CN1274052C - Method for producing lithium ion secondary cell - Google Patents
Method for producing lithium ion secondary cell Download PDFInfo
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- CN1274052C CN1274052C CNB031140394A CN03114039A CN1274052C CN 1274052 C CN1274052 C CN 1274052C CN B031140394 A CNB031140394 A CN B031140394A CN 03114039 A CN03114039 A CN 03114039A CN 1274052 C CN1274052 C CN 1274052C
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- lithium
- rechargeable battery
- lithium rechargeable
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The present invention discloses a method for making a secondary lithium ion cell of which a positive electrode is made by adopting water paste coating plate making. In the method, positive electrode paste is made by that water soluble adhesive is dissolved in deionized water in the process of paste coating plate making, and a positive electrode active substance, a carbon material electric conduction agent, a viscosity increaser, and an additive used for improving the adherence of a positive electrode layer are added to the deionized water according to a certain order to be fully dispersed. A secondary lithium ion cell produced by the method can reduce production cost and prevent environmental pollution.
Description
[technical field]
The present invention relates to a kind of manufacture method of lithium rechargeable battery, particularly relate to a kind of manufacture method that adopts the lithium rechargeable battery of anodal water system slurry film-making.
[background technology]
After proposing " rocking chair battery " notion (RCB) in 1980, Sony corporation of Japan and Sanyo are respectively at beginning the lithium rechargeable battery practical research in 1985 and 1988.Because outstanding advantages such as lithium rechargeable battery has the operating voltage height, specific energy is big, self discharge is little, temperature limit is wide, stable operating voltage, storage life length, countries in the world all illustrate great interest and enthusiasm to the application table of lithium rechargeable battery at aspects such as communication field, portable type electronic product, electric motor car and Aero-Space, and have carried out continuous exploration and improvement at the performance and the manufacturing process of lithium rechargeable battery.
Must use suitable bonding to finish the preparation of electrode in the manufacturing process of lithium rechargeable battery, adhesive in battery mainly in order to active material and electrode current collecting body is together bonded to each other.At present, lithium ion secondary battery positive electrode mostly adopts polyvinylidene fluoride (PVDF) as adhesive, with the solvent as PVDF such as strong polar organic compound such as N-dimethyl pyrrolidone (NMP), dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), promptly adopt the film-making of organic system slurry.Need use costliness during the film-making of organic system slurry and have corrosive organic solvent such as NMP etc., use amount is big and be difficult to recovery, has increased production cost widely.Simultaneously, need during the slurry film-making organic solvent heating is removed, must install a large amount of environmental protection equipments additional in case environmental pollution brings inconvenience to production operation.
[summary of the invention]
The object of the present invention is to provide the manufacture method of a kind of low cost, free of contamination lithium rechargeable battery.
For realizing above purpose, the technical scheme that the present invention proposes is:
The positive pole of lithium rechargeable battery adopts water system slurry flaking method, be characterized in, anode sizing agent passes through water soluble adhesive dissolves in deionized water in slurry film-making process, add positive active material, carbon-based material conductive agent, tackifier respectively according to a graded again and, make after disperseing fully in order to improve the additive of anodal layer adherence.Above-mentioned prepared slurry is coated on the plus plate current-collecting body aluminium foil equably, dry under uniform temperature, can obtain certain thickness positive plate after the calendering.
The positive plate of described lithium rechargeable battery contains the stratiform composite oxides of a kind of lithium and transition metal, and they are the active materials with certain ad hoc structure, can carry out reversible reaction with lithium ion.
The negative electrode active material of described lithium rechargeable battery be for can make lithium ion embed and take off the carbon-based material of embedding repeatedly, and negative pole also contains the electrode current collecting body (being Copper Foil usually) of metal material and negative material is bonded to adhesive on the electrode current collecting body.
The electrolyte of described lithium rechargeable battery is to contain the chain acid esters of lithium salts and the mixed solution of ring-type acid esters.
The invention has the advantages that: in anodal slurry film-making process, can replace costliness and have corrosive organic solvent with cheap, free of contamination deionized water, need not install environmental protection equipment additional, thereby greatly reduce the cost of battery raw material and investment of production equipment; And the lithium rechargeable battery that makes of method has good high-multiplying power discharge characteristic and cycle characteristics thus.
Concrete enforcement of the present invention, performance and advantage thereof are further specified by embodiment.
[embodiment]
The lithium rechargeable battery of the anodal water system slurry of the present invention flaking method, it is made of major parts such as positive pole, negative pole, electrolyte and barrier films.Wherein:
The positive pole of described lithium rechargeable battery contains the stratiform composite oxides of a kind of lithium and transition metal, and they are the active materials with certain ad hoc structure, can carry out reversible reaction with lithium ion.The example of this type of active material comprises: Li
xNi
1-yCo
yO
2(wherein, 0.9≤x≤1.1,0≤y≤1.0), Li
xMn
2-yB
yO
2(wherein, B is a transition metal, 0.9≤x≤1.1,0≤y≤1.0) etc.And the anodal electrode current collecting body (being aluminium foil usually) that also contains metal material, carbon-based material conductive agent, positive electrode is bonded to adhesive on the electrode current collecting body, tackifier and in order to improve the additive of anodal layer adherence.Wherein the example of carbon-based material conductive agent comprises carbon black, carbon fiber and graphite etc.
Described anode sizing agent be by with a kind of suitable water soluble adhesive dissolves in deionized water, add positive active material, carbon-based material conductive agent, tackifier respectively according to a graded again and, make after disperseing fully in order to improve the additive of anodal layer adherence.Described in the present invention water-soluble binder is selected from PTFE and SBR, can use one of them or its mixture, and consumption is preferably 0.5～15.0wt% of positive active material.Tackifier are selected from MC, CMC, HPMC, CMHEC and HPC etc., can use one of them or its mixture, and consumption is preferably 0.2～10.0wt% of positive active material.In order to the additive that improves anodal layer adherence is methyl-silicone oil and carbon fiber, and wherein the consumption of methyl-silicone oil is preferably 0.1～8.0wt% of positive active material, and the consumption of carbon fiber is preferably 0.1～15.0wt% of positive active material.
To be coated on equably on the plus plate current-collecting body aluminium foil according to the said method prepared slurry, dry under uniform temperature, can obtain certain thickness positive plate after the calendering.
In the present invention, the purpose that adds the methyl-silicone oil additive is in order to reduce the generation of bubble in batching and the pulling phase, to strengthen the adherence of slurry and plus plate current-collecting body aluminium foil, making the pole piece surface smooth more smooth.Simultaneously, methyl-silicone oil surface of good activity has also been improved the wettability of electrolyte to pole piece.In the present invention, the purpose that adds the carbon fiber additive is flexibility and the mechanical strength in order to strengthen pole piece, improves the adherence of anodal layer.Therefore,, can make the attached material of anodal layer tightr, thereby improve the cycle characteristics and the high-multiplying power discharge characteristic of lithium rechargeable battery by adding above-mentioned two kinds of additives.
The negative electrode active material of lithium rechargeable battery of the present invention is for can make lithium ion embed and take off the carbon-based material of embedding repeatedly, and the example comprises native graphite, Delanium, MCMB, MCF etc.And negative pole also contains the electrode current collecting body (being Copper Foil usually) of metal material and negative material is bonded to adhesive on the electrode current collecting body, and the example of adhesive comprises polyolefin compound such as PTFE and SBR etc.
The electrolyte of lithium rechargeable battery of the present invention is to contain the chain acid esters of lithium salts and the mixed solution of ring-type acid esters.The example of lithium salts comprises LiClO4, LiPF6, LiBF4, lithium halide, chlorine lithium aluminate, fluorocarbon based fluorine oxygen lithium phosphate and fluorocarbon based sulfonic acid lithium etc., can use one of them or its mixture.The example of chain acid esters comprises that DMC, DEC, EMC, MPC, DPC, MA, EA, PA and other are fluorine-containing, sulfur-bearing or contain the chain organosilane ester of unsaturated bond, can use one of them or its mixture.The example of ring-type acid esters comprises that EC, PC, VC, γ-BL, sultone and other are fluorine-containing, sulfur-bearing or contain the ring-type organosilane ester of unsaturated bond, can use one of them or its mixture.
[embodiment 1]
At first with LiCoO2 and acetylene black at 150 ℃ of dry 2h down, batch mixing 2h according to a certain percentage then.In deionized water, add methyl-silicone oil, carbon fiber, CMC and PTFE respectively, stir 4h again.Add LiCoO2 and the acetylene black that mixes at last, fully be mixed and made into anode sizing agent.It consists of LiCoO2: acetylene black: PTFE: CMC: methyl-silicone oil: carbon fiber=90: 3: 3: 1.5: 0.5: 2.Prepared slurry is coated on equably on the aluminium foil of 20 μ m, dry down in 90 ℃.Obtain the positive plate that thickness is 140 μ m after the calendering.
A certain amount of PTFE is dissolved in the deionized water with certain ratio, Delanium and CMC are added in this solution, fully be mixed and made into slurry, it consists of Delanium: PTFE: CMC=90: 7: 3.Again this slurry is coated on the Copper Foil of 20 μ m equably, dry down in 90 ℃.Obtain the negative plate that thickness is 140 μ m after the calendering.
The electric core of the lithium rechargeable battery of polypropylene microporosity membrane coil coiled that above-mentioned positive and negative plate and 25 μ m are thick, pack into and weld in the battery case, subsequently LiPF6 is dissolved in EC/DMC=1 by the concentration of 1mol/dm3: formed electrolyte injects battery case in 1 the mixed solvent, lithium rechargeable battery is made in sealing.
[embodiment 2]
Use and 1 similar method of embodiment, but anode sizing agent consists of LiCoO2: acetylene black: SBR: CMC: methyl-silicone oil: carbon fiber=90: 3: 3: 1.5: 0.5: 2.
[embodiment 3]
Use and 1 similar method of embodiment, but anode sizing agent consists of LiCoO2: acetylene black: PTFE: HPMC: methyl-silicone oil: carbon fiber=90: 3: 3: 1.5: 0.5: 2.
[embodiment 4]
Use and 1 similar method of embodiment, but anode sizing agent consists of LiCoO2: acetylene black: SBR: HPMC: methyl-silicone oil: carbon fiber=90: 3: 3: 1.5: 0.5: 2.
[comparative example 5]
Use and 1 similar method of embodiment, but anode sizing agent consists of LiCoO2: acetylene black: PTFE: CMC: methyl-silicone oil :=90: 4: 4: 1.5: 0.5.
[comparative example 6]
Use and 1 similar method of embodiment, but anode sizing agent consists of LiCoO2: acetylene black: PTFE: CMC: carbon fiber=90: 3: 3: 1.5: 2.5.
[comparative example 1]
Use and 1 similar method of embodiment, but positive plate is obtained by following method: a certain amount of PVDF is dissolved among the NMP with certain ratio, LiCoO2 and acetylene black are added in this solution, fully be mixed and made into slurry, it consists of LiCoO2: acetylene black: PVDF=92: 4: 4.This slurry is coated on equably on the aluminium foil of 20 μ m, dry down in 120 ℃.Obtain the positive plate that thickness is 140 μ m after the calendering.
The battery behavior test
[discharge performance]
With the lithium rechargeable battery made as stated above with the constant current charge of 400mA to 4.2V, after voltage rises to 4.2V with constant-potential charge, by electric current 50mA; Constant current with 400mA discharges again, by voltage 2.75V.Measure initial capacity.
[cycle characteristics]
The lithium rechargeable battery of making is is as stated above discharged and recharged 500 circulations with above-mentioned charge-discharge mechanism.Be determined at the capacity sustainment rate of 500 circulation times.
[part throttle characteristics]
With the lithium rechargeable battery made as stated above with the constant current charge of 400mA to 4.2V, after voltage rises to 4.2V with constant-potential charge, by electric current 50mA; Constant current with 2000mA discharges again, by voltage 2.75V.Be determined under the high-load condition the capacity sustainment rate and the discharge in threshold voltage.More than Shi Yan result is as shown in the table.
The performance of lithium-ion secondary battery test result
| Adhesive | Tackifier | Additive level (wt%) | Initial discharge capacity (mA h) | 500 circulation back capacity sustainment rates (%) | 2A/0.4A discharge capacity sustainment rate (%) | ||||
| Kind | Content (wt %) | Kind | Content (wt %) | Methyl-silicone oil | Carbon fiber | ||||
| Embodiment 1 | PTFE | 3.0 | CMC | 1.5 | 0.5 | 2.0 | 752 | 86.2 | 92.1 |
| Embodiment 2 | SBR | 3.0 | CMC | 1.5 | 0.5 | 2.0 | 756 | 88.7 | 94.7 |
| Embodiment 3 | PTFE | 3.0 | HPMC | 1.5 | 0.5 | 2.0 | 748 | 84.5 | 90.2 |
| Embodiment 4 | SBR | 3.0 | HPMC | 1.5 | 0.5 | 2.0 | 751 | 88.1 | 90.6 |
| Embodiment 5 | PTFE | 4.0 | CMC | 1.5 | 0.5 | - | 747 | 80.4 | 79.2 |
| Embodiment 6 | PTFE | 3.0 | CMC | 1.5 | - | 2.5 | 745 | 79.3 | 86.1 |
| Comparative example 1 | PVDF | 4.0 | - | - | - | - | 765 | 78.5 | 81.4 |
According to above result as seen, the lithium rechargeable battery of each embodiment is compared with the comparative example 1 that adopts organic system slurry flaking method, is keeping under the constant substantially situation of battery initial capacity, has more good cycle performance and high-rate discharge ability.And the relative embodiment 1～4 with the combination property of embodiment 6 of embodiment 5 descends to some extent, and this has illustrated methyl-silicone oil and carbon fiber as additive, and the adherence for improving anodal layer increases attached material intensity, plays crucial effect.
Claims (6)
1, a kind of method for preparing lithium rechargeable battery, it comprises following steps:
The preparation of a anode sizing agent;
B is coated on anode sizing agent on the electrode current collecting body equably, obtains certain thickness positive plate after drying, the calendering;
The preparation of c cathode size;
D is coated on cathode size on the electrode current collecting body equably, obtains certain thickness negative plate after drying, the calendering;
Positive and negative plate that e will prepare and membrane coil coiled battery, also welding injects the electrolyte in the battery case subsequently in the battery case of packing into, and lithium rechargeable battery is made in sealing;
It is characterized in that:
Described step a will comprise that positive active material, carbon-based material conductive agent, water-soluble binder, tackifier are dissolved in the water, and stirring promptly makes anode sizing agent; This water-soluble binder is made up of one of them or its mixture of polytetrafluoroethylene PTFE or styrene butadiene rubber sbr, and consumption is 0.5～15.0wt% of positive active material; These tackifier are one of them or its mixture of methylcellulose MC, sodium carboxymethylcellulose CMC, hydroxypropyl methylcellulose HPMC, carboxymethyl hydroxyethyl cellulose CMHEC and hydroxypropyl cellulose HPC, and consumption is 0.2～10.0wt% of positive active material;
Comprise also in the anode sizing agent of described step a that methyl-silicone oil or carbon fiber one of them or its mixture are as additive, wherein the consumption of methyl-silicone oil is 0.1～8.0wt% of positive active material, and the consumption of carbon fiber is 0.1～15.0wt% of positive active material.
2, the method for preparing lithium rechargeable battery according to claim 1, wherein the described positive plate of step b contains the stratiform composite oxides of a kind of lithium and transition metal, and these stratiform composite oxides comprise the active material that following chemical formula is represented: Li
xNi
1-yCo
yO
2, wherein, 0.9≤x≤1.1,0≤y≤1.0; Li
xMn
2-yB
yO
2, wherein, B is a transition metal, 0.9≤x≤1.1,0≤y≤1.0.
3, the method for preparing lithium rechargeable battery according to claim 1, wherein the solvent of the described cathode size of step c is a water.
4, the method for preparing lithium rechargeable battery according to claim 1, it is characterized in that: the described negative pole of steps d contains a kind of carbon-based material that can make lithium ion embed and take off embedding repeatedly, and this carbon-based material comprises native graphite, Delanium, MCMB MCMB, carbon fiber MCF.
5, the method for preparing lithium rechargeable battery according to claim 1, it is characterized in that: the described electrolyte of step e comprises the lithium salts that is selected from lithium perchlorate, chlorine lithium aluminate, lithium hexafluoro phosphate, LiBF4, lithium halide, fluorocarbon based fluorine oxygen lithium phosphate and fluorocarbon based sulfonic acid lithium, can use one of them or its mixture.
6, the method for preparing lithium rechargeable battery according to claim 1, it is characterized in that: the described electrolyte of step e comprises the mixed solvent of chain acid esters and ring-type acid esters, the chain acid esters is selected from dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, ethyl propyl carbonic acid ester, diphenyl carbonate, methyl acetate, ethyl acetate, methyl propionate, ethyl propionate and other is fluorine-containing, sulfur-bearing or contain the chain organosilane ester of unsaturated bond, can use one of them or its mixture.The ring-type acid esters is selected from ethylene carbonate, propene carbonate, vinylene carbonate, gamma-butyrolacton, sultone and other is fluorine-containing, sulfur-bearing or contain the ring-type organosilane ester of unsaturated bond, can use one of them or its mixture.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031140394A CN1274052C (en) | 2003-03-21 | 2003-03-21 | Method for producing lithium ion secondary cell |
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|---|---|---|---|
| CNB031140394A CN1274052C (en) | 2003-03-21 | 2003-03-21 | Method for producing lithium ion secondary cell |
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|---|---|
| CN1532984A CN1532984A (en) | 2004-09-29 |
| CN1274052C true CN1274052C (en) | 2006-09-06 |
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