CN108807845A - A kind of button full battery and preparation method thereof of metatitanic acid pole piece and graphite pole piece composition - Google Patents

A kind of button full battery and preparation method thereof of metatitanic acid pole piece and graphite pole piece composition Download PDF

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Publication number
CN108807845A
CN108807845A CN201810878961.0A CN201810878961A CN108807845A CN 108807845 A CN108807845 A CN 108807845A CN 201810878961 A CN201810878961 A CN 201810878961A CN 108807845 A CN108807845 A CN 108807845A
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Prior art keywords
pole piece
full battery
graphite
metatitanic acid
button full
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CN201810878961.0A
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CN108807845B (en
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朱敏
付健
黄绍丰
姜建成
张怡
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Anhui Keda Power New Material Co Ltd
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Anhui Keda Power New Material Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/04Construction or manufacture in general
    • H01M10/0422Cells or battery with cylindrical casing
    • H01M10/0427Button cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/058Construction or manufacture
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses the button full batteries and preparation method thereof that a kind of metatitanic acid pole piece and graphite pole piece form.The preparation method of the button full battery includes:The metatitanic acid pole piece and graphite pole piece of preparation prepare metal lithium sheet;Using graphite pole piece as anode pole piece, metal lithium sheet is assembled into button full battery one, then part discharge treatment as cathode pole piece in glove box;It dismantles the button full battery one after discharge treatment to obtain lithium intercalated graphite pole piece, then using lithium intercalated graphite pole piece as cathode pole piece, using metatitanic acid pole piece as anode pole piece, button full battery two is assembled into glove box;Button full battery two is stood into finished product.The present invention to graphite pole piece by carrying out lithium ion insertion, to obtain the button full battery using metatitanic acid pole piece as anode pole piece, using graphite pole piece as cathode pole piece, and the security and stability of the button full battery is good, rapid charging performance is excellent, have extended cycle life, high temperature resistance is good.

Description

A kind of button full battery and preparation method thereof of metatitanic acid pole piece and graphite pole piece composition
Technical field
The button formed the present invention relates to battery technology field more particularly to a kind of metatitanic acid pole piece and graphite pole piece is entirely electric Pond and preparation method thereof.
Background technology
For lithium titanate battery in charge and discharge, lithium ion insertion will not cause the variation of lithium titanate crystalline structure with deintercalation, because This has little effect the structure of lithium titanate material.Just because of this, lithium titanate is also referred to as " zero strain material ".Lithium titanate electricity Compared with the ferric phosphate lithium cell of current " trickle charge is at most at most used 2 years using 5 years, fast charge ", advantage is very prominent in pond.According to Test data measures, common batteries service life cycle average out to 3000 times, and the complete charge and discharge cycles number of lithium titanate battery Up to 30,000 times or more, after using 10 years as power battery, energy-storage battery may can also be used as again with 20 years.Titanium at present Sour lithium is used as the negative material of battery;It, can only be with the electricity containing lithium since lithium titanate itself can not provide lithium source Pole material is arranged in pairs or groups, so can not directly make battery between metatitanic acid pole piece and graphite.However, the present invention proposes one kind The button full battery and preparation method thereof of metatitanic acid pole piece and graphite pole piece composition.
Invention content
To solve the above-mentioned problems, the present invention provide a kind of metatitanic acid pole piece and graphite pole piece composition button full battery and Preparation method, the present invention to graphite pole piece by carrying out lithium ion insertion, to obtain using metatitanic acid pole piece as positive pole Piece, the button full battery using graphite pole piece as cathode pole piece, the security and stability of the button full battery is good, rapid charging performance is excellent It is different, have extended cycle life, high temperature resistance it is good.
In order to achieve the above purpose, technical scheme is as follows:
Present invention aims at a kind of preparation method for the button full battery for providing metatitanic acid pole piece and graphite pole piece composition, Step is:
(1) metatitanic acid pole piece and graphite pole piece, are then dried in vacuo by the metatitanic acid pole piece and graphite pole piece prepared, Prepare metal lithium sheet;
(2) using graphite pole piece as anode pole piece, it is complete to be assembled into button as cathode pole piece in glove box for metal lithium sheet Then button full battery one is placed in test cabinet by battery one, with 12~14h of test software discharge treatment;
(3) the button full battery one after discharge treatment is put into glove box, dismantles button full battery one and obtains lithium intercalated graphite Pole piece, using metatitanic acid pole piece as anode pole piece, is assembled into then using lithium intercalated graphite pole piece as cathode pole piece in glove box Button full battery two.
(4) button full battery two is stood into 2h~obtain button full battery finished product for 24 hours.
Further, in the step (1) metatitanic acid pole piece preparation process:By lithium titanate, conductive agent, binder solution By (80~83):(8~10):(7~12) weight ratio is added in beaker, and additional NMP obtains mixed solution, the addition of NMP For lithium titanate, conductive agent and binder gross mass 5%~10%;Beaker is put into high speed dispersor, with 1500~ 5~10min of rotating speed high speed rotation of 2000r/min;The mixed solution of mixing is uniformly coated on copper foil with automatic coating machine; The copper foil coated is put into baking oven, 60~80min is toasted at a temperature of 80~100 DEG C;By the pole piece electromotive roller after drying Press carries out roll-in, and roll-in to compacted density is 1.1~1.3g/cm3;The good pole piece of roll-in is obtained into diameter with punching machine punch For the metatitanic acid pole piece of 10~12mm.
Further, in the step (1) graphite pole piece preparation process:By graphite, conductive agent, binder by (92~ 95):(1.5~2.5):(2.5~6.5) weight ratio is in beaker, additional NMP mixed solutions, the addition of NMP be graphite, The 10%~20% of conductive agent and binder gross mass;Beaker is put into high speed dispersor, with turning for 1500~2000r/min Fast 5~10min of high speed rotation;The mixed solution of mixing is uniformly coated on copper foil with automatic coating machine;The copper foil that will be coated It is put into baking oven, 60~80min is toasted at a temperature of 80~100 DEG C;Pole piece electricity consumption transmission roller press after drying is subjected to roll-in, Roll-in to compacted density is 1.45-1.65g/cm3;The good pole piece of roll-in is obtained a diameter of 12~14mm's with punching machine punch Graphite pole piece.
Further, the conductive agent is SP;The binder is the nmp solution of PVDF, mass fraction 5%.
Further, in the step (1):Metatitanic acid pole piece is dried in vacuo 8h~48h, graphite pole at 80~100 DEG C Piece is in 110~130 DEG C of vacuum 8h~48h.
Further, in the step (1):The graphite pole piece capacity is 1~2 times of metatitanic acid pole piece capacity;It is described Metal lithium sheet is smooth by polishing rod polishing surface, and non-oxidation layer.
Further, in the step (2) button full battery one preparation process:Negative electrode casing is placed in glove box and is put down On platform, stainless steel gasket is then placed in negative electrode casing, metal lithium sheet is placed in stainless steel gasket, is added dropwise in metal lithium sheet Then electrolyte places diaphragm on metal lithium sheet electrolyte, and ensure that position fully soaks among diaphragm, is added dropwise on diaphragm Electrolyte places graphite pole piece on the electrolyte on diaphragm, stainless steel gasket is placed on graphite pole piece, finally puts anode Shell is sealed to obtain button full battery one with electronic sealing machine.
Further, in the step (4) button full battery two preparation process:Button full battery one is dismantled, glue is used Head tweezers take out graphite pole piece as lithium intercalated graphite pole piece;Negative electrode casing is placed in glove box on platform, then in negative electrode casing Middle placement stainless steel gasket places lithium intercalated graphite pole piece in stainless steel gasket, electrolyte is added dropwise in lithium intercalated graphite pole piece, then Diaphragm is placed on lithium intercalated graphite pole piece electrolyte, and ensures that position fully soaks among diaphragm, is added dropwise electrolyte on diaphragm, Metatitanic acid pole piece is placed on electrolyte on diaphragm, stainless steel gasket is placed in metatitanic acid pole piece, finally puts anode cover, is used Electronic sealing machine is sealed to obtain button full battery two.
Further, in the glove box water and oxygen content≤0.1ppm.
Another object of the present invention is to provide the button full batteries that a kind of above-mentioned metatitanic acid pole piece and graphite pole piece form Preparation method made from button full battery.
The beneficial effects of the invention are as follows:First button full battery is made in graphite pole piece and metal lithium sheet by the present invention, and with Graphite pole piece is cathode, is anode with metal lithium sheet, then carries out discharge treatment to the button full battery so that metal lithium sheet carries Lithium intercalated graphite pole piece is obtained for lithium ion, while by lithium ion insertion graphite pole piece;Then by lithium intercalated graphite pole piece and lithium titanate Button full battery is made in pole piece, and lithium intercalated graphite pole piece provides lithium ion for metatitanic acid pole piece, to obtain obtaining with metatitanic acid Button full battery of the pole piece as anode pole piece, using graphite pole piece as cathode pole piece, and the safety of button full battery is steady It is qualitative it is good, rapid charging performance is excellent, have extended cycle life, high temperature resistance is good.
Specific implementation mode
Firstly, it is necessary to explanation, will illustrate the features and advantages of the invention etc. by way of example below, however What all descriptions were intended merely to illustrate, and should not be construed as forming any restrictions to the present invention.
To avoid repeating, first by involved in embodiment related raw material technical parameter or production method be described collectively, implement It is repeated no more in example:
The conductive agent is SP;The binder is the nmp solution of PVDF, mass fraction 5%.
The graphite pole piece capacity is 1~2 times of metatitanic acid pole piece capacity;The metal lithium sheet is polished surface by polishing rod It is smooth, and non-oxidation layer.
Content≤0.1ppm of water and oxygen in the glove box.
The embodiment just provided below by this is come the button to metatitanic acid pole piece of the present invention and graphite pole piece composition Formula full battery and preparation method thereof illustrates.
Embodiment 1
The preparation method of button full battery described in the present embodiment includes the following steps:
It is prepared by metatitanic acid pole piece:Lithium titanate, conductive agent, binder solution are pressed 80:10:Beaker is added in 10 weight ratio In, additional NMP obtains 5g mixed solutions, the addition of NMP be lithium titanate, conductive agent and binder gross mass 5%~10%; Beaker is put into high speed dispersor, with the rotating speed high speed rotation 8min of 2000r/min;The mixed solution of mixing is applied with automatic Cloth machine is uniformly coated on copper foil;The copper foil coated is put into baking oven, 60min is toasted at a temperature of 90 DEG C;After drying Pole piece electricity consumption transmission roller press carries out roll-in, and roll-in to compacted density is 1.1g/cm3;By the good pole piece punching machine punch of roll-in The metatitanic acid pole piece of a diameter of 10mm is obtained, metatitanic acid pole piece is dried in vacuo for 24 hours at 80 DEG C.
It is prepared by graphite pole piece:Graphite, conductive agent, binder are pressed 93:2:In beaker, additional NMP is obtained 5 weight ratio 5g mixed solutions, the addition of NMP be graphite, conductive agent and binder gross mass 15%;Beaker is put into high speed dispersor In, with the rotating speed high speed rotation 10min of 2000r/min;The mixed solution of mixing is uniformly coated in copper foil with automatic coating machine On;The copper foil coated is put into baking oven, 60min is toasted at a temperature of 90 DEG C;By the pole piece electricity consumption transmission roller press after drying into Row roll-in, roll-in to compacted density are 1.53g/cm3;The good pole piece of roll-in is obtained into the stone of a diameter of 12mm with punching machine punch Graphite pole piece is dried in vacuo for 24 hours by black pole piece at 120 DEG C.
Negative electrode casing is placed in glove box on platform, stainless steel gasket is then placed in negative electrode casing, in stainless steel pad On piece places metal lithium sheet, and electrolyte is added dropwise in metal lithium sheet, diaphragm is then placed on metal lithium sheet electrolyte, and ensure Position fully soaks among diaphragm, and electrolyte is added dropwise on diaphragm, graphite pole piece is placed on the electrolyte on diaphragm, in graphite Stainless steel gasket is placed on pole piece, finally puts anode cover, is sealed to obtain button full battery one with electronic sealing machine, then will Button full battery one is placed in test cabinet, with test software discharge treatment 12h.
Button full battery one is dismantled, rubber head tweezers is used to take out graphite pole piece as lithium intercalated graphite pole piece;Negative electrode casing is put It sets in glove box on platform, stainless steel gasket is then placed in negative electrode casing, lithium intercalated graphite pole is placed in stainless steel gasket Piece is added dropwise electrolyte in lithium intercalated graphite pole piece, then places diaphragm on lithium intercalated graphite pole piece electrolyte, and ensure among diaphragm Position fully soaks, and electrolyte is added dropwise on diaphragm, metatitanic acid pole piece is placed on the electrolyte on diaphragm, in metatitanic acid pole piece Upper placement stainless steel gasket, finally puts anode cover, is carried out sealing to obtain button full battery two, button full battery two with electronic sealing machine It stands 2h and obtains button full battery finished product.
Constant current charge-discharge test carried out to obtained button full battery finished product, 0.5C discharge capacities 148.3mAh/g, 1C are put Capacitance 144.7mAh/g, 3C discharge capacity 140.1mAh/g, battery high rate performance are good.
Embodiment 2
The preparation method of button full battery described in the present embodiment includes the following steps:
It is prepared by metatitanic acid pole piece:Lithium titanate, conductive agent, binder solution are pressed 83:7:10 weight ratio are added in beaker, Additional NMP obtains 6g mixed solutions, the addition of NMP be lithium titanate, conductive agent and binder gross mass 10%;Beaker is put Enter in high speed dispersor, with the rotating speed high speed rotation 10min of 2000r/min;The mixed solution automatic coating machine of mixing is equal Even is coated on copper foil;The copper foil coated is put into baking oven, 70min is toasted at a temperature of 100 DEG C;Pole piece after drying is used Electronic roll squeezer carries out roll-in, and roll-in to compacted density is 1.2g/cm3;The good pole piece of roll-in is obtained directly with punching machine punch Diameter is the metatitanic acid pole piece of 11mm, and metatitanic acid pole piece is dried in vacuo 36h at 100 DEG C.
It is prepared by graphite pole piece:Graphite, conductive agent, binder are pressed 95:2:In beaker, additional NMP is obtained 3 weight ratio 6g mixed solutions, the addition of NMP be graphite, conductive agent and binder gross mass 18%;Beaker is put into high speed dispersor In, with the rotating speed high speed rotation 10min of 2000r/min;The mixed solution of mixing is uniformly coated in copper foil with automatic coating machine On;The copper foil coated is put into baking oven, 80min is toasted at a temperature of 90 DEG C;By the pole piece electricity consumption transmission roller press after drying into Row roll-in, roll-in to compacted density are 1.65g/cm3;The good pole piece of roll-in is obtained into the stone of a diameter of 13mm with punching machine punch Graphite pole piece is dried in vacuo 36h at 130 DEG C by black pole piece.
Negative electrode casing is placed in glove box on platform, stainless steel gasket is then placed in negative electrode casing, in stainless steel pad On piece places metal lithium sheet, and electrolyte is added dropwise in metal lithium sheet, diaphragm is then placed on metal lithium sheet electrolyte, and ensure Position fully soaks among diaphragm, and electrolyte is added dropwise on diaphragm, graphite pole piece is placed on the electrolyte on diaphragm, in graphite Stainless steel gasket is placed on pole piece, finally puts anode cover, is sealed to obtain button full battery one with electronic sealing machine, then will Button full battery one is placed in test cabinet, with test software discharge treatment 14h.
Button full battery one is dismantled, rubber head tweezers is used to take out graphite pole piece as lithium intercalated graphite pole piece;Negative electrode casing is put It sets in glove box on platform, stainless steel gasket is then placed in negative electrode casing, lithium intercalated graphite pole is placed in stainless steel gasket Piece is added dropwise electrolyte in lithium intercalated graphite pole piece, then places diaphragm on lithium intercalated graphite pole piece electrolyte, and ensure among diaphragm Position fully soaks, and electrolyte is added dropwise on diaphragm, metatitanic acid pole piece is placed on the electrolyte on diaphragm, in metatitanic acid pole piece Upper placement stainless steel gasket, finally puts anode cover, is sealed to obtain button full battery two with electronic sealing machine, and button is entirely electric Pond two stands and obtains button full battery finished product for 24 hours.
Constant current charge-discharge test carried out to obtained button full battery finished product, 0.5C discharge capacities 149.2mAh/g, 1C are put Capacitance 145.2mAh/g, 3C discharge capacity 140.8mAh/g, battery high rate performance are good.
Embodiment 3
The preparation method of button full battery described in the present embodiment includes the following steps:
It is prepared by metatitanic acid pole piece:Lithium titanate, conductive agent, binder solution are pressed 82:8:Beaker is added in 10 weight ratio In, additional NMP obtains 5g mixed solutions, the addition of NMP be lithium titanate, conductive agent and binder gross mass 8%;By beaker It is put into high speed dispersor, with the rotating speed high speed rotation 10min of 1500r/min;By the mixed solution automatic coating machine of mixing Uniformly it is coated on copper foil;The copper foil coated is put into baking oven, 80min is toasted at a temperature of 80 DEG C;By the pole piece after drying Electricity consumption transmission roller press carries out roll-in, and roll-in to compacted density is 1.3g/cm3;The good pole piece of roll-in is obtained with punching machine punch Metatitanic acid pole piece is dried in vacuo 48h by the metatitanic acid pole piece of a diameter of 12mm at 100 DEG C.
It is prepared by graphite pole piece:Graphite, conductive agent, binder are pressed 92:1.5:6.5 weight ratio are in beaker, additional NMP Obtain 5g mixed solutions, the addition of NMP be graphite, conductive agent and binder gross mass 18%;Beaker is put into high speed point It dissipates in machine, with the rotating speed high speed rotation 10min of 1500r/min;The mixed solution of mixing is uniformly coated in automatic coating machine On copper foil;The copper foil coated is put into baking oven, 80min is toasted at a temperature of 100 DEG C;By the electronic roll-in of the pole piece after drying Machine carries out roll-in, and roll-in to compacted density is 1.65g/cm3;The good pole piece of roll-in is obtained into a diameter of 14mm with punching machine punch Graphite pole piece, graphite pole piece is dried in vacuo 48h at 130 DEG C.
Negative electrode casing is placed in glove box on platform, stainless steel gasket is then placed in negative electrode casing, in stainless steel pad On piece places metal lithium sheet, and electrolyte is added dropwise in metal lithium sheet, diaphragm is then placed on metal lithium sheet electrolyte, and ensure Position fully soaks among diaphragm, and electrolyte is added dropwise on diaphragm, graphite pole piece is placed on the electrolyte on diaphragm, in graphite Stainless steel gasket is placed on pole piece, finally puts anode cover, is sealed to obtain button full battery one with electronic sealing machine, then will Button full battery one is placed in test cabinet, with test software discharge treatment 14h.
Button full battery one is dismantled, rubber head tweezers is used to take out graphite pole piece as lithium intercalated graphite pole piece;Negative electrode casing is put It sets in glove box on platform, stainless steel gasket is then placed in negative electrode casing, lithium intercalated graphite pole is placed in stainless steel gasket Piece is added dropwise electrolyte in lithium intercalated graphite pole piece, then places diaphragm on lithium intercalated graphite pole piece electrolyte, and ensure among diaphragm Position fully soaks, and electrolyte is added dropwise on diaphragm, metatitanic acid pole piece is placed on the electrolyte on diaphragm, in metatitanic acid pole piece Upper placement stainless steel gasket, finally puts anode cover, is sealed to obtain button full battery two with electronic sealing machine, and button is entirely electric Pond two stands and obtains button full battery finished product for 24 hours.
Constant current charge-discharge test carried out to obtained button full battery finished product, 0.5C discharge capacities 150.1mAh/g, 1C are put Capacitance 145.8mAh/g, 3C discharge capacity 142.0mAh/g, battery high rate performance are good.

Claims (10)

1. the preparation method of a kind of metatitanic acid pole piece and the button full battery of graphite pole piece composition, it is characterised in that:
(1) metatitanic acid pole piece and graphite pole piece, are then dried in vacuo by the metatitanic acid pole piece and graphite pole piece prepared, prepare Metal lithium sheet;
(2) using graphite pole piece as anode pole piece, metal lithium sheet is assembled into button full battery as cathode pole piece in glove box One, then button full battery one is placed in test cabinet, with 12~14h of test software discharge treatment;
(3) the button full battery one after discharge treatment is put into glove box, dismantles button full battery one and obtains lithium intercalated graphite pole piece, Then using lithium intercalated graphite pole piece as cathode pole piece, using metatitanic acid pole piece as anode pole piece, button is assembled into glove box Full battery two.
(4) button full battery two is stood into 2h~obtain button full battery finished product for 24 hours.
2. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, the preparation process of metatitanic acid pole piece in the step (1):By lithium titanate, conductive agent, binder solution by (80~ 83):(8~10):(7~12) weight ratio is added in beaker, and additional NMP obtains mixed solution, and the addition of NMP is metatitanic acid The 5%~10% of lithium, conductive agent and binder gross mass;Beaker is put into high speed dispersor, with 1500~2000r/min's 5~10min of rotating speed high speed rotation;The mixed solution of mixing is uniformly coated on copper foil with automatic coating machine;The copper that will be coated Foil is put into baking oven, and 60~80min is toasted at a temperature of 80~100 DEG C;Pole piece electricity consumption transmission roller press after drying is subjected to roller Pressure, roll-in to compacted density are 1.1~1.3g/cm3;The good pole piece of roll-in is obtained into a diameter of 10~12mm with punching machine punch Metatitanic acid pole piece.
3. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, the preparation process of graphite pole piece in the step (1):Graphite, conductive agent, binder are pressed into (92~95):(1.5~ 2.5):(2.5~6.5) weight ratio is in beaker, additional NMP mixed solutions, and the addition of NMP is graphite, conductive agent and glues Tie the 10%~20% of agent gross mass;Beaker is put into high speed dispersor, with the rotating speed high speed rotation of 1500~2000r/min 5~10min;The mixed solution of mixing is uniformly coated on copper foil with automatic coating machine;The copper foil coated is put into baking oven, 60~80min is toasted at a temperature of 80~100 DEG C;Pole piece electricity consumption transmission roller press after drying is subjected to roll-in, roll-in to compacting Density is 1.45-1.65g/cm3;The good pole piece of roll-in is obtained into the graphite pole piece of a diameter of 12~14mm with punching machine punch.
4. the preparation method of the button full battery of metatitanic acid pole piece and graphite pole piece composition according to claim 2 and 3, It is characterized in that:The conductive agent is SP;The binder is the nmp solution of PVDF, mass fraction 5%.
5. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, in the step (1):Metatitanic acid pole piece is dried in vacuo 8h~48h at 80~100 DEG C, graphite pole piece 110~ 130 DEG C of vacuum 8h~48h.
6. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, in the step (1):The graphite pole piece capacity is 1~2 times of metatitanic acid pole piece capacity;The metal lithium sheet by Polishing rod polishing surface is smooth, and non-oxidation layer.
7. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, the preparation process of step (2) the button full battery one:Negative electrode casing is placed in glove box on platform, is then existed Stainless steel gasket is placed in negative electrode casing, metal lithium sheet is placed in stainless steel gasket, electrolyte is added dropwise in metal lithium sheet, then Place diaphragm on metal lithium sheet electrolyte, and ensure that position fully soaks among diaphragm, electrolyte is added dropwise on diaphragm, every Graphite pole piece is placed on electrolyte on film, stainless steel gasket is placed on graphite pole piece, finally puts anode cover, with electronic sealing Machine is sealed to obtain button full battery one.
8. the preparation method of metatitanic acid pole piece according to claim 1 and the button full battery of graphite pole piece composition, special Sign is, the preparation process of step (4) the button full battery two:Button full battery one is dismantled, stone is taken out with rubber head tweezers Black pole piece is as lithium intercalated graphite pole piece;Negative electrode casing is placed in glove box on platform, stainless steel is then placed in negative electrode casing Gasket places lithium intercalated graphite pole piece in stainless steel gasket, electrolyte is added dropwise in lithium intercalated graphite pole piece, then in lithium intercalated graphite pole Diaphragm is placed on piece electrolyte, and ensures that position fully soaks among diaphragm, is added dropwise electrolyte, the electricity on diaphragm on diaphragm Solve liquid on place metatitanic acid pole piece, stainless steel gasket is placed in metatitanic acid pole piece, finally puts anode cover, with electronic sealing machine into Row sealing obtains button full battery two.
9. the preparation method of the button full battery of metatitanic acid pole piece and graphite pole piece composition according to claim 1,8 and 9, It is characterized in that:Content≤0.1ppm of water and oxygen in the glove box.
10. a kind of preparation method of the button full battery of metatitanic acid pole piece and graphite pole piece composition as described in claim 1~9 Button full battery obtained.
CN201810878961.0A 2018-08-03 2018-08-03 Button type full cell composed of lithium titanate pole piece and graphite pole piece and preparation method thereof Active CN108807845B (en)

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CN108807845A true CN108807845A (en) 2018-11-13
CN108807845B CN108807845B (en) 2021-05-28

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CN110797582A (en) * 2019-09-27 2020-02-14 双登集团股份有限公司 Preparation method of novel lithium titanate positive electrode battery
CN114361378A (en) * 2021-12-14 2022-04-15 宁德厦钨新能源材料有限公司 Electrochemical performance detection method of ternary material
CN114613614A (en) * 2022-04-11 2022-06-10 浙江浙能技术研究院有限公司 All-solid-state lithium ion capacitor and preparation method thereof

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CN105845894A (en) * 2016-05-04 2016-08-10 合肥国轩高科动力能源有限公司 Pre-lithiation method and device for negative pole pieces of lithium-ion battery
CN106532107A (en) * 2016-12-21 2017-03-22 上海杉杉科技有限公司 Lithium-ion button-type total battery used in experiments and manufacturing method thereof
CN207651591U (en) * 2018-01-15 2018-07-24 张汉军 A kind of low pressure lithium ion battery

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CN104538194A (en) * 2014-12-18 2015-04-22 天津大学 Preparation method of lithium ion capacitor (LIC) adopting pre-lithiation hard carbon negative electrode
CN105845894A (en) * 2016-05-04 2016-08-10 合肥国轩高科动力能源有限公司 Pre-lithiation method and device for negative pole pieces of lithium-ion battery
CN106532107A (en) * 2016-12-21 2017-03-22 上海杉杉科技有限公司 Lithium-ion button-type total battery used in experiments and manufacturing method thereof
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CN110797582A (en) * 2019-09-27 2020-02-14 双登集团股份有限公司 Preparation method of novel lithium titanate positive electrode battery
CN114361378A (en) * 2021-12-14 2022-04-15 宁德厦钨新能源材料有限公司 Electrochemical performance detection method of ternary material
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CN114613614A (en) * 2022-04-11 2022-06-10 浙江浙能技术研究院有限公司 All-solid-state lithium ion capacitor and preparation method thereof

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