CN116014259A - Gel lithium ion battery and preparation method thereof - Google Patents
Gel lithium ion battery and preparation method thereof Download PDFInfo
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- CN116014259A CN116014259A CN202310310761.6A CN202310310761A CN116014259A CN 116014259 A CN116014259 A CN 116014259A CN 202310310761 A CN202310310761 A CN 202310310761A CN 116014259 A CN116014259 A CN 116014259A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000003792 electrolyte Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 238000004806 packaging method and process Methods 0.000 claims description 22
- 238000005086 pumping Methods 0.000 claims description 17
- 239000003999 initiator Substances 0.000 claims description 13
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 12
- 239000011244 liquid electrolyte Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical group CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 6
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 2
- 238000001764 infiltration Methods 0.000 claims description 2
- 238000012797 qualification Methods 0.000 claims description 2
- 238000009461 vacuum packaging Methods 0.000 claims description 2
- 238000009423 ventilation Methods 0.000 claims description 2
- 230000000284 resting effect Effects 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000006978 adaptation Effects 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001688 coating polymer Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a gel lithium ion battery and a preparation method thereof. Through the procedures of shelving, formation, air extraction and the like, a series of gas compounds generated by shelving and charging in the battery are removed; electrolyte filled with gel monomer is permeated and placed, then the air bag is punctured, and then the gel is formed under vacuum state, so that the gas produced in the gel forming process can be effectively removed, and the gel formed in the battery is uniform, no bubble remains, and the battery multiplying power performance is good.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a gel lithium ion battery and a preparation method thereof.
Background
With the deep use of lithium ion batteries in people's life, the safety of lithium ion batteries is also becoming more and more important. Most of lithium ion batteries used in commercialization are liquid, and because of hidden dangers such as liquid leakage and inflammability, research and development of safer lithium ion battery systems are urgently needed.
Gel lithium ion batteries have no fluidity because of the colloidal state of the internal electrolyte, and the risk of liquid leakage does not occur, so that more and more researches of universities and enterprises are caused. CN 101662041B coats prepared P (VDF-HFP) -TiO2 onto the pole piece. Under the heating condition, the composite porous membrane formed on the pole piece and the liquid electrolyte form gel, and then the gel battery is prepared by pre-fully containing the gel. CN 102306841a is prepared by adding monomer and thermal initiator into slurry, coating polymer glue solution containing cross-linking agent on the membrane, thermal polymerizing at a certain temperature, pre-pumping air to separate volume, and forming gel battery. Both methods are to perform thermal polymerization and pre-charge air extraction to form a gel battery, but the problem of gas production in formation of the battery after gel formation is ignored, the surface of a pole piece is wrapped by a gel layer after gel formation, and the gas produced in formation is difficult to completely remove, so that the electrical performance of the battery is affected.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a gel lithium ion battery. The method is an in-situ polymerization method. The battery is firstly formed and charged after the stock solution is injected, then the battery is pumped, and then electrolyte filled with gel monomer is filled, and finally the battery is formed into gel under certain conditions. Through the procedures of shelving, formation, air extraction and the like, a series of gas compounds generated by shelving and charging in the battery are removed; electrolyte filled with gel monomer is permeated and placed, then the air bag is punctured, and then the gel is formed under vacuum state, so that the gas produced in the gel forming process can be effectively removed, and the gel formed in the battery is uniform, no bubble remains, and the battery multiplying power performance is good.
The invention provides a preparation method of a gel lithium ion battery, which comprises the following steps:
(1) Placing the assembled qualified battery cells in a vacuum oven for baking;
(2) After baking, measuring the moisture of the pole piece in a dew point room, and injecting liquid electrolyte into the battery cell after the moisture is qualified;
(3) Vacuum seepage is carried out on the cell after liquid injection, packaging is carried out, and then the cell is placed; when the vacuum seepage is carried out, the vacuum is-80 KPa to-99 KPa, the time is 1min-3min, and the seepage times are 1-2 times; an air bag is reserved during packaging, and the size of the air bag is 40-80 mm; the battery has a shelf temperature of 35-45 ℃ and a shelf time of 12-36 h after packaging;
(4) Heating and pressurizing the placed battery to form;
(5) After the formation is finished, the battery is high Wen Gezhi;
(6) Vacuum pumping is carried out on the battery after the rest;
(7) Filling electrolyte into the battery, and then carrying out vacuum infiltration, packaging and placing; wherein the filling electrolyte comprises liquid electrolyte, gel monomer and initiator; when the vacuum seepage is carried out, the vacuum is-80 KPa to-99 KPa, the time is 1min-3min, and the seepage times are 1-2 times; an air bag is reserved during packaging, and the size of the air bag is 40-80 mm; the temperature of the packaged battery is 25-35 ℃ and the time is 24-48 hours;
(8) After the rest is finished, the battery is transferred to a dew point room; clamping the battery by using a clamping plate, placing the battery on a platform, keeping the battery air bag and the battery main body flat, and then puncturing the air bag by using a multi-needle plate; wherein the diameter of the puncture needle is 1mm-2mm, the number of the needles is not less than 3, the needling position is 20mm-40mm away from the air bag, and the air bag is provided with small air holes which are uniformly arranged after needling;
(9) Placing the battery with the clamping plate in an oven, and heating to glue; wherein the temperature of the oven is 60-80 ℃, the vacuum is-60 KPa to-90 KPa, and the time is 10-16 h;
(10) Transferring the glued battery to vacuum packaging equipment for vacuum pumping packaging, and then separating the capacity to finish battery manufacturing.
Further, in the step (1), the baking temperature of the battery cell is 75-85 ℃, the baking time is 36-72 h, and ventilation is performed every 2h in the baking process.
Further, in the step (2), the moisture qualification means: the moisture of the positive electrode sheet is less than 50ppm, and the moisture of the negative electrode sheet is less than 100 ppm.
Further, in the step (4), the heating temperature is 30-45 ℃, the pressure is determined according to the thickness of the battery, the charging current is 0.01-0.1C during formation, and the battery is charged to the upper limit voltage of the battery. The current in the process step is required to be small, so that the gas-generating side reaction in the battery can fully occur.
Further, in the step (5), the rest temperature is 35-45 ℃ and the rest time is 24-48 h.
Further, in the step (6), the vacuum is-80 KPa to-99 KPa, the time is 3S-10S, and the extraction amount of the electrolyte is required to be less than 5% of the injection amount.
Further, in the step (7), the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide.
The invention also provides a gel lithium ion battery which is prepared by adopting the method.
The invention has the beneficial effects that:
1. and (5) performing formation, charging and then forming glue. In the formation process, partial additives of the electrolyte are reduced on the pole piece preferentially, so that the reduction of partial gel monomers in the process of adding the electrolyte for the second time can be reduced, and the gel formation performance of the electrolyte is poor; on the other hand, the side reaction of the battery after formation fully occurs, and then the gas is pumped out, so that the gas in the battery can be eliminated, and the gas in the battery is not easy to be pumped out after the formation of the gel.
2. Before the glue is formed, the air bags are uniformly punctured at a certain position away from the battery main body, and then the baking oven is placed for negative pressure glue forming. The gas generated in the gelling process can be uniformly extracted, the gas generated in the gelling process is effectively removed, the gelling of the pole piece is more uniform, and the battery performance is better.
Drawings
Fig. 1 is an SEM image of a positive electrode sheet of the battery manufactured in example 1;
fig. 2 is an SEM image of the positive electrode sheet of the battery manufactured in comparative example.
Detailed Description
The present invention will be described in detail with reference to examples and comparative examples
Example 1
Taking a soft-pack high-nickel 10Ah battery as an example, the thickness of the battery is 6mm. The positive electrode is made of high nickel material, the negative electrode is made of artificial graphite, and the electrolyte is positive electrode adaptation electrolyte.
1. After the moisture of the pole piece is tested to be qualified, 50g of liquid electrolyte is injected, the liquid is permeated for 1min under the vacuum of-80 KPa for 1 time, then the pole piece is packaged, and then the pole piece is placed at 40 ℃ for 24 hours;
2. heating and pressurizing to form. Charging 0.1C to the upper limit voltage of 4.35V at 40 ℃ under 800kg pressure;
3. and (5) placing the qualified battery at 40 ℃ for 24 hours, and then pumping. Pumping for 5S under the pressure of 90KPa, and pumping out 1.5 g+/-0.5 g of electrolyte;
4. filling liquid electrolyte, gel monomer and initiator into dew point room, wherein the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide. Percolating under-85 KPa vacuum for 2min for 1 time, packaging, and standing at 25deg.C for 48 hr;
5. the air bag is punctured by a needling plate in a dew point room, and the air bag is firstly placed at 70 ℃ for 2 hours under-60 KPa, then the vacuum is adjusted to be-80 KPa, and is placed at 70 ℃ for 10 hours;
6. and after the gel forming is finished, taking out the battery, packaging under vacuum, and then separating the capacity.
Example 2
Taking a soft-pack high-nickel 10Ah battery as an example, the thickness of the battery is 6mm. The positive electrode is made of high nickel material, the negative electrode is made of artificial graphite, and the electrolyte is positive electrode adaptation electrolyte.
1. After the moisture of the pole piece is tested to be qualified, 50g of liquid electrolyte is injected, the liquid is permeated for 1min under the vacuum of-80 KPa for 1 time, then the pole piece is packaged, and then the pole piece is placed at 40 ℃ for 24 hours;
2. heating and pressurizing to form. Charging 0.1C to the upper limit voltage of 4.35V at 40 ℃ under 800kg pressure;
3. and (5) placing the qualified battery at 40 ℃ for 24 hours, and then pumping. Pumping for 5S under the pressure of 90KPa, and pumping out 1.5 g+/-0.5 g of electrolyte;
4. filling liquid electrolyte, gel monomer and initiator into dew point room, wherein the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide. Percolating under vacuum of-80 KPa for 3min for 1 time, packaging, and standing at 35deg.C for 24 hr;
5. the air bag is punctured by a needling plate in a dew point room, the air bag is firstly placed at 60 ℃ for 4 hours under-60 KPa, then the vacuum is adjusted to be-80 KPa, and the air bag is placed at 60 ℃ for 12 hours;
6. and after the gel forming is finished, taking out the battery, packaging under vacuum, and then separating the capacity.
Example 3
Taking a soft-pack high-nickel 10Ah battery as an example, the thickness of the battery is 6mm. The positive electrode is made of high nickel material, the negative electrode is made of artificial graphite, and the electrolyte is positive electrode adaptation electrolyte.
1. After the moisture of the pole piece is tested to be qualified, 50g of liquid electrolyte is injected, the liquid is permeated for 1min under the vacuum of-80 KPa for 1 time, then the pole piece is packaged, and then the pole piece is placed at 40 ℃ for 24 hours;
2. heating and pressurizing to form. Charging 0.1C to the upper limit voltage of 4.35V at 40 ℃ under 800kg pressure;
3. and (5) placing the qualified battery at 40 ℃ for 24 hours, and then pumping. Pumping for 5S under the pressure of 90KPa, and pumping out 1.5 g+/-0.5 g of electrolyte;
4. filling liquid electrolyte, gel monomer and initiator into dew point room, wherein the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide. Percolating under vacuum of-90 KPa for 1min for 1 time, packaging, and standing at 35deg.C for 24 hr;
5. the air bag is punctured by a needling plate in a dew point room, and the air bag is firstly placed at 80 ℃ for 1h under-70 KPa, then the vacuum is adjusted to be-90 KPa, and is placed at 80 ℃ for 9h;
6. and after the gel forming is finished, taking out the battery, packaging under vacuum, and then separating the capacity.
Comparative example
1. After the moisture of the pole piece is tested to be qualified, liquid electrolyte, gel monomer and initiator are injected, wherein the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide. Seepage is carried out for 1min under the vacuum of-80 KPa, seepage is carried out for 1 time, then packaging is carried out, and then the packaging is carried out for 48h at 35 ℃;
2. and (5) vacuum pumping. -extracting air for 5S under 95KPa, wherein the packaging temperature is 180 ℃/4S;
3. puncturing an air bag in a dew point room, firstly placing at 70 ℃ for 2 hours under-60 KPa, then adjusting the vacuum to-80 KPa, and continuously placing at 70 ℃ for 10 hours;
4. and (5) vacuum pumping. -air extraction is carried out for 15S under the pressure of 95KPa, and the packaging temperature is 180 ℃/4S;
5. heating and pressurizing to form. Charging 0.1C to the upper limit voltage of 4.35V at 40 ℃ under 800kg pressure;
6. and (5) pumping the qualified battery cabinet, and then separating the capacity.
The battery of example 1 and comparative example were disassembled, and both the pole piece and the separator had a glue layer. SEM was performed on the positive electrode sheet, as shown in the following figure:
the pole pieces of the example 1 positive pole SEM image 1 and the comparative example positive pole SEM image 2 are wrapped by the glue layer, but the glue layer of the comparative example pole piece is thicker, the glue layer is unevenly distributed, and the glue layer of the example 1 is slightly thinner, and the glue layer is evenly distributed.
The rate performance of the comparative cells is shown in the following table:
the comparative example was lower in both rate charge and rate discharge performance than the examples, and was associated with a thicker gel layer and non-uniformity in gel formation that could not be eliminated by the gas inside the cell.
Claims (8)
1. The preparation method of the gel lithium ion battery is characterized by comprising the following steps of:
(1) Placing the assembled qualified battery cells in a vacuum oven for baking;
(2) After baking, measuring the moisture of the pole piece in a dew point room, and injecting liquid electrolyte into the battery cell after the moisture is qualified;
(3) Vacuum seepage is carried out on the cell after liquid injection, packaging is carried out, and then the cell is placed; when the vacuum seepage is carried out, the vacuum is-80 KPa to-99 KPa, the time is 1min-3min, and the seepage times are 1-2 times; an air bag is reserved during packaging, and the size of the air bag is 40-80 mm; the battery has a shelf temperature of 35-45 ℃ and a shelf time of 12-36 h after packaging;
(4) Heating and pressurizing the placed battery to form;
(5) After the formation is finished, the battery is high Wen Gezhi;
(6) Vacuum pumping is carried out on the battery after the rest;
(7) Filling electrolyte into the battery, and then carrying out vacuum infiltration, packaging and placing; wherein the filling electrolyte comprises liquid electrolyte, gel monomer and initiator; when the vacuum seepage is carried out, the vacuum is-80 KPa to-99 KPa, the time is 1min-3min, and the seepage times are 1-2 times; an air bag is reserved during packaging, and the size of the air bag is 40-80 mm; the temperature of the packaged battery is 25-35 ℃ and the time is 24-48 hours;
(8) After the rest is finished, the battery is transferred to a dew point room; clamping the battery by using a clamping plate, placing the battery on a platform, keeping the battery air bag and the battery main body flat, and then puncturing the air bag by using a multi-needle plate; wherein the diameter of the puncture needle is 1mm-2mm, the number of the needles is not less than 3, the needling position is 20mm-40mm away from the air bag, and the air bag is provided with small air holes which are uniformly arranged after needling;
(9) Placing the battery with the clamping plate in an oven, and heating to glue; wherein the temperature of the oven is 60-80 ℃, the vacuum is-60 KPa to-90 KPa, and the time is 10-16 h;
(10) Transferring the glued battery to vacuum packaging equipment for vacuum pumping packaging, and then separating the capacity to finish battery manufacturing.
2. The method of claim 1, wherein in the step (1), the baking temperature of the battery cell is 75-85 ℃ and the baking time is 36-72 h, and ventilation is performed every 2h in the baking process.
3. The method for preparing a gel lithium ion battery according to claim 1, wherein in the step (2), the moisture qualification means: the moisture of the positive electrode sheet is less than 50ppm, and the moisture of the negative electrode sheet is less than 100 ppm.
4. The method of claim 1, wherein the heating temperature is 30-45 ℃, the pressure is determined according to the thickness of the battery, the charging current is 0.01-0.1C when the battery is formed, and the battery is charged to the upper limit voltage of the battery in the step (4).
5. The method for preparing a gel lithium ion battery according to claim 1, wherein in the step (5), the resting temperature is 35-45 ℃ and the resting time is 24-48 h.
6. The method of claim 1, wherein in the step (6), the vacuum is-80 KPa to-99 KPa, the time is 3S-10S, and the extraction amount of the electrolyte is less than 5% of the injection amount.
7. The method of claim 1, wherein in step (7), the gel monomer is pentaerythritol tetraacrylate or tripropylene glycol diacrylate; the initiator is azobisisobutyronitrile or dibenzoyl peroxide.
8. A gel lithium ion battery prepared by the method of any one of claims 1 to 7.
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