CN1770510A - A kind of preparation method of positive plate of lithium secondary battery and lithium ion secondary battery - Google Patents
A kind of preparation method of positive plate of lithium secondary battery and lithium ion secondary battery Download PDFInfo
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- CN1770510A CN1770510A CNA2004100521698A CN200410052169A CN1770510A CN 1770510 A CN1770510 A CN 1770510A CN A2004100521698 A CNA2004100521698 A CN A2004100521698A CN 200410052169 A CN200410052169 A CN 200410052169A CN 1770510 A CN1770510 A CN 1770510A
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- lithium
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Abstract
This invention relates to lithium ion second battery electrode slice process method, which comprises the following steps: coating the positive active substance on integrated fluid imbedded with lithium and beckoning and entrenching; between beckoning and entrenching step using lithium carbonate to dip or coating positive electrode surface for vacuum drying. The battery comprises positive electrode slice, isolation film, negative electrode and non-water catalyze.
Description
Technical field
The present invention relates to a kind of secondary cell, particularly relate to a kind of anode piece preparation method that can effectively improve high temperature safe, circulation and the storge quality of lithium secondary battery, and use the lithium rechargeable battery of this positive plate.
Background technology
Lithium rechargeable battery is since nineteen ninety succeeds in developing, since its have specific energy height, operating voltage height, self-discharge rate low, have extended cycle life, advantage such as pollution-free, progressively replaced traditional nickel every alkaline secondary cells such as, ni-mhs, at modern mobile electronic device and communication apparatus, as having obtained extensive use in mobile phone, notebook computer, laptop computer, PDA(Personal Digital Assistant), small-sized camera, digital camera, portable DVD player/VCD and the MP3 player.
Lithium rechargeable battery is when charging, and lithium ion takes off embedding from the interlayer of the anodal oxide with layer structure that positive plate applies, and arrives negative plate by barrier film between the positive/negative plate and electrolyte, embeds the interlayer of the material with carbon element with layer structure; When discharge, lithium ion takes off embedding from the interlayer of the material with carbon element with layer structure that negative plate applies, and arrives positive plate by barrier film between the positive/negative plate and electrolyte, embeds the interlayer of the anodal oxide with layer structure.Positive and negative plate is connected with circuit with extraneous with lug by collector, forms loop current when discharge.
The positive electrode that is currently applied in the lithium ion battery mainly contains LiCoO
2, LiMn
2O
4, LiNiO
2In charge and discharge cycles or storage process, all exist the capacity attenuation under in various degree capacity attenuation, the especially high temperature even more serious Deng, above-mentioned material.Therefore, the high temperature circulation, the storge quality that how to solve lithium ion battery also become a current research focus, and wherein, main method has:
(1) at LiMn2O4 coated with carbon acid lithium, sodium carbonate, metal carbonates such as potash improve storage and cycle performance (J Electrochem.Soc., 2000,147 (1): 4023-4028 under the high temperature; US5783328);
(2) at cobalt acid lithium surface clad oxide (US2003148182)/transition metal oxide (CN1459131A), improve cycle life and security feature;
(3) in cobalt acid lithium slurry, sneak into the lithium carbonate of 0.1～0.6wt%, suppress reaction (JP2001238692A) anodal and electrolyte.
In the said method, the shortcoming of (1), (2) is:
A. coat the metal carbonate or the metal oxide that contain elements such as sodium, potassium and in battery system, introduce metal ions such as sodium ion, potassium ion easily, these ions can embed the carbon material used as anode interlayer altogether with lithium ion, cause battery capacity to descend, cycle performance is variation on the contrary;
B. chemical packs coating process complexity, and need carry out long high temperature sintering to coating and just can obtain the coating layer that needs, manufacturing cycle is long, the cost height;
C. the amount of uniformity coefficient of Bao Fuing and coating is difficult to control;
The shortcoming of method (3) is:
A. under the high temperature; anodal side reaction with electrolyte at first occurs in the surface of pole piece in the battery; after lithium carbonate sneaked into anode sizing agent and be coated on the pole piece; the lithium carbonate that is distributed in the pole piece outer surface only accounts for a few part; can not form fine and close protective layer, therefore, along with the carrying out that discharges and recharges; side reaction takes place from outside to inside gradually, causes battery circulation, storge quality variation.
B. owing to be to adopt the method for mixing, lithium carbonate particle great majority are scattered in the gap of anode constituents such as active material, conductive agent, are difficult to directly be adsorbed on the surface of active particle, are difficult for forming uniform sealer.Even if strengthen the consumption of lithium carbonate, the problems referred to above still exist, but also can reduce the consumption of active material, sacrifice the capacity of battery.
Summary of the invention
The technical problem to be solved in the present invention aims to provide a kind of positive plate preparation method of improved lithium rechargeable battery, with high temperature safe, circulation and the storge quality that improves lithium rechargeable battery.
The another kind of technical problem that the present invention will solve aims to provide a kind of lithium rechargeable battery, and it has adopted the lithium-ion secondary battery positive plate that improves the preparation method, makes battery possess high temperature safe, circulation and storge quality.
For solving first technical problem, the invention provides a kind of preparation method of lithium-ion secondary battery positive plate, comprise that can embed the positive active material that disengages lithium is coated on the plus plate current-collecting body, baking, calendering, wherein, between baking procedure and calendering step or after the calendering step:, and carry out vacuumize with lithium carbonate solution impregnation or spray treatment positive plate surface.
Described lithium carbonate solution can be lithium carbonate aqueous solution, and its mass percent concentration is greater than 0.01%, and concentration is crossed low immersion positive plate lithium carbonate amount very little, can not play positive effect.Because of the solubility of lithium carbonate aqueous solution is not high, preferred lithium carbonate solution concentration be saturated concentration.
The described time with lithium carbonate solution impregnation positive plate is 0.1～600 minute, and the easy hardening of the long pole piece of dip time is unfavorable for the carrying out of subsequent handling, preferred 5～120 minutes.
For solving second technical problem, the invention provides a kind of lithium rechargeable battery, it comprises positive plate, barrier film, negative pole and nonaqueous electrolytic solution, the preparation process of described positive plate comprises that can embed the positive active material that disengages lithium is coated on the plus plate current-collecting body, baking, calendering, wherein, between baking procedure and calendering step or after the calendering step:, and carry out vacuumize with lithium carbonate solution impregnation or spray treatment positive plate surface.
Described lithium carbonate solution can be lithium carbonate aqueous solution, and its mass percent concentration is greater than 0.01%, and concentration is crossed low immersion positive plate lithium carbonate amount very little, can not play positive effect.Because of the solubility of lithium carbonate aqueous solution is not high, preferred lithium carbonate solution concentration be saturated concentration.
The described time with lithium carbonate solution impregnation positive plate is 0.1～600 minute, and the easy hardening of the long pole piece of dip time is unfavorable for the carrying out of subsequent handling, preferred 5～120 minutes.
Above-mentioned positive active material is not particularly limited, and can disengage the positive active material of lithium for embedding of this area routine, is preferably a kind of, the perhaps multiple mixture in the lithium transition-metal oxide shown in formula (1), formula (2) and the formula (3):
Li
1+xM
yMn
2-yO
4 ---------(1)
In the formula ,-0.1≤x≤0.2,0≤y≤1.0, M is at least a in the elements such as lithium, boron, magnesium, aluminium, titanium, chromium, iron, cobalt, nickel, copper, zinc, gallium, yttrium, fluorine, iodine, sulphur.
Li
mNi
nCo
1-nO
2 ---------(2)
In the formula, 0.9≤m≤1.1,0≤n≤1.0
Li
aL
bMn
1-bO
2 ---------(3)
In the formula, 0.9≤a≤1.1,0≤b≤1.0, L is at least a in the elements such as cobalt, nickel.
Also can further contain the conductive agent that weight percentage is 1-15% in the described positive active material, described conductive agent is not particularly limited, can be the anodal conductive agent of this area routine, at least a such as in acetylene black, conductive carbon black and the electrically conductive graphite, preferred acetylene black.
Described negative pole is to make on the negative current collector by adhesive being dissolved in the solvent, adding negative electrode active material again, being coated on after disperseing fully.Negative electrode active material of the present invention is not particularly limited, can disengage the negative electrode active material of lithium for embedding of this area routine, such as native graphite, electrographite, petroleum coke, organic cracking carbon, MCMB (carbonaceous mesophase spherules), MCF (carbon fiber), ashbury metal, silicon alloy etc., can select one of them or its mixture for use, preferred electrographite.Described solvent can be selected from NMP (N-methyl pyrrolidone), DMF (dimethyl formamide), DEF (diethyl methylformamide), DMSO (dimethyl sulfoxide (DMSO)), THF (oxolane) and water and alcohols etc., can use one of them or its mixture, preferred NMP.Described adhesive comprises fluorine resin and polyolefin compound such as PVDF (polyvinylidene fluoride), PTFE (polytetrafluoroethylene), VDF-HFP-TFE copolymer (vinylidene fluoride-tetrafluoraoethylene-hexafluoropropylene copolymer), SBR (butadiene-styrene rubber) etc., can select one of them or its mixture for use.
Described nonaqueous electrolytic solution is the mixed solution of electrolyte lithium salt and nonaqueous solvents, and it is not particularly limited, and can use the nonaqueous electrolytic solution of this area routine.Can be LiClO such as electrolyte lithium salt
4(lithium perchlorate), LiPF
6(lithium hexafluoro phosphate), LiBF
4(LiBF4), LiAsF
6(hexafluoroarsenate lithium), 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, preferred LiPF
6Organic solvent is selected chain acid esters and ring-type acid esters mixed solution for use, the chain acid esters can be DMC (dimethyl carbonate), DEC (diethyl carbonate), EMC (ethyl-methyl carbonic ester), MPC (carbonic acid first propyl ester), DPC (dipropyl carbonate), MA (methyl acetic acid ester), EA (ethylhexoate), PA (propyl-acetic acid ester), dimethoxy-ethane 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 EC (vinyl carbonate), PC (third rare carbonic ester), VC (inferior vinyl carbonate), γ-BL (gamma-butyrolacton), sultone and other are fluorine-containing, sulfur-bearing or contain at least a in the ring-type organosilane ester of unsaturated bond.
Described barrier film and positive and negative electrode collector body are not particularly limited, and can be barrier film and positive and negative electrode collector body conventional in the lithium rechargeable battery, barrier film preferred polyolefm micro-porous film, the preferred aluminium foil of positive electrode collector, the preferred Copper Foil of negative electrode collector.
Compared with prior art, contribution of the present invention is to efficiently solve high temperature safe, circulation and the storge quality problem of lithium rechargeable battery:
(1) under the high temperature; anodal side reaction with electrolyte at first occurs in the surface of pole piece in the battery; with the lithium carbonate solution impregnation or after being sprayed on the pole piece; the lithium carbonate that is distributed in the pole piece outer surface effectively forms fine and close protective layer, so battery has good high-temperature safety, circulation and storge quality.
(2) owing to be the method that adopts dipping or spraying lithium carbonate solution, compare with the method for mixed carbonic acid lithium in the prior art, lithium carbonate particle great majority are scattered in the positive plate surface, form uniform sealer easily.In addition, only need use a spot of lithium carbonate just can play the effect of obvious suppression battery capacity decay.
(3) technology of positive plate processing is simple, has shortened manufacturing cycle, has reduced production cost.
Description of drawings
Fig. 1 is the high temperature circulation curve comparison diagram of the embodiment of the invention 2,4 and comparative example 1.
Embodiment
The following example is to further explanation of the present invention and explanation, and the present invention is not constituted any limitation.
Embodiment 1
Binding agent PVDF is dissolved among the nonaqueous solvents NMP, with positive active material LiMn
2O
4Add in this solvent with conductive agent acetylene black, fully be mixed and made into slurry, it consists of LiMn
2O
4: acetylene black: PVDF=91: 5: 4.This slurry is coated on equably on the aluminium foil of 20 μ m, down baking is dry in 120 ℃, this positive plate is immersed in 0.01% the lithium carbonate aqueous solution, takes out vacuumize after 20 minutes, and calendering obtains positive plate.
Binding agent PVDF is dissolved among the non-water NMP, the negative electrode active material Delanium is added in this solvent, fully be mixed and made into slurry, it consists of Delanium: PVDF=95: 5.This slurry is coated on the Copper Foil of 20 μ m equably, baking is dry down in 120 ℃, obtains negative plate after the calendering again.
The polypropylene screen that above-mentioned positive and negative plate and 25 μ m are thick is wound into the pole piece of a square lithium ion battery and is accommodated in the rectangular cell shell, subsequently with LiPF
6Press 1mol/dm
3Concentration be dissolved in EC/DMC=1: formed electrolyte injects battery case in 1 the mixed solvent, and sealing is made thick 5mm, wide 34mm, the square lithium ion battery of high 50mm.
Embodiment 2
Except the concentration of lithium carbonate aqueous solution is 0.2%, other operating procedures and process conditions are with embodiment 1.
Embodiment 3
Except dip time is 10 seconds, other operating procedures and process conditions are with embodiment 2.
Embodiment 4
Except dip time is 2 minutes, other operating procedures and process conditions are with embodiment 2.
Embodiment 5
Except dip time is 120 minutes, other operating procedures and process conditions are with embodiment 2.
Embodiment 6
Except dip time is 200 minutes, other operating procedures and process conditions are with embodiment 2.
Embodiment 7
Except adopting positive plate to carry out after calendering the impregnation process, other operating procedures and process conditions are with embodiment 2.
Embodiment 8
Except adopting positive plate to carry out after calendering the spray treatment, other operating procedures and process conditions are with embodiment 2.
Comparative example 1
Except positive plate not being carried out the impregnation process, other operating procedures and process conditions are with embodiment 1.
The battery that makes with said method is carried out characteristic test respectively.Method of testing is as follows: 1. high temperature cyclic performance test
Under 60 ℃ of conditions, with embodiment and comparative example battery respectively with the 1CmA current charges to 4.2V, with constant-potential charge, cut-off current is 0.05CmA after voltage rises to 4.2V, shelves 5 minutes; Battery, was shelved 5 minutes to 3.0V with the 1CmA current discharge.Repeat above step 300 time, obtain the capacity of 300 circulation backs of battery 1CmA current discharge to 3.0V, capacity sustainment rate before and after the computation cycles, its cyclic curve as shown in Figure 1, test data sees the following form:
Table 1
| Example | Capacity sustainment rate (%) |
| Embodiment 1 | 83.8 |
| Embodiment 2 | 86.7 |
| Embodiment 3 | 74.9 |
| Embodiment 4 | 78.5 |
| Embodiment 5 | 87.6 |
| Embodiment 6 | 81.4 |
| Embodiment 7 | 85.5 |
| Embodiment 8 | 86.1 |
| Comparative example 1 | 67.8 |
2. high-temperature storage performance test
Under the room temperature condition, with embodiment and comparative example battery respectively with the 1CmA current charges to 4.2V, with constant-potential charge, cut-off current is 0.05CmA after voltage rises to 4.2V, shelve 5 minutes after, accurately measure cell thickness; Then above-mentioned battery is stored a week under 60 ℃ of conditions, measure battery with the capacity of 1CmA current discharge, and measure cell thickness once more to 3.0V, counting cell capacity sustainment rate and change value of thickness, test result sees the following form:
Table 2
| Example | Capacity sustainment rate (%) | Change value of thickness (mm) |
| Embodiment 1 | 92.6 | 0.06 |
| Embodiment 2 | 95.4 | 0.05 |
| Embodiment 3 | 84.1 | 0.09 |
| Embodiment 4 | 87.3 | 0.07 |
| Embodiment 5 | 95.7 | 0.04 |
| Embodiment 6 | 91.5 | 0.07 |
| Embodiment 7 | 94.2 | 0.05 |
| Embodiment 8 | 93.6 | 0.04 |
| Comparative example 1 | 74.5 | 0.20 |
3. security performance test
Under the room temperature condition, with embodiment and comparative example battery respectively with the 1CmA current charges to 4.2V, with constant-potential charge, cut-off current is 0.05CmA after voltage rises to 4.2V, shelves 5 minutes; Carry out the test of 150 ℃ of stove heat, the results are shown in following table:
Table 3
| Example | It is no abnormal behind the 1h to be that battery has | The battery surface maximum temperature (℃) |
| Embodiment 1 | Do not have | 163 |
| Embodiment 2 | Do not have | 160 |
| Embodiment 3 | Do not have | 170 |
| Embodiment 4 | Do not have | 167 |
| Embodiment 5 | Do not have | 158 |
| Embodiment 6 | Do not have | 165 |
| Embodiment 7 | Do not have | 161 |
| Embodiment 8 | Do not have | 161 |
| Comparative example 1 | Venting is opened after 41 minutes | 175 |
According to above test result, adopt the inventive method that positive plate is handled after, compare with undressed comparative example, the security performance of battery and the circulation under the high temperature, storge quality be improved significantly.
Claims (8)
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| CNB2004100521698A CN100344015C (en) | 2004-11-06 | 2004-11-06 | Method for preparing lithium secondary battery anode tab and lithium ion secondary battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101174684B (en) * | 2006-11-02 | 2010-12-22 | 比亚迪股份有限公司 | Battery anode and lithium ion battery using the same and their production method |
| CN102456916A (en) * | 2010-10-29 | 2012-05-16 | 株式会社日立制作所 | Lithium ion secondary battery |
| CN101295804B (en) * | 2007-04-27 | 2013-02-27 | 三洋电机株式会社 | Non aqueous electrolyte secondary cell and method for producing same |
| CN103794794A (en) * | 2012-10-30 | 2014-05-14 | 华为技术有限公司 | Lithium battery anode and preparation method, lithium battery and preparation method and application |
| CN104779366A (en) * | 2015-04-15 | 2015-07-15 | 东莞市创明电池技术有限公司 | A kind of preparation method of lithium-ion battery negative plate and prepared lithium-ion battery |
| CN106803593A (en) * | 2017-01-09 | 2017-06-06 | 浙江薄睿新材料有限公司 | A kind of complex function conductive coating and preparation method thereof |
| CN110534708A (en) * | 2019-08-26 | 2019-12-03 | 贵州大学 | A kind of preparation method of lithium carbonate cladding lithium cobaltate composite electrode |
| CN117976927A (en) * | 2024-02-05 | 2024-05-03 | 武汉船用电力推进装置研究所(中国船舶集团有限公司第七一二研究所) | A method for preparing a lithium manganese dioxide battery |
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Family Cites Families (3)
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| JPH09147864A (en) * | 1995-11-24 | 1997-06-06 | Sanyo Electric Co Ltd | Nonaqueous electrolyte battery and its manufacture |
| JPH09219188A (en) * | 1996-02-08 | 1997-08-19 | Sony Corp | Non-aqueous electrolyte secondary battery and method of manufacturing the same |
| JP4292761B2 (en) * | 2002-07-23 | 2009-07-08 | 日鉱金属株式会社 | Method for producing positive electrode material for lithium secondary battery |
-
2004
- 2004-11-06 CN CNB2004100521698A patent/CN100344015C/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101174684B (en) * | 2006-11-02 | 2010-12-22 | 比亚迪股份有限公司 | Battery anode and lithium ion battery using the same and their production method |
| CN101295804B (en) * | 2007-04-27 | 2013-02-27 | 三洋电机株式会社 | Non aqueous electrolyte secondary cell and method for producing same |
| CN102456916A (en) * | 2010-10-29 | 2012-05-16 | 株式会社日立制作所 | Lithium ion secondary battery |
| CN103794794A (en) * | 2012-10-30 | 2014-05-14 | 华为技术有限公司 | Lithium battery anode and preparation method, lithium battery and preparation method and application |
| CN103794794B (en) * | 2012-10-30 | 2016-08-10 | 华为技术有限公司 | Lithium battery anode and preparation method thereof, lithium battery and preparation method and application |
| CN104779366A (en) * | 2015-04-15 | 2015-07-15 | 东莞市创明电池技术有限公司 | A kind of preparation method of lithium-ion battery negative plate and prepared lithium-ion battery |
| CN106803593A (en) * | 2017-01-09 | 2017-06-06 | 浙江薄睿新材料有限公司 | A kind of complex function conductive coating and preparation method thereof |
| CN106803593B (en) * | 2017-01-09 | 2019-11-29 | 浙江薄睿新材料有限公司 | A kind of complex function conductive coating and preparation method thereof |
| CN110534708A (en) * | 2019-08-26 | 2019-12-03 | 贵州大学 | A kind of preparation method of lithium carbonate cladding lithium cobaltate composite electrode |
| CN117976927A (en) * | 2024-02-05 | 2024-05-03 | 武汉船用电力推进装置研究所(中国船舶集团有限公司第七一二研究所) | A method for preparing a lithium manganese dioxide battery |
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