CN103715394B - A kind of lithium ion cell positive and preparation method thereof - Google Patents
A kind of lithium ion cell positive and preparation method thereof Download PDFInfo
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- CN103715394B CN103715394B CN201310692645.1A CN201310692645A CN103715394B CN 103715394 B CN103715394 B CN 103715394B CN 201310692645 A CN201310692645 A CN 201310692645A CN 103715394 B CN103715394 B CN 103715394B
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002238 carbon nanotube film Substances 0.000 claims abstract description 68
- 239000011521 glass Substances 0.000 claims abstract description 63
- 239000005030 aluminium foil Substances 0.000 claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 48
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000007774 positive electrode material Substances 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims description 48
- 239000011248 coating agent Substances 0.000 claims description 40
- 239000010410 layer Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000004513 sizing Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- 238000003466 welding Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000006258 conductive agent Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000006245 Carbon black Super-P Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 5
- 238000004026 adhesive bonding Methods 0.000 claims description 4
- 238000007755 gap coating Methods 0.000 claims description 4
- 229910001453 nickel ion Inorganic materials 0.000 claims description 4
- -1 after fixing Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- DJZIBVUGARDLOC-UHFFFAOYSA-N [Ni]=O.[Co]=O.[Li] Chemical compound [Ni]=O.[Co]=O.[Li] DJZIBVUGARDLOC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000010405 anode material Substances 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003273 ketjen black Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 4
- OTYYBJNSLLBAGE-UHFFFAOYSA-N CN1C(CCC1)=O.[N] Chemical compound CN1C(CCC1)=O.[N] OTYYBJNSLLBAGE-UHFFFAOYSA-N 0.000 claims 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims 2
- 239000004964 aerogel Substances 0.000 claims 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims 2
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims 1
- SGDMQXAOPGGMAH-UHFFFAOYSA-N phenol;thiophene Chemical compound C=1C=CSC=1.OC1=CC=CC=C1 SGDMQXAOPGGMAH-UHFFFAOYSA-N 0.000 claims 1
- 239000010453 quartz Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000011888 foil Substances 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 238000010586 diagram Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 3
- 239000011149 active material Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 208000032953 Device battery issue Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/50—Current conducting connections for cells or batteries
- H01M50/531—Electrode connections inside a battery casing
-
- 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
Abstract
The invention discloses a kind of lithium ion cell positive and preparation method thereof, the carbon nano-tube film that positive pole is formed with carbon nano-tube macroscopic pipe is for collector, and positive electrode material layer is formed on carbon nano-tube film.Lithium ion cell positive prepared by the method and traditional aluminum foil current collector positive pole phase specific mass are lighter, and positive electrode material layer is combined more firm with collector.Manufacture method is as follows: the carbon nano-tube macroscopic pipe non-individual body utilizing reactor mouth to produce, obtained High Strength Carbon Nanotubes film on the glass substrate, positive electrode material layer is generated subsequently on carbon nano-tube rete, again the carbon nano-tube rete being loaded with positive electrode material layer is separated with glass substrate, finally installs lug to pole piece.Under same size, carbon nano-tube film is far lighter than aluminium foil, and this part quality saved is replaced to positive electrode, and battery capacity exceeds 15%-50% by than the battery taking aluminium foil as plus plate current-collecting body.The present invention is with low cost, and formation efficiency is high, and equipment is simple, can realize semicontinuous operation, be suitable for a large amount of production.
Description
Technical field
The present invention relates to cell manufacturing techniques field, particularly relate to a kind of lithium ion cell positive and preparation method thereof.
Background technology
Surely belong to lithium ion battery at the most popular power supply of current field of mobile equipment, its major part comprises positive pole, negative pole, barrier film, electrolyte and shell body.Wherein, electrode fabrication is the core technology in lithium ion battery manufacture process, and positive pole comprises plus plate current-collecting body (containing lug) and is evenly formed in the positive electrode material layer of collection liquid surface.The Weak current that active particle in electrode material layer produces need be brought together by collector and export external circuit to larger current form, and lug can coordinate collector from battery core, both positive and negative polarity to be caused external circuit better.At present, lithium ion battery generally adopts aluminium foil as plus plate current-collecting body, the good conductivity of aluminium, be easily processed into paper tinsel, mechanical strength feature that is good, relative low price makes it be used in a large number.Along with the extensive use of lithium ion battery, people have higher requirement for battery: quality is lighter, energy is higher, environmental protection more.But, aluminium foil as plus plate current-collecting body for the capacity of battery without any contribution, its quality but accounts for about 15% of whole positive pole, and this will reduce the energy density of battery greatly.In addition, because adhesion between positive electrode material layer and aluminium foil is not strong, occurs that the situation of dry linting happens occasionally, cause battery performance to worsen.
Carbon nano-tube is a kind of novel nano material, the geometry of its uniqueness and electronic band structure, make it have excellent electric property, add the low-density far below aluminium, the Macro film that carbon nano-tube gathering is formed is expected to alternative aluminium foil becomes anode current collector of lithium ion battery of new generation.
Through finding the literature search of prior art, be at present also in the research and probe stage to the research of carbon nano-tube collector.
The KeWang of Tsing-Hua University, ShuLuo, YangWu etc. are in " Super-AlignedCarbonNanotubeFilmsasCurrentCollectorsforLi ghtweightandFlexibleLithiumIonBatteries " (super uniform carbon nanotubes film is used as lightweight, pliable and tough lithium ion battery as collector) literary composition of " AdvancedFunctionalMaterials " (advanced function material) the 23rd phase 846-853 page in 2013, and proposition carbon nano-tube film is as lithium ion battery plus-negative plate collector.The manufacture craft of the electrode of carbon nano-tube film collector has been set forth in the national inventing patent (CN103187574A) that the people such as Wang Jiaping, Wang Ke of Tsing-Hua University apply at it.The work that they do describes carbon nano-tube film alternative metals well, and to serve as collector be possible.This allows people, and new angle---the energy density of lithium ion battery is gone to improve in collector aspect, is no longer confined to electrode material from one.But due to the method problem made at present, there is the deficiency of following several times in carbon nano-tube film collector: (1) masking efficiency is low, the size-constrained system of film, mechanical strength is not high; (2) although can connecting tab, but with conducting resinl connecting tab and collector, the conducting resinl of introducing have not only increased the weight of pole piece, and conducting resinl long period of soaking is easily aging in the electrolytic solution simultaneously; (3) be first form electrode material layer in electrode fabrication process, then on electrode material layer, carbon nano-tube rete is formed, compared with the technique of this coating electrode pulp layer on a current collector in making with conventional lithium ion battery, change is too large, if be used in actual production, mean that manufacturer need adjust production line on a large scale, cost is too high.
Summary of the invention
The invention provides a kind of high efficiency based on carbon nano-tube film, high-quality, and the lithium ion cell positive preparation method easily integrated with existing cell making process.
The present invention adopts following technical scheme:
The carbon nano-tube film that lithium ion cell positive of the present invention is formed with carbon nano-tube macroscopic pipe is for collector, and positive electrode material layer is formed on carbon nano-tube film; Positive plate lug adopts the form of biplate aluminium foil folder carbon nano-tube film, and realizes electrical connection by spot welding.This carbon nano-tube film surface density is lower than 1.0 × 10
-3gcm
-2, mechanical strength is 100-150Mpa.
The manufacture method of the New Type of Carbon nanotube films collector that the present invention relates to, the method is applicable to button cell, the positive pole of cylindrical battery, particularly laminated battery plate makes, and comprises the steps:
Step one, High Strength Carbon Nanotubes film preparation.The reaction solution formula of Formed nanotube of the present invention and the synthetic method of carbon nano-tube macroscopic tubulose non-individual body, with reference to patent ZL201010230938.4, then prepare High Strength Carbon Nanotubes film by carbon nano-tube macroscopic tubulose non-individual body.First, in glass bar and rectangle glass, substrate size (0.01-1.5) m × (0.01-2) m, surface sprinkling last layer volume fraction is 15%-50% alcohol water blend; Then, the macroscopical pipe non-individual body glass bar generated from reactor mouth is drawn on square glass substrate.Adopt the form of graticules in length and breadth, that is: first cover carbon nano-tube macroscopic pipe on a glass along mouth of pipe direction, obtain the rete of about 0.1 μm; Then, by glass plate half-twist, before continuation, cover carbon nano-tube macroscopic pipe in the direction, obtain, again by glass plate half-twist after the rete of about 0.1 μm, so repeating until obtain the High Strength Carbon Nanotubes film (thickness 0.2-100 μm) of desired thickness.
Step 2, carbon nano-tube rete generates positive electrode material layer.Positive active material (cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4, lithium nickel cobalt dioxide, nickel ion doped, in cobalt nickel ion doped one or more), conductive agent (in Super-P, electrically conductive graphite, Ketjen black one or more), binding agent (one in Kynoar, polyvinylidene fluoride, polytetrafluoroethylene, butadiene-styrene rubber) are mixed in proportion, wherein: conductive agent quality accounts for 3%-15%, binding agent quality accounts for 5%-10%, all the other are positive active material, regulate slurry viscosity with nitrogen methyl-prop pyrrolidone (NMP), solid content controls at 40%-50%.Ball milling 8-24h on planetary ball mill, rotating speed remains on 220-270rmin
-1above, anode sizing agent is obtained.Adopt the mode of " it is fixed that cutter moves film ", namely the glass plate being loaded with film is motionless, scraper is with certain edge of a knife (120-400 μm) feed above film, by anode sizing agent " gap coating " on carbon nano-tube film, the coating of so-called gap, be coated with exactly ink area is separated by certain white space (non-coating), has material region and white space to be alternately arranged.Coatings area lateral dimension accounts for the 0.85-0.95 of carbon nano-tube film lateral dimension, and occupy center; Pole piece width or length needed for the target battery that coatings area longitudinal size equals 2.2 times.Coating portion is not reserved by installing lug, and coating portion longitudinal size is not the 1/8-3/8 of coating portion longitudinal size.Concrete condition is shown in Fig. 1.After coating terminates, glass plate is placed in 100-120 DEG C of baking oven to dry, drying time is 30-60min.
Step 3, is separated coating carbon nano-tube rete with glass substrate.The glass substrate being loaded with coating carbon nano-tube rete is kept flat, dips the one (after mentioning hairbrush, being standard when dripless falls) of NMP, deionized water or alcohol with hairbrush.Gently brush in the carbon nanotube regions not being coated with slurry (not expanding to coating position for standard with NMP).After non-coating portion is wetting, gently scrape the edge of carbon nano-tube film with blade of carving knife, the edge of film is separated with glass substrate, after film and glass substrate separate section area can be clamped, use holder carbon nano-tube film separate section instead, with 0.5-1cms
-1speed to be not separated side lift, until the carbon nano-tube film scribbling slurry is separated completely from glass plate.The carbon nano-tube membrane portions that top scribbles anode material can be taken off from glass plate without gluing with sticking easily, and non-coating portion is dry has taken off sticky a little sticking, but also can take off from glass substrate with sticking without gluing after wetted.After end to be separated, the carbon nano-tube film being loaded with material is put into 100-120 DEG C of baking oven and place 20-30min.
Step 4, cut-parts also install lug.Film is cut into segment by the transversal centerline along each non-coatings area, uses twin rollers by positive electrode material layer and carbon nano-tube film compacting.For button cell pole piece, only each section need be placed on mould and go out
namely 5-15mm disk obtains positive plate, without the need to installing lug; For needing the battery pole piece installing lug, each section need be cut into further required pole piece size in battery making, the pole piece obtained has material part to account for 7/10-9/10, and non-coating portion accounts for 1/10-3/10.The invention provides the installation method of lug under two kinds of situations: first, when lug is positioned at pole piece side (right side is obtained in left side), (longitudinal size is 1.1-1.3 times of pole piece longitudinal size non-for pole piece coating portion to be placed in two panels aluminium foil, thickness≤20 μm) in the middle of, with pneumatic spot welding machine by the seam of upper and lower two panels aluminium foil, concrete condition is shown in Fig. 2; Second, when above lug is positioned at pole piece, with two panels aluminium foil, (lateral dimension is 1/2 of non-coatings area lateral dimension, longitudinal size is 1.4-1.6 times of lateral dimension, thickness≤20 μm) be clipped in the middle 1/2 of non-for pole piece coating portion (transverse direction), with pneumatic spot welding machine by the seam of upper and lower two panels aluminium foil, concrete condition is shown in Fig. 4.Because carbon nano-tube film is positioned in the middle of two panels aluminium foil, in two panels aluminium foil welding process, carbon nano-tube film is also just firmly fixed in the middle of two panels aluminium foil.After fixing, aluminium foil is trimmed to required form, as Fig. 3, Fig. 5, the aluminium foil wherein clamping carbon nano-tube film is lug.For making laminated battery plate, also on aluminium foil, a bit of (width equals aluminium foil width, long 1-5cm) aluminium strip with tab need be welded again.So far, positive plate just completes.
Lithium ion cell positive prepared by method of the present invention and traditional aluminum foil current collector positive pole phase specific mass are lighter, and positive electrode material layer is combined more firm with collector.Under same size, carbon nano-tube film is far lighter than aluminium foil, and this part quality saved is replaced to positive electrode, and battery capacity exceeds 15%-50% by than the battery taking aluminium foil as plus plate current-collecting body.The present invention is with low cost, and formation efficiency is high, and equipment is simple, can realize semicontinuous operation, be suitable for a large amount of production.
Good effect of the present invention is as follows:
The first, directly the carbon nano-tube macroscopic pipe non-individual body generated from reactor mouth is made film forming, masking efficiency is high, can prepare the carbon nano-tube film of arbitrary dimension size in theory, and in practical operation, prepared maximum carbon nano-tube film size reaches 1.5m × 2m.
The second, adopt the thin film-forming method of graticules in length and breadth, each carbon nanotube macroscopic view pipe in rete is interlaced, and each carbon nano-tube on microcosmic is interweaved, and the mechanical strength (100-150Mpa) that this makes the film produced have, is convenient to later use.
3rd, because carbon nano-tube film density is minimum, surface density (10 μm) < 1.0 × 10
-3gcm
-2much smaller than aluminium foil (20 μm) 5.44 × 10
-3gcm
-2, use this film collector effectively can reduce the quality of inert matter in whole electrode, thus the energy density of battery can be improved simply and effectively.
4th, due to speciality and the good wetability of carbon nano-tube film rough surface porous, its surface is more conducive to slurry attachment, enhances the cohesive force between slurry and collector, not easily occurs dry linting phenomenon.
5th, lug adopts the form of aluminium foil folder carbon nano-tube film, realizes electrical connection by spot welding.This mode is without the need to using conducting resinl, and owing to saving the quality of conducting resinl and avoiding the battery failure defect caused because conducting resinl is aging, pole piece quality is lighter simultaneously; Monolithic aluminium foil THICKNESS CONTROL is below 20 μm, and the thickness of lug part is suitable with positive electrode layer thickness, and ensureing can close contact between laminated battery plate positive/negative plate.
Accompanying drawing explanation
Fig. 1 is gap coating schematic diagram
Fig. 2 is the schematic diagram before the cutting of aluminium foil lug when lug is positioned at side
Fig. 3 is the schematic diagram after the cutting of aluminium foil lug when lug is positioned at side
Fig. 4 is schematic diagram before aluminium foil lug cutting when above lug is positioned at
Fig. 5 is schematic diagram after aluminium foil lug cutting when above lug is positioned at
1 carbon nano-tube rete, 2 positive electrode material layers, 3 aluminium foil lugs, 4 positive plates.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
The preparation of Snap-type cell positive: spraying upper volume mark on glass substrate (20cm × 20cm) and glass bar is 30% alcohol water blend, draws the macroscopical pipe non-individual body glass bar generated from reactor mouth on square glass substrate.Adopt the form of graticules in length and breadth, will the carbon nano-tube film of thickness about 10 μm be obtained on the glass substrate.By active material (LiCoO
2), conductive agent (Super-P), binding agent (Kynoar) mix with NMP (solid content remains on 45%) in the ratio of 90:4:6, puts into ball mill ball milling 10h, rotating speed 232rmin
-1, obtain anode sizing agent.Keep scraper edge 180 μm, on film, uniform application last layer slurry, puts into baking oven, 120 DEG C, 40min.Subsequently, the glass substrate being loaded with coating carbon nano-tube rete is kept flat, dips NMP with hairbrush, gently brush in the carbon nanotube regions not being coated with slurry.After non-coating portion is wetting, gently scrape the edge of carbon nano-tube film with blade of carving knife, the edge of film is separated with glass substrate, after film and glass substrate separate section area can be clamped, use holder carbon nano-tube film separate section instead, with 0.5-1cms
-1speed to be not separated side lift, until the carbon nano-tube film scribbling slurry is separated completely from glass plate.After end to be separated, the carbon nano-tube film being loaded with material is put into 120 DEG C of baking oven 20min.The carbon nano-tube film being loaded with material, after roll-in, perforating press is gone out
the disk of 12mm.So far, button cell positive pole just completes.
Embodiment 2
The preparation of individual layer laminated batteries positive pole: spraying upper volume mark on glass substrate (20cm × 36cm) and glass bar is 30% alcohol water blend, draws the macroscopical pipe non-individual body glass bar generated from reactor mouth on square glass substrate.Adopt the form of graticules in length and breadth, will the carbon nano-tube film of thickness about 13 μm be obtained on the glass substrate.By active material (LiCoO
2), conductive agent (Super-P), binding agent (Kynoar) mix with NMP (solid content 45%) in the ratio of 90:4:6, puts into ball mill ball milling 12h, rotating speed 232rmin
-1, obtain anode sizing agent.Adopt the mode of " it is fixed that cutter moves film ", the glass plate being namely loaded with film is motionless, and scraper is with 230 μm of edge of a knife feeds above film, anode sizing agent is coated with over the carbon nanotube film in " gap coating " mode, every block coating is of a size of 8cm × 18cm, gap width 4cm, and concrete condition is shown in Fig. 1.After coating terminates, glass plate is placed in 120 DEG C of baking ovens to dry.Afterwards, with non-coating portion on the hairbrush wetting carbon nanotubes layer being moistened with NMP, the edge of carbon nano-tube film is gently scraped afterwards with blade of carving knife, the edge of carbon nano-tube film is separated with glass substrate, after film and glass substrate separate section area can be clamped, use holder carbon nano-tube film separate section instead, with 0.5-1cms
-1speed to be not separated side lift, until the carbon nano-tube film scribbling slurry is separated completely from glass plate.After end to be separated, the carbon nano-tube film being loaded with material is put into 120 DEG C of baking oven 30min.The film taken off being cut into 12cm × 20cm(has material part 8cm × 18cm to be positioned at center, and all the other are non-coating portion), roll-in; After roll-in, pole piece is cut into 4.0cm × 3.0cm, wherein anode sizing agent be of a size of 3.0cm × 3.0cm(residual area by make lug stayed).Preprepared aluminium foil (thick 20 μm) is cut into 0.8cm × 3.5cm, be clipped in the middle whole for non-for pole piece coating portion with two panels aluminium foil, notice that aluminium foil does not cover anode sizing agent layer, pneumatic spot welding machine welds, the little aluminium flake and the aluminium foil that by the length with tab are 1.5cm are again welded together, aluminium foil width are trimmed to the carbon nano-tube film that 0.5cm(aluminium foil includes and also prune away in the lump).So far, individual layer laminated batteries positive pole just completes.
Embodiment 3
The preparation of multi-layer stacks anode: spraying upper volume mark on glass substrate (20cm × 36cm) and glass bar is 30% alcohol water blend, draws the macroscopical pipe non-individual body glass bar generated from reactor mouth on square glass substrate.Adopt the form of graticules in length and breadth, will the carbon nano-tube film of thickness about 13 μm be obtained on the glass substrate.By active material (LiCoO
2), conductive agent (Super-P), binding agent (Kynoar) mix with NMP (solid content 45%) in the ratio of 90:4:6, puts into ball mill ball milling ball milling 12h, rotating speed 248rmin
-1, obtain anode sizing agent.Adopt the mode of " it is fixed that cutter moves film ", anode sizing agent gap, with 230 μm of edge of a knife feeds above film, is applied on carbon nano-tube film by scraper, and every block coating is of a size of 8cm × 18cm, gap width 4cm, and concrete condition is shown in Fig. 1.After coating terminates, glass plate is placed in 120 DEG C of baking ovens to dry.Afterwards, with non-coating portion on the hairbrush wetting carbon nanotubes layer being moistened with NMP, the edge of carbon nano-tube film is gently scraped afterwards with blade of carving knife, the edge of carbon nano-tube film is separated with glass substrate, after film and glass substrate separate section area can be clamped, use holder carbon nano-tube film separate section instead, with 0.5-1cms
-1speed to be not separated side lift, until the carbon nano-tube film scribbling slurry is separated completely from glass plate.After end to be separated, the carbon nano-tube film being loaded with material is put into 120 DEG C of baking oven 30min.The film taken off being cut into 12cm × 20cm(has material part 8cm × 18cm to be positioned at center, and all the other are non-coating portion), roll-in; After roll-in, pole piece is cut into 4.0cm × 3.0cm, wherein anode sizing agent be of a size of 3.0cm × 3.0cm(residual area by make lug stayed).Preprepared aluminium foil (thick 20 μm) is cut into 1.5cm × 2.3cm, be clipped in the middle 1/2 of non-for pole piece coating portion (transverse direction) with two panels aluminium foil, see Fig. 4, notice that aluminium foil does not cover anode sizing agent layer, pneumatic spot welding machine welds, aluminium foil width is trimmed to " convex " shape shown in Fig. 5, wherein " convex " shape upper width 0.8cm.So far, multi-layer stacks anode just completes.
Embodiment 4
Table 1 is assembled into battery performance list after button cell battery for the positive pole prepared by embodiment one.As described above, made button cell is with lithium sheet for negative pole, and barrier film is thick 12 μm for the positive plate situation of example one,
the disk of 12mm.Electric performance test is carried out, through 0.1C(2.75-4.2V after battery standing 24h) after multiplying power changes into, in identical voltage range, 1C circulation obtains table 1 data.
Table 1 example one make button cell performance list
Table 2 is assembled into battery performance list after individual layer laminated batteries for the positive pole prepared by embodiment two.As described above, made individual layer laminated batteries take graphite as negative pole (negative pole material size 3.5cm × 3.5cm) to the positive plate situation of example two, and thick 12 μm of barrier film used, is of a size of 4.0cm × 4.0cm.Electric performance test is carried out, through 0.1C(2.75-4.2V after battery standing 24h) after multiplying power changes into, in identical voltage range, 1C circulation obtains table 2 data.
Table 2 example two make individual layer laminated batteries performance list
As can be seen from above data, good performance is just had prepared by the present invention, for the carbon nano-tube film of same size, it is qualitatively far below aluminium foil, if this part quality under being saved by carbon nano-tube film replaces to positive electrode, the capacity of battery exceeds 20%-50% by than the battery taking aluminium foil as plus plate current-collecting body.
Present invention process is simple, and product not only can apply in the middle of the making of conventional batteries, more obvious in the effect of flexible foldable field of batteries.Raw material of the present invention is simple and easy to get, with low cost, environmentally safe; Efficiency is high, and equipment is simple, can realize semicontinuous operation, be suitable for a large amount of production.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (10)
1. prepare a method for lithium ion cell positive, the carbon nano-tube film that this lithium ion cell positive is formed with carbon nano-tube macroscopic tubulose non-individual body is for collector, and positive electrode material layer is formed on carbon nano-tube film; Positive plate lug adopts the form of biplate aluminium foil folder carbon nano-tube film, and realizes electrical connection by spot welding; It is characterized in that: the method concrete steps are as follows:
Step one, the preparation of carbon nano-tube film, utilizes carbon nano-tube macroscopic tubulose non-individual body to prepare High Strength Carbon Nanotubes film, first, is 15%-50% alcohol water blend at glass bar and rectangle glass surface sprinkling last layer volume fraction; Then, the carbon nano-tube macroscopic tubulose non-individual body glass bar generated from reactor mouth is drawn on square glass substrate; Adopt the form of graticules in length and breadth, that is: first cover carbon nano-tube macroscopic tubulose non-individual body on a glass along mouth of pipe direction, obtain the rete of 0.1 μm; Then, by glass plate half-twist, before continuation, cover carbon nano-tube macroscopic tubulose non-individual body in the direction, obtain, again by glass plate half-twist after the rete of 0.1 μm, so repeating until obtain the carbon nano-tube film that thickness is 0.2-100 μm;
Step 2, carbon nano-tube rete generates positive electrode material layer, positive active material, conductive agent, binding agent is mixed in proportion, and regulate slurry viscosity with nitrogen methyl pyrrolidone (NMP), solid content controls at 40%-50%; Ball milling 8-24h on planetary ball mill, rotating speed remains on 220-270rmin
-1above, anode sizing agent is obtained; Adopt the mode of " it is fixed that cutter moves film ", namely the glass plate being loaded with film is motionless, scraper is with the feed above film of certain edge of a knife, by anode sizing agent " gap coating " on carbon nano-tube film, the coating of so-called gap, be coated with exactly ink area is separated by the white space of necessarily non-coating, has material region and white space to be alternately arranged; Coatings area lateral dimension accounts for the 0.85-0.95 of carbon nano-tube film lateral dimension, and occupy center; Pole piece width or length needed for the target battery that coatings area longitudinal size equals 2.2 times; Coating portion is not reserved by installing lug, and coating portion longitudinal size is not the 1/8-3/8 of coating portion longitudinal size; After coating terminates, glass plate is placed in 100-120 DEG C of baking oven to dry, drying time is 30-60min;
Step 3, coating carbon nano-tube rete is separated with glass substrate, the glass substrate being loaded with coating carbon nano-tube rete is kept flat, the one of nitrogen methyl pyrrolidone (NMP), deionized water or alcohol is dipped with hairbrush, gently brush in the carbon nanotube regions not being coated with slurry, after non-coating portion is wetting, the edge of carbon nano-tube film is gently scraped with blade of carving knife, the edge of film is separated with glass substrate, after film and glass substrate separate section area can be clamped, use holder carbon nano-tube film separate section instead, with 0.5-1cms
-1speed to be not separated side lift, until the carbon nano-tube film scribbling slurry is separated completely from glass plate; The carbon nano-tube membrane portions that top scribbles anode material can be taken off from glass plate without gluing with sticking easily, and non-coating portion is dry has taken off sticky a little sticking, but also can take off from glass substrate with sticking without gluing after wetted; After end to be separated, the carbon nano-tube film being loaded with material is put into 100-120 DEG C of baking oven and place 20-30min;
Step 4, cut-parts also install lug, film is cut into segment by the transversal centerline along each non-coatings area, use twin rollers by positive electrode material layer and carbon nano-tube film compacting, for button cell pole piece, only each section need be placed in and diameter 5-15mm disk gone out by mould namely obtain positive plate, without the need to installing lug; For needing the battery pole piece installing lug, each section need be cut into further required pole piece size in battery making, the pole piece obtained has material part to account for 7/10-9/10, and non-coating portion accounts for 1/10-3/10; Because carbon nano-tube film is positioned in the middle of two panels aluminium foil, in two panels aluminium foil welding process, carbon nano-tube film is also just firmly fixed in the middle of two panels aluminium foil, after fixing, aluminium foil is trimmed to required form, and the aluminium foil wherein clamping carbon nano-tube film is lug, for making laminated battery plate, also need weld a bit of aluminium strip with tab again on aluminium foil, the width of this section of aluminium strip equals aluminium foil width, long 1-5cm, and positive plate just completes;
Described carbon nano-tube macroscopic tubulose non-individual body is transparent, continuous print, and diameter is between 5-35mm, and density is 0.1gcm
-3, be made up of carbon nano-tube; Surface energy is lower than 73 × 10
-3nm
-2material contact with this macroscopical pipe non-individual body and all can be adsorbed by it; Its synthetic method comprises following concrete steps:
Step one is 99.8% in purity, and diameter is that quartz capillary is installed in the exit of the horizontal alundum tube reactor of 10-40mm, capillary is uniformly distributed in alundum tube exit, and number of capillary is 4-16 root, capillary inner diameter 0.5-1mm, and in each capillary, pass into nitrogen, nitrogen flow 5-30Lh
- 1;
Step 2, after the temperature of alundum tube reactor is increased to 1600-1750 DEG C, continuous print passes into nitrogen in the reactor, nitrogen flow 10-100Lh
-1;
Step 3, generates the reaction solution formula of the transparent macro pipe non-individual body be made up of carbon nano-tube, is made up of n-hexane, ferrocene, thiophene phenol; After nitrogen passes into 10 minutes in the reactor, by reaction solution with 0.5-5mlmin
- 1speed, and to pass under the bringing into of nitrogen in reactor; Reaction solution is passed into after 1 minute in reactor, the porch of reaction tube can obtain the carbon nanotube aerogel of gaseous state, continue to pass into reaction solution, by taking away the porch of reaction tube, continuous print sprays the transparent macro pipe non-individual body be made up of carbon nano-tube to carbon nanotube aerogel then in alundum tube in the exit of reaction tube, generates the speed of this non-individual body at 5-50mmin
-1between.
2. the method for claim 1, is characterized in that: this carbon nano-tube film surface density is lower than 1.0 × 10
-3gcm
-2, mechanical strength is 100-150MPa.
3. the method for claim 1, is characterized in that: the described edge of a knife is 120-400 μm.
4. method as claimed in claim 3, is characterized in that: in step one, glass substrate is of a size of (0.01-1.5) m × (0.01-2) m.
5. method as claimed in claim 3, is characterized in that: in step 2, and positive active material is one or more in cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4, lithium nickel cobalt dioxide, nickel ion doped, cobalt nickel ion doped.
6. method as claimed in claim 3, it is characterized in that: in step 2, conductive agent is one or more in Super-P, electrically conductive graphite, Ketjen black.
7. method as claimed in claim 3, it is characterized in that: in step 2, binding agent is the one in Kynoar, polyvinylidene fluoride, polytetrafluoroethylene, butadiene-styrene rubber.
8. method as claimed in claim 3, it is characterized in that: in step 2, conductive agent quality accounts for 3%-15%, and binding agent quality accounts for 5%-10%, and all the other are positive active material.
9. method as claimed in claim 3, it is characterized in that: in step 4, the installation method of lug, when lug is positioned at pole piece side, non-for pole piece coating portion is placed in the middle of two panels aluminium foil, aluminium foil longitudinal size is 1.1-1.3 times of pole piece longitudinal size, and thickness≤20 μm, with pneumatic spot welding machine by the seam of upper and lower two panels aluminium foil.
10. method as claimed in claim 3, it is characterized in that: in step 4, the installation method of lug, when above lug is positioned at pole piece, be clipped in the middle 1/2 of non-for pole piece coating portion transverse direction with two panels aluminium foil, aluminium foil lateral dimension is 1/2 of non-coatings area lateral dimension, and longitudinal size is 1.4-1.6 times of lateral dimension, thickness≤20 μm, with pneumatic spot welding machine by the seam of upper and lower two panels aluminium foil.
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