixtures in polypropylene, polyethylene, Kynoar, Kynoar-tetrafluoeopropene, polymethyl methacrylate, polyacrylonitrile, sodium carboxymethylcellulose, butadiene-styrene rubber, the polyethylene glycol oxide, or for polyacetylene, polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, gather one or more mixtures in two alkynes.
Above-mentioned electric conducting material is selected from one or more mixtures in amorphous carbon, carbon fiber, CNT, the Graphene.
The present invention provides a kind of preparation method of combination electrode active particle, and its step is following:
A) polymer adhesive is dissolved in forms polymer solution in the solvent; A certain amount of electric conducting material is joined in the polymer solution; The quality of electric conducting material is 10%～90% of a polymer adhesive quality, fully stirs, and electric conducting material is dispersed in the polymer solution;
B) a certain amount of electrode activity particle is added in the above-mentioned polymer solution, the quality of electrode activity particle is 1～18 times of polymer adhesive quality, and after fully stirring, oven dry obtains the combination electrode material mixture in 60 ~ 200 ℃ of scopes;
C) the combination electrode material mixture that makes is adopted jet mill grinding, perhaps, the combination electrode material mixture is put into water, the powerful stirring smashed, and adopts the hydraulic elutria-tion method classification then, obtains average grain diameter greater than 1 micron combination electrode active particle.
The solvent of above-mentioned steps in a) is selected from N-methyl pyrrolidone, N, N-DMAA, oxolane, N, dinethylformamide or dimethyl sulfoxide (DMSO), deionized water, ethanol.
The present invention further provides a kind of electrode suspension, and said electrode suspension is scattered in the electrolyte by above-mentioned combination electrode active particle and constitutes, and the combination electrode active particle is 1:0.2 ~ 1:4.5 with the quality of electrolyte than scope.The anodal suspension that is that contains the anode composite active particle in the said electrode suspension; What contain the composite negative pole active particle in the said electrode suspension is negative pole suspension.
Above-mentioned electrolyte adopts lithium hexafluoro phosphate or biethyl diacid lithium borate to be dissolved in organic solvent or ion liquid solution; Said organic solvent comprises one or more of dimethyl carbonate, diethyl carbonate, ethylene carbonate, propene carbonate; Said ionic liquid comprises N-methyl-N-propyl pyrrole-two (trifluoromethyl sulphonyl) imines, 1-methyl-4-butyl-pyridinium-two (trifluoromethyl sulphonyl) imines, 1, one or more mixtures of 2-dimethyl-3-N-butyl imidazole, 1-methyl-3-ethyl imidazol(e) tetrafluoro boric acid, 1-methyl-3-butyl imidazole hexafluorophosphoric acid.
The present invention further provides the application of above-mentioned electrode suspension in the lithium ion flow battery; Said lithium ion flow battery can use anodal suspension separately or use negative pole suspension separately, and said lithium ion flow battery also can use anodal suspension and negative pole suspension simultaneously.
Technical advantage of the present invention is embodied in:
Traditional lithium ion electrode of liquid flow cell suspension is made up of electrode activity particle, conductive agent and electrolyte, and wherein, electrode activity particle and conductive agent are scattered in the electrolyte.The density of electrode activity particle is much larger than density of electrolyte, and therefore, the electrode activity particle is sedimentation easily in electrolyte, thereby influences its mobile performance, causes it to lose activity.Conductive agent particle average grain diameter is less, is generally hundreds of even tens nanometers, in the cell reaction process, is easy to pass through the hole of porous septum, causes the generation of lithium ion flow battery short circuit accident.
Combination electrode active particle provided by the invention; Electric conducting material is scattered in the polymer adhesive; Polymer adhesive is become possess the polymer of electric conductivity; Promptly do not lose the electric conductivity of conductive agent, also tiny electric conducting material has been played fixation simultaneously, prevent that electric conducting material from passing through the porous septum hole and causing the short circuit of lithium ion flow battery; The present invention simultaneously is combined with each other electrode activity particle and polymer adhesive; Can reduce the density of electrode active material effectively; The electrode activity particle can be suspended in the electrolyte, reduce the speed of electrode active material sedimentation, thereby can improve the mobile performance of electrode suspension.In addition, the combination electrode active particle can not lose activity because of rapid sedimentation, and the utilance of electrode activity particle and the whole efficiency of battery get a promotion.
Embodiment
Embodiment one:
A kind of anode composite active particle and preparation method:
Polymer adhesive is Kynoar (PVDF), and solvent is N-methyl pyrrolidone (NMP), and electric conducting material is conductive black (amorphous carbon a kind of), and anodal active particle is a LiFePO4.
A) Kynoar (PVDF) is dissolved in formation solution in the N-methyl pyrrolidone (NMP); In conductive black and PVDF mass ratio is the ratio of 1:2; Conductive black is joined in the PVDF solution, and fully stirring is dispersed in the PVDF solution conductive black;
The LiFePO4 that b) will equate with the polymer adhesive quality adds in the PVDF solution of a) step preparation, fully stirs, and solution is dried under 120 ℃ of temperature, obtains the anode composite material blends alive of different-grain diameter;
C) the composite positive pole mixture of the different-grain diameter that makes is put into water, the powerful stirring smashed, and adopts the hydraulic elutria-tion method classification then, obtains average grain diameter greater than 1 micron combination electrode active particle.
The anode composite active particle of above-mentioned preparation is blended in (mass ratio of anode composite active particle and electrolyte is 1:1.5) in the 1mol/L LiPF6/PC+EC+DMC electrolyte, fully stirs, form anodal suspension.
Embodiment two:
A kind of composite negative pole active particle and preparation method:
Wherein polymer adhesive is Kynoar (PVDF), and solvent is N-methyl pyrrolidone (NMP), and electric conducting material is a Graphene, and the negative electrode active particle is a lithium titanate.
A) Kynoar (PVDF) being dissolved in formation solution in the N-methyl pyrrolidone (NMP), is the ratio of 1:1.5 in Graphene and PVDF mass ratio, and Graphene is joined in the PVDF solution, fully stirs Graphene is dispersed in the PVDF solution;
B) be that the lithium titanate of 10 times of polymer adhesive quality adds in the PVDF solution of a) step preparation with quality, fully stir, solution is dried under 120 ℃ of temperature, obtain the composite negative pole material mixture of different-grain diameter;
C) the composite negative pole material mixture of the different-grain diameter that makes is put into water, the powerful stirring smashed, and adopts the hydraulic elutria-tion method classification then, obtains average grain diameter greater than 1 micron combination electrode active particle.
The composite negative pole active particle of above-mentioned preparation is blended in 1mol/L LiPF
6In/PC+EC+DMC the electrolyte (mass ratio of composite negative pole active particle and electrolyte is 1:2), fully stir, form negative pole suspension.
Embodiment three:
A kind of anode composite active particle and preparation method:
Wherein polymer adhesive is the mixture of sodium carboxymethylcellulose and butadiene-styrene rubber, and solvent is a deionized water, and electric conducting material is a Graphene, and anodal active particle is a cobalt acid lithium.
A) mixture of sodium carboxymethylcellulose and butadiene-styrene rubber is dissolved in forms mixture aqueous solution in the deionized water; In Graphene and mixture quality than being the ratio of 1:2; Graphene is joined in the mixture aqueous solution, and fully stirring is dispersed in the mixture aqueous solution Graphene;
B) be that the cobalt acid lithium of 5 times of polymer adhesive quality adds in the mixture aqueous solution of a) step preparation with quality, fully stir, solution is dried under 80 ℃ of temperature, obtain the composite positive pole mixture of different-grain diameter;
C) the composite positive pole mixture to the different-grain diameter that makes carries out comminution by gas stream, and carries out classification, obtains average grain diameter greater than 1 micron combination electrode active particle.The anode composite active particle of above-mentioned preparation is blended in 1mol/LLiPF
6In/PC+EC+DMC the electrolyte (mass ratio of anode composite active particle and electrolyte is 1:0.8), fully stir, form anodal suspension.
Embodiment four:
A kind of anode composite active particle and preparation method:
Wherein polymer adhesive is the mixture of sodium carboxymethylcellulose and butadiene-styrene rubber, and solvent is a deionized water, and electric conducting material is a conductive black, and anodal active particle is a LiMn2O4.
A) mixture of sodium carboxymethylcellulose and butadiene-styrene rubber is dissolved in forms mixture aqueous solution in the deionized water; In conductive black and mixture quality than being the ratio of 1:2.5; Conductive black is joined in the mixture aqueous solution, and fully stirring is dispersed in the mixture aqueous solution conductive black;
B) LiMn2O4 that quality is equated with the polymer adhesive quality adds in the mixture aqueous solution of a) step preparation, fully stirs, and solution is dried under 80 ℃ of temperature, obtains the composite positive pole mixture of different-grain diameter;
C) the composite positive pole mixture to the different-grain diameter that makes carries out comminution by gas stream, and carries out classification, obtains average grain diameter greater than 1 micron combination electrode active particle.
The anode composite active particle of above-mentioned preparation is blended in contains 1mol/L LiPF
61-methyl-3-butyl imidazole hexafluorophosphoric acid ionic liquid in (mass ratio of anode composite active particle and solion is 1:0.7), fully stir, form anodal suspension.
Embodiment five:
A kind of anode composite active particle and preparation method:
Wherein polymer adhesive is self-conductive polymer poly pyrroles and Kynoar (PVDF) mixture according to the 4:1 mixed; Solvent is N-methyl pyrrolidone (NMP); Electric conducting material is a carbon fiber, and anodal active particle is the nickle cobalt lithium manganate ternary material.
A) mixture with self-conductive polymer poly pyrroles and Kynoar (PVDF) is dissolved in formation mixture solution in the N-methyl pyrrolidone (NMP); In carbon fiber and mixture quality than being the ratio of 1:2; Carbon fiber is joined in the mixture solution, and fully stirring is dispersed in the mixture solution carbon fiber;
B) be that the nickle cobalt lithium manganate ternary material of 2 times of polymer adhesive quality adds in the mixture solution of a) step preparation with quality, fully stir, solution is dried under 120 ℃ of temperature, obtain the composite positive pole mixture of different-grain diameter;
C) the composite positive pole mixture of the different-grain diameter that makes is put into water, the powerful stirring smashed, and adopts the hydraulic elutria-tion method classification then, obtains average grain diameter greater than 1 micron combination electrode active particle.
The anode composite active particle of above-mentioned preparation is blended in (mass ratio of anode composite active particle and electrolyte is 1:0.5) in the 1mol/L LiPF6/PC+EC+DMC electrolyte, fully stirs, form anodal suspension.
It should be noted that at last; The purpose of publicizing and implementing mode is to help further to understand the present invention; But it will be appreciated by those skilled in the art that: in the spirit and scope that do not break away from the present invention and appended claim, various replacements and to revise all be possible.Therefore, the present invention should not be limited to the disclosed content of embodiment, and the scope that the present invention requires to protect is as the criterion with the scope that claims define.
Claims (10)
1. combination electrode active particle; It is characterized in that; But the electrode activity particle by polymer adhesive, electric conducting material and removal lithium embedded is formed; Electric conducting material is scattered in the polymer adhesive, but the electrode activity Dispersion of Particles of removal lithium embedded is in polymer adhesive or be attached to the surface of polymer adhesive.
2. combination electrode active particle as claimed in claim 1 is characterized in that, in the above-mentioned combination electrode active particle, and polymer adhesive: electric conducting material: but the mass ratio of the electrode activity particle of removal lithium embedded is 5%～40%:1%～30%:40%～94%.
3. combination electrode active particle as claimed in claim 1; It is characterized in that; Said polymer adhesive is one or more mixtures in polypropylene, polyethylene, Kynoar, Kynoar-tetrafluoeopropene, polymethyl methacrylate, polyacrylonitrile, sodium carboxymethylcellulose, butadiene-styrene rubber, the polyethylene glycol oxide, or for polyacetylene, polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, gather one or more mixtures in two alkynes.
4. combination electrode active particle as claimed in claim 1; It is characterized in that; But the electrode activity particle of removal lithium embedded is anodal active particle or negative electrode active particle; But above-mentioned anodal active particle is one or more mixtures of LiFePO 4, lithium manganese phosphate, lithium metasilicate, ferric metasilicate lithium, sulphate cpd, titanium sulphur compound, molybdenum sulfur compound, iron sulphur compound, doped lithium manganese oxide, lithium and cobalt oxides, Li-Ti oxide, lithium-barium oxide, Li, Ni, Mn oxide, lithium-nickel-cobalt-oxygen thing, lithium-nickel-manganese-cobalt oxidation thing and other removal lithium embedded compound, one or more mixtures of the acieral that above-mentioned negative electrode active particle is reversible embedding lithium, silicon-base alloy, kamash alloy, lithium-barium oxide, Li-Ti oxide, material with carbon element.
5. combination electrode active particle as claimed in claim 1 is characterized in that, above-mentioned electric conducting material is selected from one or more mixtures in amorphous carbon, carbon fiber, CNT, the Graphene.
6. the preparation method of combination electrode active particle as claimed in claim 1, its step is following:
A) polymer adhesive is dissolved in forms solution in the solvent, electric conducting material is joined in this polymer solution, the quality of electric conducting material is 10%～90% of a polymer adhesive quality, fully stirs, and electric conducting material is dispersed in the polymer solution;
B) a certain amount of electrode activity particle is added in the above-mentioned polymer solution, the quality of electrode activity particle is 1～18 times of polymer adhesive quality, and after fully stirring, oven dry obtains the combination electrode material mixture in 60 ~ 200 ℃ of scopes;
C) the combination electrode material mixture that makes is adopted jet mill grinding, obtain average grain diameter greater than 1 micron combination electrode active particle; Perhaps, the combination electrode material mixture is put into water, the powerful stirring smashed, and adopts the hydraulic elutria-tion method classification then, obtains average grain diameter greater than 1 micron combination electrode active particle.
7. preparation method as claimed in claim 6 is characterized in that, the solvent of above-mentioned steps in a) is selected from N-methyl pyrrolidone, N, N-DMAA, oxolane, N, dinethylformamide or dimethyl sulfoxide (DMSO), deionized water, ethanol.
8. an electrode suspension is characterized in that, said electrode suspension is scattered in the electrolyte by combination electrode active particle as claimed in claim 1 and constitutes, and the combination electrode active particle is 1:0.2 ~ 1:4.5 with the quality of electrolyte than scope.
9. electrode suspension as claimed in claim 8; It is characterized in that; Said electrolyte adopts lithium hexafluoro phosphate or biethyl diacid lithium borate to be dissolved in organic solvent or ion liquid solution; Said organic solvent comprises one or more of dimethyl carbonate, diethyl carbonate, ethylene carbonate, propene carbonate; Said ionic liquid comprises N-methyl-N-propyl pyrrole-two (trifluoromethyl sulphonyl) imines, 1-methyl-4-butyl-pyridinium-two (trifluoromethyl sulphonyl) imines, 1, one or more mixtures of 2-dimethyl-3-N-butyl imidazole, 1-methyl-3-ethyl imidazol(e) tetrafluoro boric acid, 1-methyl-3-butyl imidazole hexafluorophosphoric acid.
10. the application of electrode suspension as claimed in claim 8 in the lithium ion flow battery.
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| CN103872370A (en) * | 2012-12-11 | 2014-06-18 | 苏州宝时得电动工具有限公司 | Flow battery |
| CN104300129A (en) * | 2013-07-19 | 2015-01-21 | 苏州宝时得电动工具有限公司 | Battery, battery cathode, battery cathode material and preparation method thereof |
| CN108511759A (en) * | 2018-03-28 | 2018-09-07 | 北京华灿康国际医药研究有限公司 | A kind of Medical Devices |
| CN108807982A (en) * | 2018-07-10 | 2018-11-13 | 江西星盈科技有限公司 | A kind of making formula of the positive electrode of high compacted density |
| CN108807904A (en) * | 2018-06-12 | 2018-11-13 | 四会市恒星智能科技有限公司 | A kind of preparation method of lithium battery modified phosphate iron lithium anode material |
| CN106033821B (en) * | 2015-03-17 | 2019-06-11 | 北京好风光储能技术有限公司 | A kind of preparation method of lithium ion flow battery electrode suspension |
| CN110299507A (en) * | 2018-03-23 | 2019-10-01 | 丰田自动车株式会社 | Lithium ion secondary battery |
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| CN103872370A (en) * | 2012-12-11 | 2014-06-18 | 苏州宝时得电动工具有限公司 | Flow battery |
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| CN108807982A (en) * | 2018-07-10 | 2018-11-13 | 江西星盈科技有限公司 | A kind of making formula of the positive electrode of high compacted density |
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Application publication date: 20120912 |