CN103165863A - Positive pole piece and preparation method thereof and battery - Google Patents
Positive pole piece and preparation method thereof and battery Download PDFInfo
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- CN103165863A CN103165863A CN2012105238426A CN201210523842A CN103165863A CN 103165863 A CN103165863 A CN 103165863A CN 2012105238426 A CN2012105238426 A CN 2012105238426A CN 201210523842 A CN201210523842 A CN 201210523842A CN 103165863 A CN103165863 A CN 103165863A
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Abstract
The invention provides a positive pole piece which is characterized by comprising a positive pole current collector, a buffer conducting layer and a positive pole active layer in a sequential stacking mode. The buffer conducting layer comprises phosphate, a first conductive agent and a first binder. The phosphate has the following general formula: LiMPO4, wherein M is selected from one of Fe, Mn and Co or a composite of a plurality of Fe, Mn and Co. The thickness of the buffer layer is 2-50 millimeters, and the grain size of the first conductive agent is smaller than 75 millimeters. In the buffer conductive layer, the phosphate content is 40-90wt%, the first conductive agent content is 5-10wt%, and the first binder content is 5-50wt%. Meanwhile, the invention further discloses a preparation method of the positive pole piece and a battery adopting the positive pole piece. The battery prepared from the provided positive pole piece has good over-charging performance and the safety of the battery is greatly promoted.
Description
Technical field
The present invention relates to a kind of anode pole piece and preparation method thereof, and the battery that adopts this anode pole piece.
Background technology
Lithium ion battery is a kind of chargeable secondary cell, lithium ion battery is large owing to having a capacity, safety and volume energy density advantages of higher, extensive use and various portable type electronic product, large-scale electric equipment, form huge application scale as fields such as energy storage, electric automobiles at present.
Along with the development of battery to the high-energy-density direction, the capacity of cell is more and more higher, and security performance more and more receives publicity, particularly in abuse, be easy to because charging device lost efficacy over-charging of battery, cause inner micro-short circuit, and then thermal runaway, very large potential safety hazard had.
Summary of the invention
In prior art, there is the problem of larger potential safety hazard in battery when overcharging in order to overcome, and the invention provides a kind of anode pole piece, and it has good over-charging, has greatly improved the fail safe of battery.
Anode pole piece provided by the invention comprises plus plate current-collecting body, buffering conductive layer and the anodal active layer that stacks gradually; Described buffering conductive layer comprises phosphate, the first conductive agent and the first binding agent, and described phosphate has following general formula: LiMPO
4, wherein M is selected from one or more compound in Fe, Mn, Co, and described buffer layer thickness is 2-50 μ m, and the first conductive agent particle diameter is less than 75 μ m; In described buffering conductive layer, phosphate content is 40-90wt%, and the first conductive agent content is 5-10wt%, and the first binder content is 5-50wt%.
Simultaneously, the invention also discloses the preparation method of above-mentioned anode pole piece, comprising:
S1, with phosphate, the first conductive agent, the first binding agent in mass ratio 40-90:5-10:5-50 mix, add solvent, obtain cushioning the conductive layer slurry, wherein, the solid content of buffering conductive layer slurry is 10-50%, viscosity is 200-1500Pas;
S2, will cushion the conductive layer slurry and be coated on plus plate current-collecting body, baking, forming thickness on plus plate current-collecting body is the buffering conductive layer of 2-50 μ m;
S3, form anodal active layer at described buffering conductive layer surface.
In addition, the invention also discloses a kind of battery, the battery core assembly and the electrolyte that comprise battery container and be positioned at battery container inside, described battery core assembly comprises anode pole piece, barrier film and the cathode pole piece that stacks gradually, and described anode pole piece is the anode pole piece that above-mentioned anode pole piece or employing said method prepare.
The present invention is by at plus plate current-collecting body surface-coated buffering conductive layer, and when the charging discharge range that is above standard, the buffering conductive layer can take off lithium, electronic conductance is significantly increased, thereby the anode pole piece internal resistance significantly increases, and battery obtains over-charge protective.
And, buffering conductive layer thickness in anode pole piece disclosed by the invention is 2-50 μ m, can't cause energy content of battery density to reduce, simultaneously, phosphate content is 40-90wt% in described buffering conductive layer, the first conductive agent content is 5-10wt%, the first binder content is under the prerequisite of 5-50wt%, adopt particle diameter less than the first conductive agent of 75 μ m, the very big anti-overcharge performance of the performance of degree avoids existing that anode pole piece is local forms conduction path and make when overcharging the anode pole piece internal resistance increase to be affected.
Description of drawings
Fig. 1 is anode pole piece cutaway view provided by the invention.
Fig. 2 is the cycle performance test curve of embodiment 1.
Fig. 3 is the discharge performance test curve of embodiment 1.
Wherein, 1, plus plate current-collecting body; 2, buffering conductive layer; 3, anodal active layer.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Anode pole piece disclosed by the invention comprises plus plate current-collecting body, buffering conductive layer and the anodal active layer that stacks gradually; Described buffering conductive layer comprises phosphate, the first conductive agent and the first binding agent, and described phosphate has following general formula: LiMPO
4, wherein M is selected from one or more compound in Fe, Mn, Co, and described buffer layer thickness is 2-50 μ m, and the first conductive agent particle diameter is less than 75 μ m; In described buffering conductive layer, phosphate content is 40-90wt%, and the first conductive agent content is 5-10wt%, and the first binder content is 5-50wt%.
Above-mentioned phosphate is well known in the art, for example LiFePO
4Can be commercially available.
Described the first conductive agent is selected from one or more in carbon black, graphite, acetylene black, carbon fiber, carbon nano-tube, Graphene.
Under preferable case, the first conductive agent particle diameter is less than 50 μ m, and is more favourable to further raising over-charging.
Described the first binding agent is selected from one or more in polyacrylic acid, polytetrafluoroethylene, Kynoar, butadiene-styrene rubber.
Described anodal active layer can adopt in prior art commonly used, and for example anodal active layer comprises positive electrode active materials, the second binding agent and the second conductive agent; In described anodal active layer, the addition of positive electrode active materials is 80-98%, and the addition of described the second binding agent is 1.5-10%, and the addition of the second conductive agent is 0.5-10%.
Concrete, described positive electrode active materials is selected from cobalt acid lithium, ferrous phosphate salt, LiMn2O4, silicate, reaches one or more in polynary nickel, cobalt, manganese multi-element composite material; Described the second conductive agent be selected from carbon black, graphite, acetylene black, carbon fiber, carbon nano-tube, Graphene, carbonyl nickel powder, copper powder, iron powder, zinc powder or aluminium powder one or more; Described the second binding agent is selected from one or more in polytetrafluoroethylene, Kynoar, butadiene-styrene rubber.
Simultaneously, the invention also discloses the preparation method of above-mentioned anode pole piece, comprising:
S1, with phosphate, the first conductive agent, the first binding agent in mass ratio 40-90:5-10:5-50 mix, add solvent, obtain cushioning the conductive layer slurry, wherein, the solid content of buffering conductive layer slurry is 10-50%, viscosity is 200-1500Pas;
S2, will cushion the conductive layer slurry and be coated on plus plate current-collecting body, baking, forming thickness on plus plate current-collecting body is the buffering conductive layer of 2-50 μ m;
S3, form anodal active layer at described buffering conductive layer surface.
Solvent in above-mentioned steps S1 is 1-METHYLPYRROLIDONE or deionized water.
In the present invention, as step S1, during preparation buffering conductive layer, solid content is transferred to 10-50%, viscosity transfers to 200-1500Pas, after drying on plus plate current-collecting body, be beneficial to phosphate and the first conductive agent reasonable layout in the buffering conductive layer at buffering conductive layer slurry, very favourable to improving over-charging.
After step S1, also comprise before S2 buffering conductive layer slurry is crossed 200 mesh sieves.
The preparation method of described anodal active layer comprises: positive electrode active materials, the second binding agent, the second conductive agent are mixed, then add 1-METHYLPYRROLIDONE to stir, obtain anodal active slurry, anodal active slurry is coated on the buffering conductive layer surface, then roll-in, die-cut with the speed of 1-8m/min.
As known in the art, with positive electrode active materials, the second binding agent, the second conductive agent in mass ratio 80-98:1.5-10:0.5-10 mix.
Can prepare anode pole piece disclosed by the invention by above-mentioned side, as shown in Figure 1, this anode pole piece comprises plus plate current-collecting body 1, buffering conductive layer 2 and the electrode activity layer 3 that stacks gradually from the bottom to top.
In addition, the invention also discloses the battery that adopts above-mentioned anode pole piece, the battery core assembly and the electrolyte that comprise battery container and be positioned at battery container inside, described battery core assembly comprises anode pole piece, barrier film and the cathode pole piece that stacks gradually, and described anode pole piece is the anode pole piece that preceding method prepares.
The present invention can adopt various material of the prior art for the not restriction of the plus plate current-collecting body/negative current collector, positive electrode active materials, negative active core-shell material, the second conductive agent, cathode conductive agent and the second binding agent that adopt.For example, described positive electrode active materials is selected from cobalt acid lithium, ferrous phosphate salt, LiMn2O4, silicate, reaches one or more in polynary nickel, cobalt, manganese multi-element composite material.Described negative electrode active material is selected from one or more in graphite, petroleum coke, organic cracking carbon, carbonaceous mesophase spherules, carbon fiber, ashbury metal, silicon alloy.Cathode conductive agent be selected from acetylene black, carbon nano-tube, Graphene, carbonyl nickel powder, copper powder, iron powder, zinc powder or aluminium powder one or more.Described negative pole binding agent is selected from one or more in polytetrafluoroethylene, Kynoar, carboxymethyl cellulose, butadiene-styrene rubber, silane coupler, titanate coupling agent, hydroxyethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, methylcellulose, polyacrylic acid.Described negative pole binding agent also can form jelly with solvent, and described solvent is selected from one or more in water, acetone, 1-METHYLPYRROLIDONE, oxolane, dimethyl sulfoxide (DMSO), methylethylketone, ethyl acetate.
The various electrode current collecting bodies that electrode current collecting body is known to the skilled person, for example, plus plate current-collecting body can be aluminium foil, aluminium net etc.Negative current collector can be Copper Foil.
In battery disclosed by the invention, anode pole piece is that method disclosed by the invention prepares, cathode pole piece can prepare by existing method, for example above-mentioned negative active core-shell material, butadiene-styrene rubber breast (SBR), methylcellulose (CMC) and super-P being added appropriate amount of deionized water mixes, be coated on 9 μ m Copper Foils, drying, after roll-in, die-cut getting final product.
It is commonly used that battery miscellaneous part, such as battery container, barrier film, electrolyte etc. are this area, restriction not.
For example, barrier film has electrical insulation capability and liquid retainability energy, is arranged between positive pole and negative pole, and is sealed in battery container together with positive pole, negative pole and electrolyte.Described barrier film can be this area various barrier films commonly used, and for example capable field technique personnel are at the modified poly ethylene felt of respectively producing the trade mark, modified polypropene felt, ultra-fine fibre glass felt, vinylon felt or nylon felt and the composite membrane of wettability microporous polyolefin film through welding or boning and form of known each manufacturer production.
Electrolyte is this area electrolyte commonly used, as the mixed solution of electrolyte lithium salt and nonaqueous solvents.Electrolyte lithium salt is selected from lithium hexafluoro phosphate (LiPF
6), one or more in lithium perchlorate, LiBF4, hexafluoroarsenate lithium, lithium halide, chlorine lithium aluminate, fluorocarbon based Sulfonic Lithium.Organic solvent can be selected from chain acid esters and ring-type acid esters mixed solution.Wherein, the chain acid esters can be for dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), methyl propyl carbonate (MPC), dipropyl carbonate (DPC) and other are fluorine-containing, sulfur-bearing or contain at least a in the chain organosilane ester of unsaturated bond.The ring-type acid esters can be ethylene carbonate (EC), propene carbonate (PC), vinylene carbonate (VC), gamma-butyrolacton (γ-BL), sultone and other are fluorine-containing, sulfur-bearing or contain one or more in the ring-type organosilane ester of unsaturated bond.In described electrolyte, the concentration of electrolyte lithium salt is generally 0.1-2mol/l, is preferably 0.8-1.2mol/l.
Described battery can adopt existing method to prepare, for example above-mentioned positive plate, polypropylene diaphragm and negative plate are overlapped into battery core successively, pack in battery container, inject the electrolyte in battery container, through seal, change into, partial volume, the standing battery that is made into.
By the following examples the present invention is further detailed.
The present embodiment is used for illustrating anode pole piece disclosed by the invention and preparation method thereof.
The preparation of buffering conductive layer slurry:
With 16 gram LiCoPO
4Active material (D
50Less than 5 μ m), 4 gram conductive carbon powder Super-P(D
50Less than 50 μ m), 20 gram binding agent PAA mix, and add 60 gram deionized water and stirring, adjusting viscosity 800-1200Pas crosses 200 mesh sieves.Be coated on 14 μ m aluminum foil current collector 85 degree vacuum bakeouts 1 hour.Form the thick buffering conductive layer of 25 μ m.
The anode pole piece preparation:
Weigh 95 gram cobalt acid lithium active materials, 2 gram conductive carbon powders, 3 gram binding agent PVDF mixing, add 200 gram NMP and stir, obtain active material slurry, it is coated on the aluminium collector that coating paste processed, control baking temperature and coating speed, obtain anode pole piece.
Battery is made:
Cathode pole piece preparation: take 95 gram graphite, 2.5 gram butadiene-styrene rubber breast SBR, 1.5 gram CMC CMC, 1 gram conductive agent Super-p, add appropriate deionized water to mix, be coated on 9 μ m Copper Foils and make cathode pole piece, then 85 degree vacuum bakeout is 8 hours, and the pole piece water content is controlled at below 200ppm.
With make positive/negative plate, according to operation: roll-in, die-cut, lamination, drying, fluid injection, seal, change into, partial volume, the standing 454261 model soft-package batteries that are made into.Fluid injection time perfusion electrolyte (1MLiPF wherein
6, EC:DMC:EMC=1:1:1), microporous polypropylene membrane is barrier film.
The over-charging of battery test: with the 1C/2C/3C constant-current constant-voltage charging, cut-ff voltage 10V, constant voltage time 12 hours, monitoring sample state.
The circulating battery test: with the 0.5C constant-current constant-voltage charging, cut-ff voltage 4.2V, cut-off current 0.05C; Standing 10min, discharge are with the 0.5C constant-current discharge, and cut-ff voltage 3.0V circulated for 300 weeks, capability retention.
The cycle performance test curve of battery is seen Fig. 2, and the discharge performance curve is seen Fig. 3.
The present embodiment is used for illustrating anode pole piece disclosed by the invention and preparation method thereof.
The preparation of buffering conductive layer slurry:
With 16 gram LiFePO
4Active material (D
50Less than 2 μ m), 4 gram conductive carbon powder Super-P(D
50Less than 50 μ m), 20 gram binding agent PAA mix, and add 60 gram deionized water and stirring, adjusting viscosity 800-1200Pas crosses 200 mesh sieves.Be coated on 14 μ m aluminum foil current collector 85 degree vacuum bakeouts 1 hour.Form the thick buffering conductive layer of 25 μ m.
Positive plate preparation, battery preparation method and method of testing are identical with embodiment 1.
The present embodiment is used for illustrating anode pole piece disclosed by the invention and preparation method thereof.
The preparation of buffering conductive layer slurry:
With 16 gram LiMnPO
4Active material (D
50Less than 2 μ m), 4 gram conductive carbon powder Super-P(D
50Less than 50 μ m), 20 gram binding agent PAA mix, and add 60 gram deionized water and stirring, adjusting viscosity 800-1200Pas crosses 200 mesh sieves.Be coated on 14 μ m aluminum foil current collector 85 degree vacuum bakeouts 1 hour.Form the thick buffering conductive layer of 25 μ m.
Positive plate preparation, battery preparation method and method of testing are identical with embodiment 1.
Comparative Examples 1
This Comparative Examples is used for comparative illustration anode pole piece disclosed by the invention and preparation method thereof.
Battery preparation method is similar to Example 1, and different is to cushion conductive layer for making.
Method of testing is identical with embodiment 1.
The test result of embodiment 1-3, Comparative Examples 1 is inserted table 1 and table 2.
Table 1
| Project | 3C/4.8V | 1C/ |
2C/ |
2C/10V | 3C/ |
| Embodiment | |||||
| 1 | Pass(10/10) | Pass(10/10) | Pass(10/10) | Pass(10/10) | Pass(10/10) |
| |
Pass(10/10) | Pass(10/10) | Pass(10/10) | Pass(10/10) | Fail(5/10) |
| |
Pass(10/10) | Pass(10/10) | Pass(10/10) | Pass(10/10) | Fail(2/10) |
| Comparative Examples 1 | Pass(10/10) | Fail(10/10) | Fail(8/10) | Fail(10/10) | Fail(10/10) |
Table 2
Can find out from the test result of table 1 and table 2 and Fig. 2 and Fig. 3, anode pole piece disclosed by the invention is used for battery, can significantly improve the over-charging of battery, and cycle performance and multiplying power discharging property also are improved.
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. an anode pole piece, is characterized in that, comprises the plus plate current-collecting body, buffering conductive layer and the anodal active layer that stack gradually; Described buffering conductive layer comprises phosphate, the first conductive agent and the first binding agent, and described phosphate has following general formula: LiMPO
4, wherein M is selected from one or more compound in Fe, Mn, Co, and described buffer layer thickness is 2-50 μ m, and the first conductive agent particle diameter is less than 75 μ m; In described buffering conductive layer, phosphate content is 40-90wt%, and the first conductive agent content is 5-10wt%, and the first binder content is 5-50wt%.
2. anode pole piece according to claim 1, is characterized in that, described the first conductive agent is selected from one or more in carbon black, graphite, acetylene black, carbon fiber, carbon nano-tube, Graphene, and described the first conductive agent particle diameter is less than 50 μ m; Described the first binding agent is selected from one or more in polyacrylic acid, polytetrafluoroethylene, Kynoar, butadiene-styrene rubber.
3. anode pole piece according to claim 1 and 2, is characterized in that, described anodal active layer comprises positive electrode active materials, the second binding agent and the second conductive agent; In described anodal active layer, the addition of positive electrode active materials is 80-98%, and the addition of described the second binding agent is 1.5-10%, and the addition of the second conductive agent is 0.5-10%.
4. anode pole piece according to claim 3, is characterized in that, described positive electrode active materials is selected from cobalt acid lithium, ferrous phosphate salt, LiMn2O4, silicate, reaches one or more in polynary nickel, cobalt, manganese multi-element composite material; Described the second conductive agent be selected from carbon black, graphite, acetylene black, carbon fiber, carbon nano-tube, Graphene, carbonyl nickel powder, copper powder, iron powder, zinc powder or aluminium powder one or more; Described the second binding agent is selected from one or more in polytetrafluoroethylene, Kynoar, butadiene-styrene rubber.
5. as the preparation method of the described anode pole piece of any one in claim 1-4, comprising:
S1, with phosphate, the first conductive agent, the first binding agent in mass ratio 40-90:5-10:5-50 mix, add solvent, obtain cushioning the conductive layer slurry, wherein, the solid content of buffering conductive layer slurry is 10-50%, viscosity is 200-1500Pas;
S2, will cushion the conductive layer slurry and be coated on plus plate current-collecting body, baking, forming thickness on plus plate current-collecting body is the buffering conductive layer of 2-50 μ m;
S3, form anodal active layer at described buffering conductive layer surface.
6. preparation method according to claim 5, is characterized in that, after step S1, also comprises before S2 buffering conductive layer slurry is crossed 200 mesh sieves.
7. according to claim 5 or 6 described preparation methods, is characterized in that, described solvent is 1-METHYLPYRROLIDONE or deionized water.
8. preparation method according to claim 7, it is characterized in that, the preparation method of described anodal active layer comprises: positive electrode active materials, the second binding agent, the second conductive agent are mixed, then add 1-METHYLPYRROLIDONE to stir, obtain anodal active slurry, anodal active slurry is coated on the buffering conductive layer surface, then roll-in, die-cut with the speed of 1-8m/min.
9. preparation method according to claim 8, is characterized in that, mixing positive electrode active materials, the second binding agent, the second conductive agent in mass ratio, 80-98:1.5-10:0.5-10 mixes.
10. battery, the battery core assembly and the electrolyte that comprise battery container and be positioned at battery container inside, described battery core assembly comprises anode pole piece, barrier film and the cathode pole piece that stacks gradually, it is characterized in that, described anode pole piece is the anode pole piece that in claim 5-9, the described method of any one prepares.
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