CN101436655A - Cathode pole piece of lithium ion secondary battery and preparation method thereof - Google Patents
Cathode pole piece of lithium ion secondary battery and preparation method thereof Download PDFInfo
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- CN101436655A CN101436655A CNA200710177231XA CN200710177231A CN101436655A CN 101436655 A CN101436655 A CN 101436655A CN A200710177231X A CNA200710177231X A CN A200710177231XA CN 200710177231 A CN200710177231 A CN 200710177231A CN 101436655 A CN101436655 A CN 101436655A
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Abstract
The invention provides a negative pole piece of a lithium ion secondary cell, which comprises: a current collection body; a negative pole material layer deposited on the current collection body wherein the negative pole material layer comprises an active material layer containing one or two of the elements of silicon and tin; and a polymer coating coated on the negative pole material layer. Compared with the prior common traditional graphite negative pole piece, the negative pole piece of the lithium ion secondary cell saves the traditionally used diaphragm special for a lithium ion cell, and has better battery performances such as charging and discharging capacity, current density, discharging capability and cycle performance. Besides, the production cost is reduced, the production efficiency is improved, electrolyte flowing in the cell is reduced, and the security of the cell is improved.
Description
Technical field
The present invention relates to a kind of cathode pole piece of lithium ion secondary battery and preparation method thereof.
Background technology
Recently, size and weight minimizing along with portable set, to having the demand of high-energy-density and high power density battery, and, make that the requirement that obtains the lithium rechargeable battery that size is littler, weight is lighter, energy storage capability is higher, charge-discharge performance is more excellent is more urgent for improving the growth requirement that environment uses large power, electrically electrical automobile etc.
Lithium ion battery is divided into liquid lithium ionic cell and solid lithium ion battery, and liquid lithium ionic cell uses liquid electrolyte.Solid lithium ion battery is generally known as polymer Li-ion battery, and what this battery contained a kind of half-dried attitude or was called gel state is adsorbed on the electrolyte that forms in the polymer hole by liquid electrolyte.As lithium ion battery of new generation, polymer Li-ion battery has more superior electrochemical properties and better security performance.In addition,, can adapt to different application demands widely, therefore be considered to the most potential novel battery in future because polymer Li-ion battery has flexibility more fully aspect shaped design.
The negative material of polymer Li-ion battery remains traditional carbon-based material at present, for example hard carbon, Delanium and native graphite.The theoretical specific capacity of graphite is 372mAh/g, and graphite active material density low (solid density is 2.2g/cc), so the energy density of carbon back cathode pole piece is on the low side.The process of traditional preparation negative pole is relatively complicated, be described as: at first prepare graphitic carbon or carbonaceous mesophase spherules powder, then add conductive agent, bonding agent and other additive therein and form slurry, utilize coating machine on copper (Cu) collector, to be coated with then, toast, roll the cathode pole piece that technologies such as sheet obtain lithium ion battery again.The pole piece that adopts method for preparing also needs to use the special-purpose barrier film of lithium ion battery when making battery.This method complex procedures, there is certain environmental pollution in the cost height, and rete is thicker, and battery behaviors such as charge/discharge capacity, cycle life, current density, discharge also have certain limitation.Therefore, the someone has proposed the substitute of the non-material with carbon element of jumbo negative pole (material that for example contains silicon, tin, aluminium and W elements) as the conventional graphite negative material.
Application number is that 200380104240.6 Chinese patent discloses a kind of particle that comprises the carbonaceous material of the siliceous and/or silicon compound on the part surface at least that is deposited in the carbon granule with graphite-structure.Wherein disclose a kind of execution mode and be at carbon granule as nuclear, the carbonaceous material of siliceous and/or silicon compound has been deposited on the part surface at least of described carbon granule with graphite-structure.The preparation method is as follows: at first adopt the carbon granule with graphite-structure as the particle that serves as nuclear, the composition that then will contain polymer is deposited on to the described carbon granule of small part, and heat-treat, purpose is expansion and the contraction for the compound generation volume that prevents carbon granule, silicon and silicon, thereby cause dropping or separating of silicon and silicon compound, perhaps carbon fiber dropping or peeling off.This polymer is the compound that carbon fiber and silicon/silicon compound is had adhesive force, as long as this polymer shows when (as mixing, stir, remove solvent or heat treatment) compression, crooked, glass impact, the tolerance that stretches or the active force that causes such as tear standing any processing, thereby this polymer is gone up substantially and can not be caused peeling off from carbon fiber.The composition that repeats again to contain carbon fiber and silicon/silicon compound is deposited on the carbonaceous particle, subsequently the composition that is deposited on the carbonaceous material is cured 1-20 time, afterwards the carbonaceous particle that obtains is heat-treated, removing solvent by heated-air drying or vacuum drying method.The secondary cell that adopts the technical scheme of this invention finally to obtain has the charging-flash-over characteristic excellent characteristics under high discharge capacity, cycle characteristics and the big electric current.
Summary of the invention
An object of the present invention is to provide a kind of cathode pole piece of lithium ion secondary battery, this cathode pole piece has the favorable charge-discharge capacity, good current density discharge capability, and have excellent cycle performance.
Another object of the present invention provides the preparation method of preparation cathode pole piece of lithium ion secondary battery.
In the present invention, used term " porosity " is meant the shared ratio in polymer coating mesopore of unit are.
Among the present invention, used term " amorphous carbon " is meant the carbon with impalpable structure.
The invention provides a kind of cathode pole piece of lithium rechargeable battery, this cathode pole piece comprises:
Collector,
Be deposited on the negative electrode material layer on the collector, wherein comprise the active material layer that contains a kind of in silicon, the tin element or two kinds,
Be coated in the polymer coating on the negative electrode material layer.
Unlike the prior art, the present invention directly is deposited on coat polymers coating on the negative electrode material layer that comprises silicon, tin element particle on the collector, thereby has saved the special-purpose barrier film of the lithium ion battery that uses traditionally.The purpose that adopts silicon, tin element particle is because they are to have attracting deposits and discharge Li
+The negative active core-shell material of ability.
Preferably, described collector is Copper Foil or aluminium foil, more preferably Copper Foil.
Preferably, described negative electrode material layer also comprises one deck carbon-coating at least, and described carbon-coating and active material layer space are arranged on the collector, and the layer that contacts with described collector is an active material layer.The purpose that adds carbon-coating is specific capacity and the cycle performance in order to keep active material.Described negative electrode material layer has impalpable structure, and the number of plies of carbon-coating and active material layer is respectively 1-4 layers.Along with the increase of the number of plies of carbon-coating and active material layer, the charging and discharging capabilities of cathode pole piece increases.
Described active material layer preferably also comprises doped chemical, and this doped chemical is selected from one or more in aluminium, copper, boron and the iron.The purpose of adding above-mentioned element at active material layer is to play the expansion that suppresses the negative electrode material layer volume, and has better cycle ability with respect to the active material layer that does not add above-mentioned element.
The preferred gross thickness of described negative electrode material layer is 5-20 μ m.No matter the carbon-coating of negative electrode material layer and active material layer always total which floor, its gross thickness preferably is controlled at 5-20 μ m, purpose is in order to make it have higher specific capacity and excellent cycle performance.
Preferably, element in the described active material layer and the carbon in the described carbon-coating all exist with impalpable structure.
Preferably, the thickness of described polymer coating is 10-50 μ m, and the porosity of described polymer coating is 40-60%.Thickness is excessive, porosity is crossed the chemical property that the young pathbreaker influences battery; Thickness is too small, porosity is crossed the security performance that senior general influences battery.
Preferably, the polymer of described polymer coating is selected from polyolefin, fluorine-containing polyolefin, fluorine-containing polyolefin copolymer, polyacrylate, one or more in polyacrylonitrile and the poly-alkyl oxide.
Described polymer is one or more in polyethylene, Kynoar, Kynoar-hexafluoropropylene, polymethyl methacrylate, polyacrylonitrile, poly(ethylene oxide), the PPOX more preferably.
Preferably, also comprise oxide particle in the described polymer coating, and described oxide particle is 1%-30% of a polymer quality.The content of oxide particle is 1%-30% can be so that cathode pole piece conductivity the best.
More preferably, described oxide particle is SiO
2, TiO
2, Al
2O
3With among the MgO one or more, the purpose that adds oxide particle in polymer coating is mechanical strength and the conductivity in order to improve polymer coating.
Another aspect of the present invention also provides a kind of method for preparing cathode pole piece of the present invention, and this method may further comprise the steps:
A) method of employing vapour deposition deposits negative electrode material layer on collector, forms the collector with negative electrode material layer,
B) then polymer coating is dissolved in the organic solvent, forms polymer solution,
C) more described polymer solution is coated on the collector with negative electrode material layer, after the film forming, places baking oven dry, remove solvent, form described cathode pole piece.
The layer thickness of the polymer coating among the present invention is 10-50 μ m, wherein polymer is selected from polyolefin, fluorine-containing polyolefin, fluorine-containing polyolefin copolymer, polyacrylate, in polyacrylonitrile and the poly-alkyl oxide one or more, the solvent of polymer is an acetone, butanone, N-methyl pyrrolidone, dimethyl formamide, dimethylacetylamide, in the dimethyl sulfoxide (DMSO) one or more, oxide particle and second kind of solvent are made organic suspension liquid, and second kind of solvent wherein is selected from ethanol, butanols, oxolane, ethylene carbonate, dimethyl carbonate, in the diethyl carbonate one or more.Also be added with plasticizer in the slurry system of polymer, common plasticizers is ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, and purpose is in order to increase the porosity of polymer porous film.The volume ratio of the solvent of polymer in the present invention and second kind of solvent is 3:1～20:1.The method of polymer-coated on collector is The tape casting, rubbing method or high pressure painting method.
Advantage of the present invention is: the deposition negative electrode material layer is by using magnetron sputtering, the auxiliary physical gas-phase deposite method of multi-arc ion coating gas ions on collector in the present invention, use the solid target as sedimentary origin, operating voltage is 100-1000V, and the target current density is 5-50mA/cm
2Working gas is an inert gas argon, reacting gas O
2, N
2Deng, operating pressure is less than 10Pa.Compare with conventional graphite negative pole commonly used at present, this cathode pole piece is directly finished in the collector deposition from raw material, and the thickness of negative electrode material layer is thinner, and the active material adhesion is higher, and battery performances such as charge/discharge capacity, current density discharge capability and cycle characteristics are more excellent simultaneously.
Another advantage of the present invention is at the direct coat polymers material of negative terminal surface, utilize phase separation method to form the porous rete, saved the special-purpose barrier film of the lithium ion battery that uses traditionally, reduced production cost, improved production efficiency, reduced the electrolyte that inside battery flows, the fail safe that has improved battery, and the cathode pole piece of the lithium rechargeable battery among the present invention not only can be used for solid lithium ion battery and also can be used for liquid lithium ionic cell.
Description of drawings
The cathode pole piece of lithium ion secondary battery sectional schematic diagram of active material layer that Fig. 1 prepares on collector for the present invention and polymer coating.
The active material layer of the interpolation doped chemical that Fig. 2 prepares on collector for the present invention and the cathode pole piece of lithium ion secondary battery sectional schematic diagram of polymer coating.
The cathode pole piece of lithium ion secondary battery sectional schematic diagram of active material layer/carbon-coating that Fig. 3 prepares on collector for the present invention/active material layer/carbon-coating and polymer coating.
Fig. 4 is the electrochemical properties resolution chart of the negative material in the embodiment of the present invention, and two Trendline among the figure are respectively the Trendline of the charging and the discharge of cathode pole piece.
Fig. 5 is a cathode pole piece cycle performance curve chart corresponding among the embodiment 1.
Fig. 6 is a cathode pole piece cycle performance curve chart corresponding among the embodiment 2.
Fig. 7 is a cathode pole piece cycle performance curve chart corresponding among the embodiment 3.
In the drawings:
1-collector; 2-active material layer; 3-polymer coating; 4-doped chemical; 5-carbon-coating.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Utilize the magnetically controlled DC sputtering technology, piecing together target with crystal Si, Al is target, is deposition Si-Al laminated film on the Cu paper tinsel of 15 μ m at thickness, forms the collector with negative electrode material layer.Target as sputter power is 500W, and gas Ar flow is 58sccm, and gained negative material bed thickness is 10 μ m, and wherein the atomic ratio of Si:Al is about 100:50.
The preparation of polymer coating: select for use Kynoar-hexafluoropropylene (PVDF-HFP) as the polymer coating material, butanone is a solvent, and diethyl carbonate is a plasticizer, and oxide particle is selected SiO for use
2, oxide particle is dissolved in the butanols, and butanone, butanols volume ratio are 3:1, SiO
2Content is 10% of PVDF-HFP weight.With the SiO that is dissolved in the butanols
2Join successively among the PVDF-HFP that is dissolved in the butanone with the plasticizer diethyl carbonate, fully mix, disperse, form polymer coating solution, adopt the scraper rubbing method to be to have film forming on the collector of negative electrode material layer, thicknesses of layers is 20 μ m.After the rete moulding in 80 ℃ of vacuum drying ovens dry 24h, obtain porosity and be 40% polymer coating.
The positive electrode pole piece that lithium ion battery uses in the embodiment of the invention can prepare according to following method: utilize solvent such as N-first class-2-pyrrolidones (NMP), disperse the mixture LiMO of composite oxides
2(wherein M is at least a transition metal) is as LixCoO
2, LixNiO
2, LiMn
2O
4, LixMnO
3Deng, use electric conducting material such as carbon black and binding agent such as Kynoar (PVDF) simultaneously, adopt the mixture that forms to apply such as above the aluminum foil current collector.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.4mA/cm
2, the charging/discharging voltage scope is at 0～2.0V.The specific discharge capacity of cathode pole piece can reach 1000mAh/g, and 200 times circulation volume remains on about 80%.
Utilize radiofrequency magnetron sputtering technology, be target with crystal Si-Al assembly target, graphite target simultaneously, be to deposit negative electrode material layer on the Cu paper tinsel of 15 μ m at thickness, formation has the collector of negative electrode material layer, according to being respectively the Si layer that contains Al to order away from the Cu paper tinsel near the Cu paper tinsel, thickness is 5 μ m, just active material layers; Carbon-coating, thickness are 1 μ m; The Si layer that contains Al, thickness are 5 μ m, are active material layer; C layer, thickness are 1 μ m.During deposition Si-Al layer, SiAl target as sputter power is 500W, and gas Ar flow is 58sccm; Sputtering power when depositing amorphous C rete is 400W, and gas Ar flow is 36sccm, and wherein in the active material rete, the atomic ratio of Si:Al is about 100:50.
The preparation of polymer coating: select for use polyethylene as the polymer coating material, dimethyl sulfoxide (DMSO) is a solvent, and ethylene carbonate is a plasticizer, oxide particle TiO
2, being dissolved in the oxolane, dimethyl sulfoxide (DMSO) and oxolane volume ratio are 10:1, TiO
2Content is 5% of PVDF-HFP weight.With the polyethylene that is dissolved in the dimethyl sulfoxide (DMSO), plasticizer and the TiO that is dissolved in the oxolane
2Fully mix, disperse, form polymer coating solution, adopt The tape casting having film forming on the collector of negative electrode material layer, thicknesses of layers is 10 μ m.After the rete moulding in 80 ℃ of vacuum drying ovens dry 24h.Obtain porosity and be 50% polymer coating.Form cathode pole piece.
The positive electrode pole piece that lithium ion battery uses in the embodiment of the invention can prepare according to following method: utilize solvent such as N-first class-2-pyrrolidones (NMP), disperse the mixture LiMO of composite oxides
2(wherein M is at least a transition metal) is as LixCoO
2, LixNiO
2, LiMn
2O
4, LixMnO
3Deng, use electric conducting material such as carbon black and binding agent such as Kynoar (PVDF) simultaneously, adopt the mixture that forms to apply such as above the aluminum foil current collector.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.4mA/cm
2, the charging/discharging voltage scope is at 0～2.0V.The specific discharge capacity of cathode pole piece can reach 1200mAh/g, and 200 times circulation volume remains on about 90%.
Utilize radiofrequency magnetron sputtering technology, be target with crystal SiSn assembly target, graphite target simultaneously, at thickness deposition carbon-coating and active material layer on the Cu paper tinsel of 15 μ m, totally four layers, formation has the collector of negative electrode material layer, these four layers of negative electrode material layers are according to the order difference Si-Sn layer that arrives near the Cu paper tinsel away from the Cu paper tinsel, and thickness is 5 μ m; C layer, thickness are 5 μ m; Si-Sn layer, thickness are 5 μ m; Be the C layer, thickness is 1 μ m.During deposition Si-Sn layer, SiAl target as sputter power is 850W, and gas Ar flow is 52sccm; Sputtering power when depositing amorphous C rete is 400W, and gas Ar flow is 36sccm, and wherein in rete Si-Sn layer, the atomic ratio of Si:Sn is 100:25.
The preparation of polymer coating: select for use polymethyl methacrylate as the polymer coating material, acetone is solvent, propylene carbonate ester plasticiser, oxide particle Al
2O
3Mix with methyl alcohol, acetone, methyl alcohol volume ratio are 15:1, Al
2O
3Content is 30% of polymethyl methacrylate weight.Above-mentioned substance is fully mixed under certain condition, disperses, form polymer coating, adopt spraying process having film forming on the collector of negative electrode material layer, thicknesses of layers is 35 μ m.After the rete moulding in 80 ℃ of vacuum drying ovens dry 24h.Obtain porosity and be 60% polymer coating, form cathode pole piece.
The positive electrode pole piece that lithium ion battery uses in the embodiment of the invention can prepare according to following method: utilize solvent such as N-first class-2-pyrrolidones (NMP), disperse the mixture LiMO of composite oxides
2(wherein M is at least a transition metal) is as LixCoO
2, LixNiO
2, LiMn
2O
4, LixMnO
3Deng, use electric conducting material such as carbon black and binding agent such as Kynoar (PVDF) simultaneously, adopt the mixture that forms to apply such as above the aluminum foil current collector.
Gained film cathode pole piece and with LiCoO
2Be the anode pole piece of positive electrode active materials, be assembled into battery, change into aluminum plastic film encapsulation and fluid injection in the mode of lamination according to the conventional method preparation.Can change pole piece size and lamination sheet number as requested, obtain the polymer lithium ion secondary battery of different rated capacities.
When positive plate is of a size of 100 * 60mm, when the anodal lamination number of plies was 4 layers, the first charge-discharge capacity of gained battery was 1200mAh, and 65 times circulation volume remains on about 93%.
Utilize radiofrequency magnetron sputtering technology, be target with crystal SiB assembly target, graphite target simultaneously, at thickness deposition carbon-coating and active material layer on the aluminium foil of 15 μ m, amount to six layers, formation has the collector of negative electrode material layer, these six layers of negative electrode material layers are according to being respectively the Si-B layer near the Cu paper tinsel to the order away from the Cu paper tinsel, and thickness is 4 μ m; C layer, thickness are 1 μ m; Si-B layer, thickness are 4 μ m; C layer, thickness are 1 μ m; Si-B layer, thickness are 4 μ m; C layer, thickness are 1 μ m.During deposition Si-B layer, SiAl target as sputter power is 850W, and gas Ar flow is 52sccm; Sputtering power when depositing amorphous C rete is 400W, and gas Ar flow is 36sccm, and wherein in rete Si-B layer, the atomic ratio of Si:B is 100:25.
The preparation of polymer coating: select for use PPOX as the polymer coating material, dimethyl formamide is a solvent, and dimethyl carbonate is a plasticizer, and oxide particle MgO mixes with butanols, dimethyl formamide, butanols volume ratio are 20:1,20% of MgO content PPOX weight.Above-mentioned substance is fully mixed under certain condition, disperses, form polymer coating solution, adopt spraying process having film forming on the collector of negative electrode material layer, thicknesses of layers is 50 μ m.After the rete moulding in 80 ℃ of vacuum drying ovens dry 24h.Obtain porosity and be 50% polymer coating, form cathode pole piece.
The positive electrode pole piece that lithium ion battery uses in the embodiment of the invention can prepare according to following method: utilize solvent such as N-first class-2-pyrrolidones (NMP), disperse the mixture LiMO of composite oxides
2(wherein M is at least a transition metal) is as LixCoO
2, LixNiO
2, LiMn
2O
4, LixMnO
3Deng, use electric conducting material such as carbon black and binding agent such as Kynoar (PVDF) simultaneously, adopt the mixture that forms to apply such as above the aluminum foil current collector.
Gained film cathode pole piece and with LiCoO
2Be the anode pole piece of positive electrode active materials, be assembled into battery, change into aluminum plastic film encapsulation and fluid injection in the mode of lamination according to the conventional method preparation.Can change pole piece size and lamination sheet number as requested, obtain the polymer lithium ion secondary battery of different rated capacities.
When positive plate is of a size of 100 * 60mm, when the anodal lamination number of plies was 4 layers, the first charge-discharge capacity of gained battery was 1200mAh, and 65 times circulation volume remains on about 93%.
Claims (10)
1. the cathode pole piece of a lithium rechargeable battery is characterized in that this cathode pole piece comprises:
Collector,
Be deposited on the negative electrode material layer on the described collector, wherein comprise the active material layer that contains a kind of in silicon, the tin element or two kinds,
Be coated in the polymer coating on the described negative electrode material layer.
2. cathode pole piece according to claim 1 is characterized in that described collector is Copper Foil or aluminium foil, preferred Copper Foil.
3. cathode pole piece according to claim 1, it is characterized in that described negative electrode material layer also comprises one deck carbon-coating at least, described carbon-coating and active material layer space are arranged on the described collector, and the layer that contacts with described collector is an active material layer.
4. according to each described cathode pole piece in the claim 1-3, it is characterized in that described active material layer also comprises doped chemical, this doped chemical is selected from one or more in aluminium, copper, boron and the iron.
5. according to each described cathode pole piece in the claim 1-4, the gross thickness that it is characterized in that described negative electrode material layer is 5-20 μ m.
6. according to each described cathode pole piece in the claim 3-5, it is characterized in that element on the described active material layer and the carbon on the described carbon-coating all exist with impalpable structure.
7. according to each described cathode pole piece in the claim 1-6, the thickness that it is characterized in that described polymer coating is 10-50 μ m, and the porosity of described polymer coating is 40%-60%.
8. according to each described cathode pole piece in the claim 1-7, the polymer that it is characterized in that described polymer coating is selected from one or more in polyolefin, fluorine-containing polyolefin, fluorine-containing polyolefin copolymer, polyacrylate, polyacrylonitrile and the poly-alkyl oxide, one or more in preferably polyethylene, Kynoar, Kynoar-hexafluoropropylene, polymethyl methacrylate, polyacrylonitrile, poly(ethylene oxide), the PPOX.
9. according to each described cathode pole piece in the claim 1-8, it is characterized in that also comprising in the described polymer coating oxide particle, and described oxide particle be polymer coating polymer quality 1%-30%, described oxide particle is preferably SiO
2, TiO
2, Al
2O
3With among the MgO one or several.
10. method for preparing each described cathode pole piece in the claim 1-9 is characterized in that may further comprise the steps:
A) method of employing vapour deposition deposits negative electrode material layer on described collector, forms the collector with negative electrode material layer,
B) follow described polymer dissolution in organic solvent, form polymer coating solution,
C) more described polymer coating solution is coated on the collector with negative electrode material layer, after the film forming, places baking oven dry, remove described organic solvent, form described cathode pole piece.
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| CNA200710177231XA CN101436655A (en) | 2007-11-12 | 2007-11-12 | Cathode pole piece of lithium ion secondary battery and preparation method thereof |
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- 2007-11-12 CN CNA200710177231XA patent/CN101436655A/en not_active Withdrawn
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