CN112563454A - Method for pre-lithiation of negative pole piece - Google Patents
Method for pre-lithiation of negative pole piece Download PDFInfo
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- CN112563454A CN112563454A CN202011442831.6A CN202011442831A CN112563454A CN 112563454 A CN112563454 A CN 112563454A CN 202011442831 A CN202011442831 A CN 202011442831A CN 112563454 A CN112563454 A CN 112563454A
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- pole piece
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000006138 lithiation reaction Methods 0.000 title claims abstract description 36
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 20
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000011888 foil Substances 0.000 claims abstract description 10
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 23
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 9
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 8
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- -1 aromatic hydrocarbon lithium salt Chemical class 0.000 claims description 5
- 229910003002 lithium salt Inorganic materials 0.000 claims description 5
- 235000010290 biphenyl Nutrition 0.000 claims description 4
- 239000004305 biphenyl Substances 0.000 claims description 4
- 229910021385 hard carbon Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- GBVSONMCEKNESD-UHFFFAOYSA-N 1,1'-biphenyl;lithium Chemical group [Li].C1=CC=CC=C1C1=CC=CC=C1 GBVSONMCEKNESD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002210 silicon-based material Substances 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 239000007773 negative electrode material Substances 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- 239000007784 solid electrolyte Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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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
- H01M4/139—Processes of manufacture
-
- 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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
- H01M10/446—Initial charging measures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for pre-lithiation of a negative pole piece, which comprises the steps of dissolving an aromatic hydrocarbon organic matter in an ether organic matter solvent to obtain a pre-lithiation precursor solution, then taking the negative pole piece as a working electrode and a lithium foil as a counter electrode, and carrying out discharging pre-lithiation in the pre-lithiation precursor solution by a constant current and constant voltage method. And after the constant-current constant-voltage discharge is finished, taking out the pole piece and drying the pole piece to obtain the pre-lithiated negative pole piece. The method has the advantages of simple process and capability of greatly improving the pre-lithiation effect of the negative pole piece.
Description
Technical Field
The invention relates to the field of lithium ion battery prelithiation, in particular to a method for prelithiation of a negative pole piece.
Background
In the first charge-discharge cycle of the lithium ion battery, a solid electrolyte membrane is generated on the surface of a negative electrode material, so that a large amount of lithium ions are consumed, and the capacity of the battery is greatly attenuated. Therefore, attention is paid to how to reduce the loss of lithium ions during the first charge and discharge of the battery negative electrode material. The pre-lithiation of the negative electrode material can enable the material to generate a solid electrolyte membrane or be embedded with lithium in advance before the first charge and discharge, so that the loss of lithium ions during the first charge and discharge is reduced, and the first charge and discharge efficiency is improved. However, in the prelithiation process, the conductive performance of the electrode surface is greatly reduced due to the formation of a solid electrolyte membrane, which further affects the charge and discharge effects of the lithium ion battery.
Disclosure of Invention
In order to avoid reducing the charging and discharging efficiency of the battery due to the generation of the solid electrolyte membrane, the invention aims to provide the method for pre-lithiating the negative pole piece, which has simple process and can improve the pre-lithiation effect of the negative pole piece.
The invention aims to provide the following scheme for realizing: a method for the prelithiation of a negative pole piece is disclosed, wherein aromatic hydrocarbon organic matters are dissolved in an ether organic solvent to obtain a prelithiation precursor solution, then the negative pole piece is used as a working electrode, a lithium foil is used as a counter electrode, the prelithiation is carried out in the prelithiation precursor solution by a constant current and constant voltage method, after the constant current and constant voltage discharge is finished, the pole piece is taken out and dried to obtain the prelithiation negative pole piece, and the method comprises the following steps:
the method comprises the following steps: dissolving aromatic hydrocarbon organic matters in an ether organic solvent to obtain a pre-lithiation precursor solution, wherein the concentration of the solution is 0.5M;
step two: putting the negative pole piece serving as a working electrode and the lithium foil serving as a counter electrode into the pre-lithiation precursor solution to obtain an aromatic hydrocarbon lithium salt solution;
step three: the negative pole piece is subjected to discharging pre-lithiation by a constant current and constant voltage method, wherein the constant current and constant voltage method is 0.1-0.01C, and the voltage is 0.3-0.5V (vs Li/Li)+）；
Step four: and drying the negative pole piece after the constant-current constant-voltage discharge is finished to obtain the pre-lithiated negative pole piece.
On the basis of the scheme, in the step one, the aromatic hydrocarbon organic matters are benzene, naphthalene, biphenyl and derivatives thereof; the ether organic solvent is one or two of tetrahydrofuran and ethylene glycol dimethyl ether.
Preferably, the aromatic hydrocarbon lithium salt is lithium biphenyl and its derivatives.
Preferably, the ether organic solvent is ethylene glycol dimethyl ether.
On the basis of the scheme, in the second step, the negative pole piece is made of one or more of silicon-based materials, hard carbon materials and graphite according to a conventional negative pole piece manufacturing method.
On the basis of the scheme, in the fourth step, the drying temperature is 40-90 ℃. Preferably, the drying temperature is 80 ℃.
Preferably, the constant voltage and the constant current have a current of 0.05C and a voltage of 0.45V.
The invention can effectively avoid the reduction of the charging and discharging efficiency of the battery due to the generation of the solid electrolyte membrane, has simple process and can greatly improve the pre-lithiation effect of the negative pole piece.
Drawings
FIG. 1 is a first charge-discharge curve of a half-cell of a pre-lithiated silicon negative electrode material prepared by the preparation method of the invention.
Detailed Description
Example 1:
a method for pre-lithiation of a negative pole piece is characterized in that aromatic hydrocarbon organic matters are dissolved in an ether organic solvent to obtain a pre-lithiation precursor solution, then the negative pole piece is used as a working electrode, a lithium foil is used as a counter electrode, discharging pre-lithiation is carried out in the pre-lithiation precursor solution by a constant current and constant voltage method, after constant current and constant voltage discharging is finished, the pole piece is taken out and dried to obtain the pre-lithiation negative pole piece, and the method comprises the following steps:
the method comprises the following steps: dissolving biphenyl in an ethylene glycol dimethyl ether solvent to obtain a pre-lithiation precursor solution, wherein the concentration of the solution is 0.5M;
step two: putting the negative pole piece serving as a working electrode and the lithium foil serving as a counter electrode into the pre-lithiation precursor solution to obtain an aromatic hydrocarbon lithium salt solution;
step three: the negative pole piece is subjected to discharging pre-lithiation by a constant current and constant voltage method, wherein the constant current and constant voltage method is 0.05C, and the voltage is 0.4V (vs Li/Li)+）；
Step four: and taking out the negative pole piece after the constant-current constant-voltage discharge is finished, and drying in vacuum at 80 ℃ to obtain the pre-lithiated negative pole piece.
Fig. 1 is a first charge-discharge curve diagram of a half-cell (a button cell is adopted as the half-cell, a lithium sheet is used as a counter electrode, and a conventional lithium battery electrolyte is used as the electrolyte) made of the pre-lithiated silicon negative electrode material prepared in the embodiment. The first charge-discharge efficiency of the pre-lithiated silicon oxide negative electrode material prepared in the embodiment is 91%.
Example 2:
a method for pre-lithiation of a negative pole piece is similar to that in example 1, and comprises the following steps:
the method comprises the following steps: dissolving biphenyl in tetrahydrofuran solvent to obtain a pre-lithiation precursor solution, wherein the concentration of the solution is 0.5M;
step two: putting a silicon monoxide negative pole piece serving as a working electrode and a lithium foil serving as a counter electrode into a pre-lithiation precursor solution;
step three: pre-lithiation is carried out on a silicon oxide cathode by adopting a constant voltage and constant current method, wherein the current is 0.01C, and the voltage is 0.4V (vs Li/Li)+）；
Step four: and taking out the negative pole piece after the constant-voltage constant-current discharge is finished, and drying in vacuum at 60 ℃ to obtain the pre-lithiated negative pole piece.
Example 3:
a method for pre-lithiation of a negative pole piece is similar to that in example 1, and comprises the following steps:
the method comprises the following steps: dissolving naphthalene in an ethylene glycol dimethyl ether solvent to obtain a pre-lithiation precursor solution, wherein the concentration of the solution is 0.5M;
step two: putting a hard carbon negative pole piece serving as a working electrode and a lithium foil serving as a counter electrode into a pre-lithiation precursor solution;
step three: performing pre-lithiation on the hard carbon cathode by adopting a constant voltage and constant current method, wherein the current is 0.05C, and the voltage is 0.4V (vs Li/Li)+）；
Step four: and taking out the negative pole piece after the constant-voltage constant-current discharge is finished, and drying the negative pole piece in vacuum at the temperature of 80 ℃ to obtain the pre-lithiated negative pole piece.
Example 4:
a method for pre-lithiation of a negative pole piece is similar to that in example 1, and comprises the following steps:
the method comprises the following steps: dissolving naphthalene in tetrahydrofuran solvent to obtain pre-lithiation precursor solution with the concentration of 0.5M;
step two: putting a graphite negative pole piece serving as a working electrode and a lithium foil serving as a counter electrode into the pre-lithiation precursor solution;
step three: pre-lithiation is carried out on a silicon oxide cathode by adopting a constant voltage and constant current method, wherein the current is 0.01C, and the voltage is 0.4V (vs Li/Li)+）；
Step four: and taking out the negative pole piece after the constant-voltage constant-current discharge is finished, and drying the negative pole piece in vacuum at the temperature of 80 ℃ to obtain the pre-lithiated negative pole piece.
Claims (8)
1. A method for the prelithiation of a negative pole piece is characterized in that aromatic hydrocarbon organic matters are dissolved in an ether organic solvent to obtain a prelithiation precursor solution, then the negative pole piece is used as a working electrode, a lithium foil is used as a counter electrode, the prelithiation is carried out in the prelithiation precursor solution by a constant current and constant voltage method, after the constant current and constant voltage discharge is finished, the pole piece is taken out and dried to obtain the prelithiation negative pole piece, and the method comprises the following steps:
the method comprises the following steps: dissolving aromatic hydrocarbon organic matters in an ether organic solvent to obtain a pre-lithiation precursor solution, wherein the concentration of the solution is 0.5M;
step two: putting the negative pole piece serving as a working electrode and the lithium foil serving as a counter electrode into the pre-lithiation precursor solution to obtain an aromatic hydrocarbon lithium salt solution;
step three: the negative pole piece is subjected to discharging pre-lithiation by a constant current and constant voltage method, wherein the constant current and constant voltage method is 0.1-0.01C, and the voltage is 0.3-0.5V (vs Li/Li)+）；
Step four: and drying the negative pole piece after the constant-current constant-voltage discharge is finished to obtain the pre-lithiated negative pole piece.
2. The method for prelithiation of a negative electrode tab of claim 1, wherein: in the first step, the aromatic hydrocarbon organic matters are benzene, naphthalene, biphenyl and derivatives thereof; the ether organic solvent is one or two of tetrahydrofuran and ethylene glycol dimethyl ether.
3. The method for prelithiation of a negative electrode tab of claim 1, wherein: in the second step, the negative pole piece is made of one or more of silicon-based materials, hard carbon materials and graphite according to a conventional negative pole piece manufacturing method.
4. The method for prelithiation of a negative electrode tab of claim 1, wherein: in the fourth step, the drying temperature is 40-90 ℃.
5. The method for prelithiation of a negative electrode tab of claim 4, wherein: the drying temperature was 80 ℃.
6. The method for prelithiation of a negative electrode tab of claim 2, wherein: the aromatic hydrocarbon lithium salt is lithium biphenyl and its derivative.
7. The method for prelithiation of a negative electrode tab of claim 2, wherein: the ether organic solvent is ethylene glycol dimethyl ether.
8. The method for prelithiation of a negative electrode tab of claim 1, wherein: the constant voltage and constant current has a current of 0.05C and a voltage of 0.45V.
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| CN202011442831.6A CN112563454A (en) | 2020-12-11 | 2020-12-11 | Method for pre-lithiation of negative pole piece |
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| CN202011442831.6A CN112563454A (en) | 2020-12-11 | 2020-12-11 | Method for pre-lithiation of negative pole piece |
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Citations (8)
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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 |
| CN110120496A (en) * | 2018-02-05 | 2019-08-13 | 武汉大学 | A kind of negative electrode of lithium ion battery and its prelithiation methods and applications |
| WO2020009494A1 (en) * | 2018-07-06 | 2020-01-09 | 주식회사 엘지화학 | Negative electrode for lithium secondary battery, method for pre-lithiating same, and lithium secondary battery including same |
| WO2020085823A1 (en) * | 2018-10-26 | 2020-04-30 | 주식회사 엘지화학 | Method for manufacturing anode for lithium secondary battery |
| CN111261838A (en) * | 2020-03-25 | 2020-06-09 | 上海电气集团股份有限公司 | Method for pre-lithiation of silicon monoxide negative pole piece |
| CN111615769A (en) * | 2018-03-07 | 2020-09-01 | 株式会社Lg化学 | Method for manufacturing negative electrode |
| CN111886722A (en) * | 2019-01-31 | 2020-11-03 | 株式会社Lg化学 | Method for prelithiating negative electrode of secondary battery |
| CN112038583A (en) * | 2020-08-19 | 2020-12-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for prelithiation of silicon monoxide negative pole piece |
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2020
- 2020-12-11 CN CN202011442831.6A patent/CN112563454A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110120496A (en) * | 2018-02-05 | 2019-08-13 | 武汉大学 | A kind of negative electrode of lithium ion battery and its prelithiation methods and applications |
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| WO2020085823A1 (en) * | 2018-10-26 | 2020-04-30 | 주식회사 엘지화학 | Method for manufacturing anode for lithium secondary battery |
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| CN111261838A (en) * | 2020-03-25 | 2020-06-09 | 上海电气集团股份有限公司 | Method for pre-lithiation of silicon monoxide negative pole piece |
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Application publication date: 20210326 |