CN108807845B - Button type full cell composed of lithium titanate pole piece and graphite pole piece and preparation method thereof - Google Patents
Button type full cell composed of lithium titanate pole piece and graphite pole piece and preparation method thereof Download PDFInfo
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- CN108807845B CN108807845B CN201810878961.0A CN201810878961A CN108807845B CN 108807845 B CN108807845 B CN 108807845B CN 201810878961 A CN201810878961 A CN 201810878961A CN 108807845 B CN108807845 B CN 108807845B
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/04—Construction or manufacture in general
- H01M10/0422—Cells or battery with cylindrical casing
- H01M10/0427—Button cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a button type full cell composed of a lithium titanate pole piece and a graphite pole piece and a preparation method thereof. The preparation method of the button type full cell comprises the following steps: preparing a metal lithium sheet for the prepared lithium titanate pole piece and the graphite pole piece; assembling a graphite pole piece as a positive pole piece and a metal lithium piece as a negative pole piece into a button type full cell I in a glove box, and then performing discharge treatment on the button type full cell I; disassembling the button full-cell I after discharge treatment to obtain a lithium-embedded graphite pole piece, and then assembling a button full-cell II in a glove box by taking the lithium-embedded graphite pole piece as a negative pole piece and a lithium titanate pole piece as a positive pole piece; and standing the button type full cell II to obtain a finished product. According to the invention, the lithium ion is embedded into the graphite pole piece, so that the button type full cell taking the lithium titanate pole piece as the positive pole piece and the graphite pole piece as the negative pole piece is obtained, and the button type full cell has the advantages of good safety and stability, excellent quick charging performance, long cycle life and good high temperature resistance.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a button type full battery consisting of a lithium titanate pole piece and a graphite pole piece and a preparation method thereof.
Background
When the lithium titanate battery is charged and discharged, lithium ions are inserted and de-inserted without causing the change of the crystal structure of the lithium titanate, so that the structure of the lithium titanate material is hardly influenced. As such, lithium titanate is also known as a "zero strain material". Compared with the current lithium iron phosphate battery which is used for 5 years at most after slow charging and 2 years at most after fast charging, the lithium titanate battery has very outstanding advantages. According to test data, the cycle service life of a common battery is 3000 times on average, the complete charge-discharge cycle times of the lithium titanate battery can reach more than 3 ten thousand times, and the lithium titanate battery can be used as an energy storage battery for 20 years after being used as a power battery for 10 years. At present, lithium titanate is used as a negative electrode material of a battery; because lithium titanate can not provide a lithium source and can only be matched with an electrode material containing lithium, a battery can not be directly prepared between a lithium titanate pole piece and graphite. However, the invention provides a button type full cell composed of a lithium titanate pole piece and a graphite pole piece and a preparation method thereof.
Disclosure of Invention
In order to solve the problems, the invention provides a button type full cell composed of a lithium titanate pole piece and a graphite pole piece and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention aims to provide a preparation method of a button type full cell consisting of a lithium titanate pole piece and a graphite pole piece, which comprises the following steps:
(1) preparing a lithium titanate pole piece and a graphite pole piece, and then carrying out vacuum drying on the lithium titanate pole piece and the graphite pole piece to prepare a metal lithium piece;
(2) assembling a graphite pole piece as a positive pole piece and a metal lithium piece as a negative pole piece into a button type full cell I in a glove box, then placing the button type full cell I on a test cabinet, and carrying out discharge treatment for 12-14 h by using test software;
(3) and placing the discharged button type full battery I into a glove box, disassembling the button type full battery I to obtain a lithium-embedded graphite pole piece, and assembling a button type full battery II in the glove box by taking the lithium-embedded graphite pole piece as a negative pole piece and taking a lithium titanate pole piece as a positive pole piece.
(4) And standing the button full cell II for 2-24 h to obtain a button full cell finished product.
Further, the preparation process of the lithium titanate pole piece in the step (1) comprises the following steps: adding lithium titanate, a conductive agent and a binder solution into a beaker according to the weight ratio of (80-83) to (8-10) to (7-12), and adding NMP to obtain a mixed solution, wherein the adding amount of the NMP is 5-10% of the total mass of the lithium titanate, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500-2000 r/min for 5-10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; putting the coated copper foil into an oven, and baking for 60-80 min at the temperature of 80-100 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.1-1.3 g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a lithium titanate pole piece with the diameter of 10-12 mm.
Further, the preparation process of the graphite pole piece in the step (1) comprises the following steps: putting graphite, a conductive agent and a binder into a beaker according to the weight ratio of (92-95): (1.5-2.5): 2.5-6.5), and adding an NMP mixed solution, wherein the adding amount of the NMP is 10-20% of the total mass of the graphite, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500-2000 r/min for 5-10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; putting the coated copper foil into an oven, and baking for 60-80 min at the temperature of 80-100 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.45-1.65g/cm 3; and punching the rolled pole piece by using a punching machine to obtain the graphite pole piece with the diameter of 12-14 mm.
Further, the conductive agent is SP; the binder is an NMP solution of PVDF, and the mass fraction of the binder is 5%.
Further, in the step (1): the lithium titanate pole piece is dried in vacuum for 8-48 h at the temperature of 80-100 ℃, and the graphite pole piece is dried in vacuum for 8-48 h at the temperature of 110-130 ℃.
Further, in the step (1): the capacity of the graphite pole piece is 1-2 times of that of the lithium titanate pole piece; the surface of the metal lithium sheet is polished by a polishing rod to be smooth and has no oxide layer.
Further, the preparation process of the button full cell I in the step (2) comprises the following steps: the negative electrode shell is placed on a platform in a glove box, then a stainless steel gasket is placed in the negative electrode shell, a metal lithium sheet is placed on the stainless steel gasket, electrolyte is dripped on the metal lithium sheet, a diaphragm is placed on the metal lithium sheet electrolyte, the middle part of the diaphragm is fully wetted, the electrolyte is dripped on the diaphragm, a graphite pole piece is placed on the electrolyte on the diaphragm, the stainless steel gasket is placed on the graphite pole piece, finally, a positive electrode shell is placed, and a first button type full cell is obtained by sealing with an electric sealing machine.
Further, the preparation process of the button full cell II in the step (4) comprises the following steps: disassembling the button type full battery I, and taking out the graphite pole piece by using a rubber head forceps to serve as a lithium-embedded graphite pole piece; placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a lithium-embedded graphite pole piece on the stainless steel gasket, dropwise adding electrolyte into the lithium-embedded graphite pole piece, then placing a diaphragm on the lithium-embedded graphite pole piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte onto the diaphragm, placing a lithium titanate pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the lithium titanate pole piece, finally placing a positive electrode shell, and sealing by using an electric sealing machine to obtain a secondary button type full cell.
Furthermore, the content of water and oxygen in the glove box is less than or equal to 0.1 ppm.
The invention also aims to provide a button full cell prepared by the preparation method of the button full cell composed of the lithium titanate pole piece and the graphite pole piece.
The invention has the beneficial effects that: firstly, preparing a graphite pole piece and a metal lithium piece into a button type full cell, taking the graphite pole piece as a negative electrode and the metal lithium piece as a positive electrode, then carrying out discharge treatment on the button type full cell to ensure that the metal lithium piece provides lithium ions, and simultaneously embedding the lithium ions into the graphite pole piece to obtain a lithium-embedded graphite pole piece; and then, the lithium-embedded graphite pole piece and the lithium titanate pole piece are made into a button type full cell, the lithium-embedded graphite pole piece provides lithium ions for the lithium titanate pole piece, so that the button type full cell taking the lithium titanate pole piece as a positive pole piece and the graphite pole piece as a negative pole piece is obtained, and the button type full cell has the advantages of good safety and stability, excellent quick charging performance, long cycle life and good high temperature resistance.
Detailed Description
First, it should be noted that the features and advantages of the present invention, etc., will be specifically described below by way of examples, however, all the descriptions are for illustrative purposes only and should not be construed as limiting the present invention in any way.
In order to avoid repetition, the technical parameters of the related raw materials or the manufacturing method related in the embodiments are uniformly described, and are not described again in the embodiments:
the conductive agent is SP; the binder is an NMP solution of PVDF, and the mass fraction of the binder is 5%.
The capacity of the graphite pole piece is 1-2 times of that of the lithium titanate pole piece; the surface of the metal lithium sheet is polished by a polishing rod to be smooth and has no oxide layer.
The content of water and oxygen in the glove box is less than or equal to 0.1 ppm.
The button full cell composed of lithium titanate pole piece and graphite pole piece and the preparation method thereof according to the present invention are exemplified by the following examples.
Example 1
The preparation method of the button type full cell described in this embodiment includes the following steps:
preparing a lithium titanate pole piece: adding lithium titanate, a conductive agent and a binder solution into a beaker according to the weight ratio of 80:10:10, and adding NMP to obtain 5g of a mixed solution, wherein the adding amount of the NMP is 5-10% of the total mass of the lithium titanate, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 2000r/min for 8 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking for 60min at the temperature of 90 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.1g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a lithium titanate pole piece with the diameter of 10mm, and carrying out vacuum drying on the lithium titanate pole piece for 24 hours at the temperature of 80 ℃.
Preparing a graphite pole piece: putting graphite, a conductive agent and a binder into a beaker according to the weight ratio of 93:2:5, and adding NMP to obtain 5g of mixed solution, wherein the adding amount of the NMP is 15 percent of the total mass of the graphite, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 2000r/min for 10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking for 60min at the temperature of 90 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.53g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a graphite pole piece with the diameter of 12mm, and carrying out vacuum drying on the graphite pole piece for 24 hours at the temperature of 120 ℃.
Placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a metal lithium sheet on the stainless steel gasket, dropwise adding electrolyte on the metal lithium sheet, then placing a diaphragm on the metal lithium sheet electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a graphite pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the graphite pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a first button type full cell, then placing the first button type full cell on a test cabinet, and discharging for 12 hours by using test software.
Disassembling the button type full battery I, and taking out the graphite pole piece by using a rubber head forceps to serve as a lithium-embedded graphite pole piece; placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a lithium-embedded graphite pole piece on the stainless steel gasket, dropwise adding electrolyte on the lithium-embedded graphite pole piece, then placing a diaphragm on the lithium-embedded graphite pole piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a lithium titanate pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the lithium titanate pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a secondary button type full cell, and standing the secondary button type full cell for 2h to obtain a finished product of the secondary button type full cell.
The obtained button full-cell finished product is subjected to constant-current charge and discharge tests, the 0.5C discharge capacity is 148.3mAh/g, the 1C discharge capacity is 144.7mAh/g, the 3C discharge capacity is 140.1mAh/g, and the battery rate performance is good.
Example 2
The preparation method of the button type full cell described in this embodiment includes the following steps:
preparing a lithium titanate pole piece: adding lithium titanate, a conductive agent and a binder solution into a beaker according to the weight ratio of 83:7:10, and adding NMP to obtain 6g of a mixed solution, wherein the adding amount of the NMP is 10% of the total mass of the lithium titanate, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 2000r/min for 10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking at 100 ℃ for 70 min; rolling the dried pole piece by using an electric roller press until the compaction density is 1.2g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a lithium titanate pole piece with the diameter of 11mm, and carrying out vacuum drying on the lithium titanate pole piece for 36h at the temperature of 100 ℃.
Preparing a graphite pole piece: putting graphite, a conductive agent and a binder into a beaker according to the weight ratio of 95:2:3, and adding NMP to obtain 6g of mixed solution, wherein the adding amount of the NMP is 18 percent of the total mass of the graphite, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 2000r/min for 10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking for 80min at the temperature of 90 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.65g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a graphite pole piece with the diameter of 13mm, and carrying out vacuum drying on the graphite pole piece for 36h at the temperature of 130 ℃.
Placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a metal lithium sheet on the stainless steel gasket, dropwise adding electrolyte on the metal lithium sheet, then placing a diaphragm on the metal lithium sheet electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a graphite pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the graphite pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a first button type full cell, then placing the first button type full cell on a test cabinet, and performing discharge treatment for 14h by using test software.
Disassembling the button type full battery I, and taking out the graphite pole piece by using a rubber head forceps to serve as a lithium-embedded graphite pole piece; placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a lithium-embedded graphite pole piece on the stainless steel gasket, dropwise adding electrolyte on the lithium-embedded graphite pole piece, then placing a diaphragm on the lithium-embedded graphite pole piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a lithium titanate pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the lithium titanate pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a secondary button type full cell, and standing the secondary button type full cell for 24 hours to obtain a finished product of the secondary button type full cell.
Constant-current charge and discharge tests are carried out on the obtained full button cell finished product, the 0.5C discharge capacity is 149.2mAh/g, the 1C discharge capacity is 145.2mAh/g, the 3C discharge capacity is 140.8mAh/g, and the battery rate performance is good.
Example 3
The preparation method of the button type full cell described in this embodiment includes the following steps:
preparing a lithium titanate pole piece: adding lithium titanate, a conductive agent and a binder solution into a beaker according to the weight ratio of 82:8:10, and adding NMP to obtain 5g of a mixed solution, wherein the adding amount of the NMP is 8% of the total mass of the lithium titanate, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500r/min for 10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking for 80min at the temperature of 80 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.3g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a lithium titanate pole piece with the diameter of 12mm, and carrying out vacuum drying on the lithium titanate pole piece for 48 hours at the temperature of 100 ℃.
Preparing a graphite pole piece: putting graphite, a conductive agent and a binder into a beaker according to the weight ratio of 92:1.5:6.5, and adding NMP to obtain 5g of mixed solution, wherein the adding amount of the NMP is 18 percent of the total mass of the graphite, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500r/min for 10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; placing the coated copper foil into an oven, and baking for 80min at the temperature of 100 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.65g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a graphite pole piece with the diameter of 14mm, and carrying out vacuum drying on the graphite pole piece for 48h at the temperature of 130 ℃.
Placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a metal lithium sheet on the stainless steel gasket, dropwise adding electrolyte on the metal lithium sheet, then placing a diaphragm on the metal lithium sheet electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a graphite pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the graphite pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a first button type full cell, then placing the first button type full cell on a test cabinet, and performing discharge treatment for 14h by using test software.
Disassembling the button type full battery I, and taking out the graphite pole piece by using a rubber head forceps to serve as a lithium-embedded graphite pole piece; placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a lithium-embedded graphite pole piece on the stainless steel gasket, dropwise adding electrolyte on the lithium-embedded graphite pole piece, then placing a diaphragm on the lithium-embedded graphite pole piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing a lithium titanate pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the lithium titanate pole piece, finally placing a positive electrode shell, sealing by using an electric sealing machine to obtain a secondary button type full cell, and standing the secondary button type full cell for 24 hours to obtain a finished product of the secondary button type full cell.
The obtained button full-cell finished product is subjected to constant-current charge and discharge tests, the 0.5C discharge capacity is 150.1mAh/g, the 1C discharge capacity is 145.8mAh/g, the 3C discharge capacity is 142.0mAh/g, and the battery rate performance is good.
Claims (9)
1. A preparation method of a button type full cell composed of a lithium titanate pole piece and a graphite pole piece is characterized by comprising the following steps:
(1) preparing a lithium titanate pole piece and a graphite pole piece, and then carrying out vacuum drying on the lithium titanate pole piece and the graphite pole piece to prepare a metal lithium piece;
(2) the preparation method comprises the following steps of taking a graphite pole piece as a positive pole piece and a metal lithium piece as a negative pole piece, and assembling a button type full cell I in a glove box, wherein the specific preparation process comprises the steps of placing a negative pole shell on a platform in the glove box, then placing a stainless steel gasket in the negative pole shell, placing the metal lithium piece on the stainless steel gasket, dropwise adding electrolyte on the metal lithium piece, then placing a diaphragm on the metal lithium piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte on the diaphragm, placing the graphite pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the graphite pole piece, finally placing a positive pole shell, and sealing by using an electric sealing machine to obtain the button type full cell I; then placing the button type full cell I on a test cabinet, and carrying out discharge treatment for 12-14 h by using test software;
(3) placing the discharged button type full battery I into a glove box, disassembling the button type full battery I to obtain a lithium-embedded graphite pole piece, and then assembling a button type full battery II in the glove box by taking the lithium-embedded graphite pole piece as a negative pole piece and taking a lithium titanate pole piece as a positive pole piece;
(4) and standing the button full cell II for 2-24 h to obtain a button full cell finished product.
2. The method for preparing a button type full cell composed of a lithium titanate pole piece and a graphite pole piece according to claim 1, wherein the preparation process of the lithium titanate pole piece in the step (1) is as follows: adding lithium titanate, a conductive agent and a binder solution into a beaker according to the weight ratio of (80-83) to (8-10) to (7-12), and adding NMP to obtain a mixed solution, wherein the adding amount of the NMP is 5-10% of the total mass of the lithium titanate, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500-2000 r/min for 5-10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; putting the coated copper foil into an oven, and baking for 60-80 min at the temperature of 80-100 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.1-1.3 g/cm 3; and punching the rolled pole piece by using a punching machine to obtain a lithium titanate pole piece with the diameter of 10-12 mm.
3. The method for preparing a button type full cell composed of a lithium titanate pole piece and a graphite pole piece according to claim 1, wherein the preparation process of the graphite pole piece in the step (1) is as follows: putting graphite, a conductive agent and a binder into a beaker according to the weight ratio of (92-95): (1.5-2.5): 2.5-6.5), and adding an NMP mixed solution, wherein the adding amount of the NMP is 10-20% of the total mass of the graphite, the conductive agent and the binder; putting the beaker into a high-speed dispersion machine, and rotating at a high speed of 1500-2000 r/min for 5-10 min; uniformly coating the uniformly mixed solution on a copper foil by using an automatic coating machine; putting the coated copper foil into an oven, and baking for 60-80 min at the temperature of 80-100 ℃; rolling the dried pole piece by using an electric roller press until the compaction density is 1.45-1.65g/cm 3; and punching the rolled pole piece by using a punching machine to obtain the graphite pole piece with the diameter of 12-14 mm.
4. The preparation method of the button type full cell composed of the lithium titanate pole piece and the graphite pole piece according to the claim 2 or 3 is characterized in that: the conductive agent is SP; the binder is an NMP solution of PVDF, and the mass fraction of the binder is 5%.
5. The preparation method of a button type full cell composed of a lithium titanate pole piece and a graphite pole piece according to claim 1, characterized in that in the step (1): the lithium titanate pole piece is dried in vacuum for 8-48 h at the temperature of 80-100 ℃, and the graphite pole piece is dried in vacuum for 8-48 h at the temperature of 110-130 ℃.
6. The preparation method of a button type full cell composed of a lithium titanate pole piece and a graphite pole piece according to claim 1, characterized in that in the step (1): the capacity of the graphite pole piece is 1-2 times of that of the lithium titanate pole piece; the surface of the metal lithium sheet is polished by a polishing rod to be smooth and has no oxide layer.
7. The preparation method of the button full cell composed of the lithium titanate pole piece and the graphite pole piece according to claim 1, characterized in that the preparation process of the second button full cell in the step (4): disassembling the button type full battery I, and taking out the graphite pole piece by using a rubber head forceps to serve as a lithium-embedded graphite pole piece; placing a negative electrode shell on a platform in a glove box, then placing a stainless steel gasket in the negative electrode shell, placing a lithium-embedded graphite pole piece on the stainless steel gasket, dropwise adding electrolyte into the lithium-embedded graphite pole piece, then placing a diaphragm on the lithium-embedded graphite pole piece electrolyte, ensuring that the middle part of the diaphragm is fully wetted, dropwise adding electrolyte onto the diaphragm, placing a lithium titanate pole piece on the electrolyte on the diaphragm, placing the stainless steel gasket on the lithium titanate pole piece, finally placing a positive electrode shell, and sealing by using an electric sealing machine to obtain a secondary button type full cell.
8. The preparation method of the button type full cell composed of the lithium titanate pole piece and the graphite pole piece according to claim 1 or 7, characterized in that: the content of water and oxygen in the glove box is less than or equal to 0.1 ppm.
9. A button full cell prepared by the preparation method of the button full cell composed of the lithium titanate pole piece and the graphite pole piece as claimed in claims 1-8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810878961.0A CN108807845B (en) | 2018-08-03 | 2018-08-03 | Button type full cell composed of lithium titanate pole piece and graphite pole piece and preparation method thereof |
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| CN201810878961.0A CN108807845B (en) | 2018-08-03 | 2018-08-03 | Button type full cell composed of lithium titanate pole piece and graphite pole piece and preparation method thereof |
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| CN108807845A CN108807845A (en) | 2018-11-13 |
| CN108807845B true 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 |
| CN114361378B (en) * | 2021-12-14 | 2024-03-29 | 宁德厦钨新能源材料有限公司 | Electrochemical performance detection method for 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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| 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 |
| 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 |
| CN207651591U (en) * | 2018-01-15 | 2018-07-24 | 张汉军 | A kind of low pressure lithium ion battery |
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