CN1588674A - Positive pole processing method for secondary lithium ion cell - Google Patents

Positive pole processing method for secondary lithium ion cell Download PDF

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Publication number
CN1588674A
CN1588674A CNA2004100516666A CN200410051666A CN1588674A CN 1588674 A CN1588674 A CN 1588674A CN A2004100516666 A CNA2004100516666 A CN A2004100516666A CN 200410051666 A CN200410051666 A CN 200410051666A CN 1588674 A CN1588674 A CN 1588674A
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lico
positive pole
secondary lithium
lithium battery
battery according
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郭春泰
陈国荣
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Huizhou TCL Jinneng Battery Co Ltd
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Huizhou TCL Jinneng Battery Co Ltd
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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
    • 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

Abstract

The characteristics are: easy oxidized metal or nonmetal organic or inorganic salt solution is used as oxide presoma, soaking LiCo1-xMxO2 particles, then drying 3-8 hours in temp. 80-150 deg.C, baking 3-9 hours in temp. 400-800 deg.C, by grinding, LiCo1-xMxO2-A2On positive electrode powder that surface is cladded by oxide is obtained, 0 is less than or equal to X is less than or equal to 1.0, A is easy oxidated metal or nonmetal. The other way is adding precipitating agent into said easy oxidated metal or nonmetal inorganic or organic salt solution to obtain oxide or salt emulsion, soaking LiCo1-xMxO2 particles, drying 3-8 hours in temp. 80-150 deg.C, baking 3-9 hours in temp. 400-800 deg.C, by grinding, to obtain positive electrode material that surface is cladded by oxide, M=Ni, Mn, Cr, A is easy oxidated metal or nonmetal. By the invention, problem that polymer lithium ion secondary cell capacity is attenuated rapidly when charging and discharging more than 4.2V and circulating in IC speed rate is resolved to increase capacity of positive electrode.

Description

The method for processing positive pole of secondary lithium battery
Technical field
The present invention relates to a kind of method for processing positive pole of secondary lithium battery, particularly the surface treatment method of secondary lithium battery positive pole.
Background technology
LiCoO 2Be the α-NaFeO of hexagonal crystal system 2The type layer structure has excellent electrochemical properties, is used for the positive electrode of commercialization lithium rechargeable battery, theoretical capacity 274.4.2V Reversible Cycle capacity 140mAh/g under the normal condition, Li xCoO 2Be approximately the 3.9V Open Circuit Potential when x=1, reversible x scope is 0.99-0.5 when discharging and recharging.Under charged state, when being higher than 4.3V, positive electrode is because a large amount of lithium ions are deviate from, and it is unstable that structure becomes, and analyses easily that oxygen decomposes, phenomenons such as transformation, active material dissolving mutually, while Li xCoO 2During the lithium embedding went out, volume expanded along the c-axle, and (the relative lithium of 4.2V) expansion rate is 2.6% when x=0.5, is 3% when 4.5V.Because the embedding embedding of lithium goes out, anode structure is degenerated, the Co dissolving, and capacity attenuation is very fast, even dissolve 1% Co, capacity attenuation 10% after 25 weeks of circulation.How at LiCoO 2Under the situation of shortage of resources, make full use of LiCoO 2Resource realizes the economic worth that it is maximum, has very significant meaning.
The people such as Taiwan Li Ri fine jade, point out simultaneously at US Patent No. 2004/0076884 A1 and Chinese patent CN1492527A recently, by lithium and cobalt oxides being impregnated in the aqueous solution of the ion that contains Zr, Ti, B, Al, Ga, and this impregnated lithium and cobalt oxides particle of calcining and to obtain the surface upper with inorganic oxide ZrO 2, TiO 2, B 2O 3, Al 2O 3, Ga 2O 3Modification lithium cobalt oxygen particle.The lithium cobalt oxygen of modification is as the positive electrode of lithium ion battery, and the lithium metal is a negative pole, with the 1M LiPF of EC (ethylene carbonate) and DEC (diethyl carbonate) mixed solvent 6Solution is electrolyte, assembling 2030-Type button half-cell.Circulate after 100 weeks with 0.2C (28mAh/g) charge-discharge velocity, preferably can keep the initial discharge specific capacity more than 90%.CN1501129 invents a kind of method of anode material for lithium-ion batteries of finishing, and this positive electrode is to handle the positive electrode base material by salt solution impregnation, and quench hot obtains.With LiM xN 1-xO 2Or LiM xMn 2-xO 4Be base material, M, N are a kind of among Co, Ni, Mn, the Cr, 0≤x≤0.8, and the finishing coat structure is A xB yO 2, wherein A, B are selected from a kind of among Li, Mg, Al, Sn, the B.This finishing positive electrode and electrolyte compatibility are better, stable electrochemical property.US5693435 invents Li xCoO 2(x=1--1.15) at 950 ℃--1000 ℃ of quenching 0.25h--10h obtain the lithium intercalation compound, can reach 4.4V with 0.1C speed charge and discharge cycles voltage.
Generally speaking, the charge and discharge speed of the secondary lithium battery that the positive electrode of the secondary lithium battery that obtains with technique scheme is prepared is still lower, is not more than 0.2C, the Reversible Cycle poor-performing, and the battery actual capacity is on the low side.
Summary of the invention
The purpose of this invention is to provide a kind of lithium ion secondary battery anode material LiCo 1-xM xO 2Processing method, process by this method the Reversible Cycle performance can improve lithium rechargeable battery, make LiCo 1-xM xO 2The Reversible Cycle voltage of positive electrode is to 4.2--4.6V, and can promote the lithium rechargeable battery actual capacity, promotes the lithium rechargeable battery charge-discharge velocity.
The object of the present invention is achieved like this:
Take the metal of easy oxidation or nonmetallic inorganic or organic slat solution as oxide precursor, dipping LiCo 1-xM xO 2Particle, then through 80--150 ℃ of dry 3--8h, 400--800 ℃ of roast 3--9h through grinding, obtains the LiCo of oxide coated on surface 1-xM xO 2-A 2O nPositive electrode powder, wherein 0≤x≤1.0; A is the metal of easy oxidation or nonmetal.
Or in the metal of above-mentioned easy oxidation or nonmetallic inorganic or organic slat solution, add precipitating reagent, obtain oxide or salt emulsion, dipping LiCo 1-xM xO 2Particle.Through 80--150 ℃ of dry 3--8h, 400--800 ℃ roast 3--9h, grinding, obtain the LiCo of oxide coated on surface 1-xM xO 2-A 2O xOr LiCo 1-xM xO 2-A yB zO nPositive electrode, wherein, 0≤x≤1.0; M=Ni, Mn, Cr; A is the metal of easy oxidation or nonmetal; B=C, P.
It wherein is the metal of easy oxidation or nonmetal for Mg, Al, B, Zr or Ti.
Wherein, Mg, Al, Zr salt are nitrate, oxalates, acetate and boric acid or titanate esters, precipitation reagent is lithium hydroxide, ammoniacal liquor, urea, ammonium hydrogencarbonate, carbonic acid ammonia, DAP, ammonium di-hydrogen phosphate or phosphoric acid ammonia, and processed positive electrode comprises LiCoO 2, LiNiO 2, LiMnO 2, Li 2Mn 2O 4, LiCo 1-xNi xO 2, LiCo 1-xMn xO 2, LiCo 1-xCr xO 2
The LiCo that will obtain with said method 1-xM xO 2-A 2O x(or LiCo 1-xM xO 2-A yB zO nBut) be negative material, 1M LiPF as the lamellar graphite of positive electrode, BF, MCMB and other embedding lithium 6(EC/DEC=1: 1), PP (or PE) is barrier film to electrolyte, makes the flexible package shell with aluminum-plastic composite membrane.Core strueture is with positive pole/barrier film/negative pole/barrier film stacked (or positive pole/barrier film/negative pole/membrane winding formula), carry out 3--4.2V, 4.4V, 3--4.6V loop test at cell tester, charging and discharging currents is 1C, experimental results show that, the lithium ion battery that the positive electrode that use prepares by method of the present invention prepares can improve the Reversible Cycle performance of lithium rechargeable battery, makes LiCo 1-xM xO 2The Reversible Cycle voltage of positive electrode is to 4.2V--4.6V, and can promote the lithium rechargeable battery actual capacity, promotes the lithium rechargeable battery charge-discharge velocity to 1C.
The present invention compared with prior art efficiently solves polymer lithium ion secondary battery and discharges and recharges when being higher than 4.2V, and the rapid attenuation problem of capacity during with the 1C rate loop promotes anodal reversible gram volume.Its principle is: LiCo 1-xM xO 2Surface coated inorganic oxide or salt, when a large amount of embeddings of lithium ion went out, on the one hand, inorganic ions disperseed LiCo 1-xM xO 2Lattice tension force makes structure keep stable, reduces the stripping of Co, and on the other hand, the inorganic oxide such as Mg, Al, B or salt and compatibility of electrolyte are better, are conducive to improve the stability of SEI film.To utilize positive electrode that oxide that the present invention obtains or salt coats as positive electrode, the stratiform material with carbon element is negative material, 1M LiPF 6(EC/DEC=1: 1) be electrolyte, PP or PE are barrier film, form stacked or coiled lithium-ion secondary battery, in the 3--4.6V scope, circulate 100 all rear Capacitance reserves more than 90% with 1C (138mAh/g).Manufacturing conditions is all finished by the large-scale production Wiring technology among the present invention, and method is easy, be fit to large-scale production, good application prospects is arranged.
Description of drawings
Fig. 1 coats LiCoO for MgO 2Front and back circulation time discharge capacity between 3--4.2V changes
Fig. 2 coats LiCoO for MgO 2Front and back circulation time discharge capacity between 3--4.4V changes
Fig. 3 coats LiCoO for MgO 2Front and back circulation time discharge capacity between 3--4.6V changes
Embodiment
Case study on implementation 1
At first carrying out positive pole processes: with Mg (Ac) 2Be dissolved in 5 times the deionized water and obtain salting liquid, add in proportion LiCoO 2(average grain diameter 6 μ m), the consumption of inorganic salts is with LiCoO 2-M 2O xMiddle oxide content 0.5,1,1.5% calculates.Mix back 120 ℃ of preliminary treatment 7h and remove moisture,, obtain the lithium cobalt oxygen LiCoO that MgO coats at 500 ℃, 600 ℃, 700 ℃ quench respectively 3h, 5h, 7h 2-MgO, preferably 600 ℃ of 5h wherein, covering amount 1%, heat treatment 7h.
Second step, anodal preparation: coat MgO-LiCoO with the surface 2Be positive electrode, PVDF is bonding agent, and acetylene black is conductive carbon black, and three's mass ratio is positive electrode: bonding agent: conductive agent=92: 5: 3, carry out smear take aluminium foil as collector, drying, compressing tablet, the die-cut positive plate of making length * wide=41.5mm * 31mm.
The 3rd step, the negative pole preparation: with BF (or MCMB) is negative material, PVDF is a bonding agent, acetylene black is conductive agent, three's ratio is BF: bonding agent: conductive agent=92: 5: 3, with the Copper Foil is the agent fluid, smear, drying, compressing tablet, the die-cut negative plate of making length * wide=41.5mm * 31mm.
In the 4th step, lamination: with the above-mentioned positive/negative plate that is complementary, be barrier film with PP (or PE), press negative pole/barrier film/positive pole/barrier film/negative pole, top-down order is put well, at last with anodal single face bag tail, obtains laminated structure electricity core.
In the 5th step, assemble: place the battery core of folding in the plastic-aluminum flexible packing shell of in advance compression molding, three edge seals of flexible package, leaving is liquid injection port on one side with heat sealing machine.
The 6th step, fluid injection: in the Ar of drying glove box, inject an amount of 1M LiPF from above-mentioned electric core liquid injection port 6Electrolyte (EC/DEC=1: 1 (mass ratio)), shift out glove box after sealing.
In the 7th step, change into: dash to half electricity with 0.2C speed, after suitably placing, charge and discharge a week with 0.5C speed 3--4.2V again, charged and discharged for three weeks, obtain the nominal capacity 580mAh (being equivalent to 138mAh/g) of battery with 1C.
The 8th step, test: with the above-mentioned battery core that changes into, respectively in 3--4.2V, 3--4.4V, 3--4.6V, all with 1C (138mAh/g) circulation, see Fig. 1-Fig. 3, after the positive electrode surface coats and processes, in 3--4.6V, the battery core for preparing with this positive electrode has preferably cycle performance.
Case study on implementation 2
With Al (NO 3) 3Be dissolved in 5 times of deionized waters, splash into precipitating reagent ammoniacal liquor or the phosphoric acid ammonia of equivalent, obtain white emulsion, slowly add the LiCoO of certain mass 2(average grain diameter 6 μ m), inorganic salts Al (NO 3) 3Consumption with LiCoO 2-Al 2O 3Middle oxide mass is 0.5%, 1%, 1.5% calculating.Mix rear 130 ℃ of preliminary treatment 5h and remove moisture, at 500 ℃, 600 ℃, 700 ℃ quench respectively 3h, 5h, 7h, obtain Al 2O 3(or AlPO 4Or the two mixture) LiCoO that coats 2, preferably 600 ℃ of 7h, covering amount 1%.
Battery preparation technique and respective cycle test are with case study on implementation 1.
Case study on implementation 3
With Al (Ac) 3(or aluminium isopropoxide) with the dissolving of 5 times ethanol (if dissolve bad can with the Al (NO of equivalent 3) 3Mix and use), the LiCoO of adding certain mass 2(average grain diameter 6 μ m), the Al of the consumption of aluminium salt to coat 2O 3Be LiCoO 2The 0.5--1% of quality calculates.Mix rear 90 ℃ of preliminary treatment 7h and remove moisture, at 500 ℃, 600 ℃, 700 ℃ quench respectively 3h, 5h, 7h, obtain Al 2O 3The lithium cobalt oxygen LiCoO that coats 2-Al 2O 3, preferably 600 ℃ of 5h, covering amount 1%.
Battery preparation technique and respective cycle test are with case study on implementation 1.
Case study on implementation 4
With Al (Ac) 3With Mg (Ac) 2Mixing is dissolved in 5 times of deionized waters, adds in proportion LiCoO 2(average grain diameter 6 μ m), aluminium salt and magnesium salts quality are calculated by coating 1% oxide, wherein Al 2O 3: MgO=1: 1 (mass ratio).Mix rear 90 ℃ of preliminary treatment 6h and remove moisture, at 500 ℃, 600 ℃, 700 ℃ quench respectively 3h, 5h, 7h, obtain Al 2O 3, the lithium cobalt oxygen LiCoO that mix to coat of MgO 2, preferably 600 ℃ of 5h mix covering amount 1%.
Battery preparation technique and respective cycle test are with case study on implementation 1.
Case study on implementation 5
Press the method Mg (Ac) of case study on implementation 1 2The aqueous solution is handled LiCo 1-xNi xO 2, obtain the LiCo that MgO coats 1-xNi xO 2Make the lamination type electric core of nominal capacity 580mAh equally, its battery performance similar embodiment 1.
Case study on implementation 6
Press the method for case study on implementation 2 and process LiCo with the emulsion of Al 1-xMn xO 2, obtain Al 2O 3Or AlPO 4The LiCo that coats 1-xMn xO 2Make the lamination type electric core of nominal capacity 580mAh equally, it is greater than 4.2V circulation similar embodiment 1.
Comparative Examples 1
With untreated LiCoO 2Be positive pole, all the other materials are with above-mentioned case study on implementation 1, and preparation technology and condition are undertaken by case study on implementation 1, obtain with respect to handling LiCoO 2The electric core of normal contrast of (comprising case study on implementation 1-4), Fig. 1, Fig. 2, Fig. 3 are seen in its 3--4.2V, 3--4.4V, 3--4.6V circulation, and greater than the 4.2V circulation time, appearance is fallen very fast at voltage, and battery life is very short.
Comparative Examples 2
Use untreated LiCo 1-xNi xO 2Be positive electrode, press the preparation of the foregoing description 5 technologies and condition with respect to the LiCo that handles 1-xNi xO 2Contrast electricity core, its different voltage cycle are similar to comparative example 1.
Comparative Examples 3
Use untreated LiCo 1-xMn xO 2Be positive electrode, press the preparation of the foregoing description 5 technologies and condition with respect to the LiCo that handles 1-xMn xO 2Contrast electric core, its different voltage cycle are similar to comparative example 1.

Claims (12)

1. the method for processing positive pole of a secondary lithium battery is characterized in that: take the metal of easy oxidation or nonmetallic inorganic or organic slat solution as oxide precursor, and dipping LiCo 1-xM xO 2Particle, then through 80--150 ℃ of dry 3--8h, 400--800 ℃ of roast 3--9h through grinding, obtains the LiCo of oxide coated on surface 1-xM xO 2-A 2O nPositive electrode powder, wherein 0≤x≤1.0; M=Ni, Mn or Cr; A is the metal of easy oxidation or nonmetal.
2. the method for processing positive pole of a secondary lithium battery is characterized in that: add precipitating reagent in the metal of easily oxidation or nonmetallic inorganic or organic slat solution, obtain oxide or salt emulsion or coagulant liquid, dipping LiCo 1-xM xO 2Particle, through 80--150 ℃ of dry 3--8h, 400--800 ℃ of roast 3--9h through grinding, obtains the LiCo of oxide coated on surface 1-xM xO 2-A 2O nOr LiCo 1-xM xO 2-A yB zO nThe positive powder powder material, wherein, 0≤x≤1.0; M=Ni, Mn or Cr; A=is the metal of easy oxidation or nonmetal; B=C or P.
3. the method for processing positive pole of secondary lithium battery according to claim 1 and 2 is characterized in that the metal of described easy oxidation or nonmetallic inorganic or organic salt are the inorganic or organic salt of solubility of Mg, Al, B, Zr or Ti.
4. the method for processing positive pole of secondary lithium battery according to claim 3 is characterized in that Mg, Al, Zr salt are nitrate, acetate or oxalates.
5. the method for processing positive pole of secondary lithium battery according to claim 3 is characterized in that the metal of easy oxidation or nonmetallic inorganic or organic salt replace with boric acid or titanate esters.
6. the method for processing positive pole of secondary lithium battery according to claim 1 is characterized in that the LiCo of oxide coated on surface 1-xM xO 2-A 2O nN=3 when middle A is Al, B, n=2 when A is Mg, Zr, Ti.
7. the method for processing positive pole of secondary lithium battery according to claim 1 is characterized in that processed positive electrode comprises LiCoO 2, LiNiO 2, LiMnO 2, Li 2Mn 2O 4, LiCo 1-xNi xO 2, LiCo 1-xMn xO 2, LiCo 1-xCr xO 2
8. the method for processing positive pole of secondary lithium battery according to claim 1 is characterized in that described emulsion or coagulant liquid are new system, and solid particle size is 3-5nm in emulsion and the coagulant liquid.
9. the method for processing positive pole of secondary lithium battery according to claim 2 is characterized in that described precipitation reagent is lithium hydroxide, ammoniacal liquor, urea, ammonium hydrogencarbonate, carbonic acid ammonia, DAP, ammonium di-hydrogen phosphate or phosphoric acid ammonia.
10. the method for processing positive pole of secondary lithium battery according to claim 1 and 2 is characterized in that LiCo 1-xM xO 2Surface coated oxide or salt thickness are 8--15nm.
11. the method for processing positive pole of secondary lithium battery according to claim 1 and 2 is characterized in that raw material Li Co 1-xCr xO 2Average grain diameter be 3--15 μ m.
12. the method for processing positive pole of secondary lithium battery according to claim 1 and 2 is characterized in that coating the soild oxide of usefulness or the quality of salt is LiCo 1-xCr xO 2The 0.5--3% of quality.
CNA2004100516666A 2004-09-28 2004-09-28 Positive pole processing method for secondary lithium ion cell Pending CN1588674A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101834289A (en) * 2010-04-28 2010-09-15 东莞新能源科技有限公司 Preparation method of lithium-ion battery anode material with oxide coated on surface
CN101950803A (en) * 2010-05-17 2011-01-19 东莞新能源科技有限公司 Preparation method of cathode material of lithium ion battery coated with metal oxides on surface
CN102163718A (en) * 2010-02-18 2011-08-24 三洋电机株式会社 Positive electrode active material for lithium secondary battery, method of manufacturing the same, and lithium secondary battery using the same
CN102623688A (en) * 2012-03-23 2012-08-01 江苏科捷锂电池有限公司 Preparation method and surface finish method for nano bedded lithium-rich material
CN102956895A (en) * 2012-11-15 2013-03-06 北大先行科技产业有限公司 Surface composite coated anode material, preparation method thereof and lithium ion battery
CN103700846A (en) * 2013-12-24 2014-04-02 广西南宁市蓝天电极材料有限公司 Coated modified lithium cobalt oxide anode material of lithium ion battery and preparation method
CN113611850A (en) * 2021-10-09 2021-11-05 天津国安盟固利新材料科技股份有限公司 Positive electrode material and preparation method and application thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102163718A (en) * 2010-02-18 2011-08-24 三洋电机株式会社 Positive electrode active material for lithium secondary battery, method of manufacturing the same, and lithium secondary battery using the same
CN101834289A (en) * 2010-04-28 2010-09-15 东莞新能源科技有限公司 Preparation method of lithium-ion battery anode material with oxide coated on surface
CN101834289B (en) * 2010-04-28 2014-03-12 东莞新能源科技有限公司 Preparation method of lithium-ion battery anode material with oxide coated on surface
CN101950803A (en) * 2010-05-17 2011-01-19 东莞新能源科技有限公司 Preparation method of cathode material of lithium ion battery coated with metal oxides on surface
CN102623688A (en) * 2012-03-23 2012-08-01 江苏科捷锂电池有限公司 Preparation method and surface finish method for nano bedded lithium-rich material
CN102956895A (en) * 2012-11-15 2013-03-06 北大先行科技产业有限公司 Surface composite coated anode material, preparation method thereof and lithium ion battery
CN102956895B (en) * 2012-11-15 2015-10-14 北大先行科技产业有限公司 Positive electrode that surface recombination is coated and preparation method thereof and lithium ion battery
CN103700846A (en) * 2013-12-24 2014-04-02 广西南宁市蓝天电极材料有限公司 Coated modified lithium cobalt oxide anode material of lithium ion battery and preparation method
CN113611850A (en) * 2021-10-09 2021-11-05 天津国安盟固利新材料科技股份有限公司 Positive electrode material and preparation method and application thereof

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