CN100341174C - Method for modifying lithium ion battery cathode - Google Patents
Method for modifying lithium ion battery cathode Download PDFInfo
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- CN100341174C CN100341174C CNB2005100428000A CN200510042800A CN100341174C CN 100341174 C CN100341174 C CN 100341174C CN B2005100428000 A CNB2005100428000 A CN B2005100428000A CN 200510042800 A CN200510042800 A CN 200510042800A CN 100341174 C CN100341174 C CN 100341174C
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- benzenesulfonic acid
- methyl benzenesulfonic
- lithium ion
- ion battery
- mixture
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- 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 present invention relates to a method for modifying a lithium ion battery cathode. Firstly, p-toluensulfonic acid natrium, p-toluensulfonic acid and pyrrole are solved into water for making mixed liquid; secondly, lithium ion cathode active material, conducting carbon black and binder are mixed for making mixture which is provided with 1-methyl 2-pyrrolidone solvent for making slurry; finally, an aluminum foil of a current collector is coated with the slurry, and the lithium ion battery cathode is made after desiccation. The cathode is immersed into the mixed liquid, and the polymerization is carried out for 1 to 300 seconds under the electric current density from 0.1 to 1.0 mA/cm<2>. Ion removing water is used for washing away the foreign matter on an electrode surface, and then the cathode is heated for 1 to 48 hours at the temperature from 60 DEG C to 300 DEG C. After the lithium ion cathode active material is provided with polypyrrole decoration, the dissolving quantity of the lithium ion battery cathode can be obviously reduced, and the discharging currents can be increased. Thus, the capacity attenuation of the cathode can be inhibited, and the cycle performance is improved.
Description
Technical field
The present invention relates to a kind of manufacture method of lithium ion battery, particularly a kind of method of modifying of lithium-ion battery pole winding core needle.
Background technology
Since the nineties in last century because have the operating voltage height, advantages such as energy density is big, self discharge is little, memory-less effect, lithium ion battery becomes secondary cell of new generation.In recent years, along with developing rapidly of portable electric appts such as notebook computer, mobile phone, the demand of lithium ion battery grows with each passing day; In addition, the greatly developing of electric vehicles such as electric automobile, electric bicycle makes the manufacturing technology of lithium ion battery enjoy the concern of researcher and production firm, becomes the emphasis and the focus of 21 century research.
At present, the LiCoO that mainly contains layer structure of lithium-ion battery pole winding core needle
2, LiNiO
2LiMn with spinel structure
2O
4Business-like LiCoO
2Material exists resource scarcity, shortcoming that cost is high, and LiMn
2O
4Have aboundresources, environmental friendliness, easily reclaim, prepare, take off advantages such as the lithium amount is big especially easily, receive much attention, so it becomes commercialization LiCoO
2One of best substitution material, become current research focus.But because LiMn
2O
4Cycle performance is relatively poor, becomes the obstacle of its commercialization maximum.
LiMn
2O
4Capacity attenuation cause by many factors, such as in charge and discharge process Mn
3+Understand the structural stability, the dissolving of manganese in electrolyte, the cubic phase Li that electrode surface forms the stability difference that the Jahn-Teller effect take place and influence material
2Mn
2O
4, the anoxic spinel structure formation, active material and electrolyte between redox reaction, electrode polarization and cause increase of cell resistance or the like.In order to suppress LiMn
2O
4Capacity attenuation, improve LiMn
2O
4Cycle performance, domestic and international research person studies from following two aspects:
(1) body is assorted disastrously mutually
People such as M.Wakihara adopt Co
3O
4Li doped Mn
2O
4Form LiCo
1/6Mn
11/6O
4, studies show that: charge and discharge cycles is after 30 weeks, LiMn
2O
4Capacity attenuation reach 25%, and LiCo
1/6Mn
11/6O
4Only be 5% (Solid State Ionics 111 (1998) 153-159).People such as G.X.Wang and D.H.Bradhurst has studied and has mixed Cr front and back LiMn
2O
4Cycle performance, the result shows: LiMn
2O
4Though initial capacity reaches 130mAh/g, only be 90mAh/g after the circulation of 50 weeks, capacity attenuation 31.8%; LiCr
0.04Mn
1.96O
4Initial capacity is 122mAh/g, is 114mAh/g after the circulation of 50 weeks, capacity attenuation 6.6% (Solid StateIonics 120 (1999) 95-101).
(2) surface coats
People such as D.Aurbach adopt MgO to coat LiMn
2O
4, discover: at 60 ℃ of circulate down 100 weeks, not LiMn of Bao Fuing
2O
4Capacity attenuation 22.1%; And the LiMn after coating
2O
4Decay to 12.3%, show excellent cycle performance (Electrochemistry Communications 5 (2003) 940-945).People such as Seung-Won Lee adopt sol-gel method at LiMn
2O
4The surface coats Al
2O
3, not only improved LiMn
2O
4Initial capacity, and improved LiMn
2O
4Cycle performance (Journal of PowerSources 126 (2004) 150-155).But above method of modifying process conditions complexity, cost are higher, are unfavorable for promoting.
For other lithium-ion battery pole winding core needle LiCoO
2, LiNiO
2, LiMnO
2, LiFePO
4Negative electrode because negative electrode has added a certain amount of organic bond when preparing, cause electrode electricity sun bigger.In addition, because active material of cathode directly contacts with electrolyte, form one deck interfacial film easily in battery.It is unfavorable that all anticathode flash-over characteristic of both of these case constitutes.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of method of modifying of lithium-ion battery pole winding core needle is provided, the method technology is simple, and cost is low, and can significantly suppress the capacity attenuation of lithium ion battery and improve its flash-over characteristic.
For achieving the above object, the technical solution used in the present invention is: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.01～0.5mol/L, the p-methyl benzenesulfonic acid of 0.01～0.5mol/L and the pyrroles's mixed liquor of 0.05～0.5mol/L made soluble in water; Then with lithium ion active material of cathode, conductive carbon black and binding agent by 65～90: 5～20: 5～15 mass ratio is mixed and made into mixture, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 30～80% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 10～1000 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.1-1.0mA/cm in current density
2Following polymerization 1-300s with deionized water cleaning electrode surface, places 60-300 ℃ of following heat treatment 1-48h to get final product.
Lithium ion active material of cathode of the present invention is LiMn
2O
4, LiCoO
2, LiNiO
2, LiMnO
2Or LiFePO
4Binding agent is Kynoar or polytetrafluoroethylene.
Because the lithium ion active material of cathode is by behind the polypyrrole modifying, can significantly reduce the meltage of lithium ion battery cathode, improve its discharging current, the capacity attenuation that therefore can suppress negative electrode, improved its cycle performance, and adopted that method technology of the present invention is simple, the cycle is short, production cost is low.
Description of drawings
Accompanying drawing is LiMn before and after the modification of the present invention
2O
4Cycle performance effect comparison diagram, wherein abscissa is the charge and discharge cycles number of times, ordinate is a discharge capacity.
Embodiment
Embodiment 1: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.5mol/L, the p-methyl benzenesulfonic acid of 0.01mol/L and the pyrroles's mixed liquor of 0.05mol/L made soluble in water; Then with LiMn
2O
4, conductive carbon black and Kynoar be mixed and made into mixture by 65: 20: 15 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 50% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 100 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.8mA/cm in current density
2Following polymerization 60 seconds with deionized water cleaning electrode surface, places 60 ℃ of following heat treatments to get final product in 48 hours.
Embodiment 2: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.01mol/L, the p-methyl benzenesulfonic acid of 0.3mol/L and the pyrroles's mixed liquor of 0.4mol/L made soluble in water; Then with LiCoO
2, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 90: 5: 5 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 80% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 1000 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.1mA/cm in current density
2Following polyase 13 00 second with deionized water cleaning electrode surface, places 150 ℃ of following heat treatments to get final product in 18 hours.
Embodiment 3: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.3mol/L, the p-methyl benzenesulfonic acid of 0.5mol/L and the pyrroles's mixed liquor of 0.1mol/L made soluble in water; Then with LiNiO
2, conductive carbon black and Kynoar be mixed and made into mixture by 80: 7: 13 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 60% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 400 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.5mA/cm in current density
2Following polymerization 150 seconds with deionized water cleaning electrode surface, places 300 ℃ of following heat treatments to get final product in 1 hour.
Embodiment 4: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.06mol/L, the p-methyl benzenesulfonic acid of 0.4mol/L and the pyrroles's mixed liquor of 0.5mol/L made soluble in water; Then with LiMnO
2, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 75: 15: 10 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 30% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 10 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 1.0mA/cm in current density
2Following polymerization 1 second with deionized water cleaning electrode surface, places 100 ℃ of following heat treatments to get final product in 6 hours.
Embodiment 5: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.4mol/L, the p-methyl benzenesulfonic acid of 0.06mol/L and the pyrroles's mixed liquor of 0.08mol/L made soluble in water; Then with LiFePO
4, conductive carbon black and Kynoar be mixed and made into mixture by 70: 18: 12 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 70% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 55 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.3mA/cm in current density
2Following polymerization 40 seconds with deionized water cleaning electrode surface, places 200 ℃ of following heat treatments to get final product in 2 hours.
Embodiment 6: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.2mol/L, the p-methyl benzenesulfonic acid of 0.2mol/L and the pyrroles's mixed liquor of 0.2mol/L made soluble in water; Then with LiMn
2O
4, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 85: 7: 8 mass ratio, adding the mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture in mixture is 50% slurry; Last on the collector aluminium foil applied thickness be that the slurry of 500 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.6mA/cm in current density
2Following polymerization 200 seconds, the impurity with deionized water cleaning electrode surface places 230 ℃ of following heat treatments to get final product in 35 hours.
Adopt the LiMn of modification of the present invention referring to accompanying drawing
2O
4Negative electrode is assembled into breadboard simulated battery (anode employing metal lithium sheet), and charge-discharge test is the result show: LiMn after the modification
2O
4Height ratio capacity be 121mAh/g, 100 week of circulation the back specific capacities be 111mAh/g, capacity attenuation only is 8.3%, 150 week of circulation the back specific capacities be 109mAh/g, capacity attenuation only is 9.9%; And unmodified LiMn
2O
4Electrode, initial capacity are 116mAh/g, and specific capacity is 89mAh/g after 100 weeks of circulation, capacity attenuation 23.3%, and circulation 150 all backs specific capacities are 62mAh/g, capacity attenuation is up to 46.6%.
Claims (9)
1, the method for modifying of lithium ion battery cathode is characterized in that:
1) at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.01～0.5mol/L, the p-methyl benzenesulfonic acid of 0.01～0.5mol/L and the pyrroles's mixed liquor of 0.05～0.5mol/L made soluble in water;
2) then with lithium ion active material of cathode, conductive carbon black and binding agent by 65～90: 5～20: 5～15 mass ratio is mixed and made into mixture, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 30～80% slurry in mixture;
3) last on the collector aluminium foil applied thickness be that the slurry of 10～1000 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.1-1.0mA/cm in current density
2Following polymerization 1-300s with deionized water cleaning electrode surface, places 60-300 ℃ of following heat treatment 1-48h to get final product.
2, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: said lithium ion active material of cathode is LiMn
2O
4, LiCoO
2, LiNiO
2, LiMnO
2Or LiFePO
4
3, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: said binding agent is Kynoar or polytetrafluoroethylene.
4, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.5mol/L, the p-methyl benzenesulfonic acid of 0.01mol/L and the pyrroles's mixed liquor of 0.05mol/L made soluble in water; Then with LiMn
2O
4, conductive carbon black and Kynoar be mixed and made into mixture by 65: 20: 15 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 50% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 100 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.8mA/cm in current density
2Following polymerization 60 seconds with deionized water cleaning electrode surface, places 60 ℃ of following heat treatments to get final product in 48 hours.
5, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.01mol/L, the p-methyl benzenesulfonic acid of 0.3mol/L and the pyrroles's mixed liquor of 0.4mol/L made soluble in water; Then with LiCoO
2, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 90: 5: 5 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 80% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 1000 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.1mA/cm in current density
2Following polyase 13 00 second with deionized water cleaning electrode surface, places 150 ℃ of following heat treatments to get final product in 18 hours.
6, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.3mol/L, the p-methyl benzenesulfonic acid of 0.5mol/L and the pyrroles's mixed liquor of 0.1mol/L made soluble in water; Then with LiNiO
2, conductive carbon black and Kynoar be mixed and made into mixture by 80: 7: 13 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 60% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 400 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.5mA/cm in current density
2Following polymerization 150 seconds with deionized water cleaning electrode surface, places 300 ℃ of following heat treatments to get final product in 1 hour.
7, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.06mol/L, the p-methyl benzenesulfonic acid of 0.4mol/L and the pyrroles's mixed liquor of 0.5mol/L made soluble in water; Then with LiMnO
2, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 75: 15: 10 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 30% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 10 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 1.0mA/cm in current density
2Following polymerization 1 second with deionized water cleaning electrode surface, places 100 ℃ of following heat treatments to get final product in 6 hours.
8, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.4mol/L, the p-methyl benzenesulfonic acid of 0.06mol/L and the pyrroles's mixed liquor of 0.08mol/L made soluble in water; Then with LiFePO
4, conductive carbon black and Kynoar be mixed and made into mixture by 70: 18: 12 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 70% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 55 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.3mA/cm in current density
2Following polymerization 40 seconds with deionized water cleaning electrode surface, places 200 ℃ of following heat treatments to get final product in 2 hours.
9, the method for modifying of lithium ion battery cathode according to claim 1 is characterized in that: at first with p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid and the pyrroles p-methyl benzenesulfonic acid sodium that contains 0.2mol/L, the p-methyl benzenesulfonic acid of 0.2mol/L and the pyrroles's mixed liquor of 0.2mol/L made soluble in water; Then with LiMn
2O
4, conductive carbon black and polytetrafluoroethylene be mixed and made into mixture by 85: 7: 8 mass ratio, adds mass concentration that 1-methyl 2-Pyrrolidone solvent obtains mixture and be 50% slurry in mixture; Last on the collector aluminium foil applied thickness be that the slurry of 500 μ m makes lithium ion battery cathode after drying, this negative electrode is immersed in mixed liquor, be 0.6mA/cm in current density
2Following polymerization 200 seconds, the impurity with deionized water cleaning electrode surface places 230 ℃ of following heat treatments to get final product in 35 hours.
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|---|---|---|---|
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020006134A (en) * | 2000-07-11 | 2002-01-19 | 이희우 | Conducting Polymer/Manganese Oxide Composite Cathode Material for Lithium Secondary Batteries and Method for Making Same |
| JP2003297424A (en) * | 2002-04-04 | 2003-10-17 | Sony Corp | Nonaqueous electrolyte battery and method for manufacturing the same |
| CN1574429A (en) * | 2003-06-11 | 2005-02-02 | 株式会社日立制作所 | Positive electrode material, its manufacturing method and lithium batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020006134A (en) * | 2000-07-11 | 2002-01-19 | 이희우 | Conducting Polymer/Manganese Oxide Composite Cathode Material for Lithium Secondary Batteries and Method for Making Same |
| JP2003297424A (en) * | 2002-04-04 | 2003-10-17 | Sony Corp | Nonaqueous electrolyte battery and method for manufacturing the same |
| CN1574429A (en) * | 2003-06-11 | 2005-02-02 | 株式会社日立制作所 | Positive electrode material, its manufacturing method and lithium batteries |
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