WO2018032322A1 - Procédé de fabrication d'électrode positive de condensateur lithium-ion - Google Patents
Procédé de fabrication d'électrode positive de condensateur lithium-ion Download PDFInfo
- Publication number
- WO2018032322A1 WO2018032322A1 PCT/CN2016/095454 CN2016095454W WO2018032322A1 WO 2018032322 A1 WO2018032322 A1 WO 2018032322A1 CN 2016095454 W CN2016095454 W CN 2016095454W WO 2018032322 A1 WO2018032322 A1 WO 2018032322A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- suspension
- electrode sheet
- positive electrode
- lithium ion
- muffle furnace
- Prior art date
Links
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 45
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 239000003990 capacitor Substances 0.000 title description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000725 suspension Substances 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000006260 foam Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract 2
- 238000000576 coating method Methods 0.000 claims abstract 2
- 239000003792 electrolyte Substances 0.000 claims description 14
- -1 polypropylene Polymers 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000004743 Polypropylene Substances 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims description 9
- 229920001155 polypropylene Polymers 0.000 claims description 9
- 229910021385 hard carbon Inorganic materials 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- 239000006258 conductive agent Substances 0.000 claims description 7
- 239000011889 copper foil Substances 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 4
- 229910010177 Li2MoO3 Inorganic materials 0.000 abstract 3
- 229920002239 polyacrylonitrile Polymers 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 16
- 229910052744 lithium Inorganic materials 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 229910013870 LiPF 6 Inorganic materials 0.000 description 6
- 239000007774 positive electrode material Substances 0.000 description 4
- 239000010406 cathode material Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- 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
- Y02E60/13—Energy storage using capacitors
Definitions
- the present invention belongs to the technical field of lithium ion supercapacitors, and in particular, to a method for preparing a lithium ion supercapacitor positive electrode sheet.
- the battery negative electrode generally uses a carbon material such as graphite
- the positive electrode uses a lithium-containing metal oxide such as lithium cobaltate or lithium manganate.
- the charged negative electrode supplies lithium ions to the positive electrode, and the lithium ion of the positive electrode of the discharge positive electrode returns to the negative electrode, so it is called a "rocking chair type battery".
- This battery is characterized by high safety and high cycle life compared to lithium batteries using metallic lithium.
- Lithium-ion capacitors generally use carbon materials such as graphite and hard carbon for the anode material, and activated carbon materials with double-layer characteristics for the cathode material, and the lithium anode is pre-diffused to the anode material, so that the potential of the anode is greatly reduced, thereby improving Energy Density.
- a lithium ion capacitor is disclosed in the special ljCN200580001498.2.
- the positive current collector and the negative current collector used in the lithium ion capacitor have holes penetrating the front and back surfaces, and the electrode layer is formed by the positive electrode active material and the negative electrode active material respectively. Electrochemical contact is made to the negative electrode, and lithium ions are carried in the negative electrode in advance.
- a pretreatment method for a negative electrode for an electrochemical capacitor is disclosed in the Japanese Patent Publication No. Hei. No. 1,200, 406, 9.6, a lithium layer is formed on a substrate by a vapor phase method or a liquid phase method, and then the lithium layer is transferred to an electrode layer of a negative electrode.
- These pre-excessive methods involve complex processes and require special handling of the raw materials, which makes the manufacturing process difficult.
- the technical problem to be solved by the present invention is to provide a method for preparing a positive electrode sheet for a lithium ion supercapacitor.
- the positive electrode sheet prepared by the method can replace the aluminum current collector and the positive active material, and can be provided in a lithium ion capacitor.
- Lithium source eliminating the need for complex pre-intercalation of lithium or lithium-ion capacitors
- the addition of lithium sheets in the device simplifies the process of preparing lithium ion capacitors and reduces the cost of the process.
- the preparation method of the lithium ion supercapacitor positive electrode sheet provided by the invention is:
- Step (1) Adding graphite oxide and polypropylene fine to a ball mill for 30-60 min, and then adding the ball-milled mixture to a mixed solution of ethanol and water to ultrasonically disperse to form a suspension having a concentration of l-20 g/L.
- Step (2) The nickel foam is soaked in the above suspension for 10-60 min, the solvent is evaporated, and then placed in a hydrogen-nitrogen mixed gas-protected muffle furnace at 800-1100 ° C for 1-10 h, after the reaction is completed. Naturally cooled.
- Step (3) The above product is immersed in l-3 mol/L hydrochloric acid, and reacted at 60-80 ° C for 5-10 h, and after completion of the reaction, foamed graphene is obtained.
- Step (4) The nano Li 2 MoO 3 is forced into toluene, sonicated for 10-30 min to form a suspension, and then Li 2 MoO 3 is contained.
- the toluene suspension droplets were applied to the foamed graphene, dried, and then placed in a muffle furnace and annealed at 200 ° C for 30-60 min. After cooling, the crucible was pressed to obtain an electrode sheet.
- the ball mill is 30-60 min;
- the mass of the polypropylene clear in the step (1) is 0.01-5% of the mass of the graphite oxide
- the volume ratio of ethanol to water in the mixed solution of ethanol and water in the step (1) is 0.25-4
- step (1) in the concentration of the graphite oxide suspension is l-20g / L of the suspension
- the foamed nickel is immersed in the graphite oxide suspension in the crucible is 10-60mi n;
- the atmosphere in the muffle furnace is a hydrogen-nitrogen mixed gas containing a volume concentration of 5% hydrogen;
- step (2) in the muffle furnace reaction temperature is 800-1100 ° C, the reaction time is 1- 10h;
- the concentration of hydrochloric acid in the step (3) is l-3mol / L;
- the reaction temperature of the step (3) in hydrochloric acid is 60-80 ° C, and the reaction time is 5-10 h ;
- the mass concentration of the Li 2 MoO 3 toluene suspension in the step (4) is 30-70%;
- the ultrasonic inter-turn is 10-30 min;
- the annealing temperature is 200-300 ° C, and the annealing time is 30-60 min;
- the electrode sheet obtained in the step (4) has a thickness of 100-500 um.
- the present invention provides a lithium ion supercapacitor preparation process as follows:
- the negative electrode sheet, the separator and the positive electrode sheet prepared by the invention are laminated to form a battery core, and then an electrolyte is injected into the battery case, and the injected electrolyte is 1 mol/ L LiPF 6 DOL-DME solution (DOL and DME volume ratio is 1:1), sealing, get lithium ion super electricity
- the graphene material Since the graphene material has high strength and high electrical conductivity, it can be used as a current collector, and the graphene having a high specific surface can be used as a positive electrode active material. Therefore, the graphene material is directly prepared into a positive electrode sheet by the present invention.
- the preparation process of the positive electrode is omitted, and the process of the lithium ion supercapacitor is a general lithium ion battery preparation process, which greatly simplifies the preparation process of the lithium ion supercapacitor.
- the graphene composite Li 2 MoO 3 material positive electrode sheet prepared by the invention is used as a lithium ion supercapacitor cathode material, and the Li 2 MoO material provides a lithium source, and the lithium ion ion stripping Li 2 Mo0 3 material is inserted into the graphite during the first charging.
- the negative electrode the negative electrode potential is pulled down, so that it is not necessary to use a metal lithium plate or a complicated pre-lithium process in the negative electrode.
- the present invention has the following beneficial effects: (1) Graphene composite Li 2 MoO rf material positive electrode sheet as the positive electrode of the lithium ion super capacitor, the anode does not need to be added with lithium sheet or complex pre-intercalation lithium process, simplifying the preparation process (2) Foamed graphene composite Li 2 MoO 3 material positive electrode sheet has high strength, high electrical conductivity and high specific surface area, which can effectively replace conventional activated carbon cathode material and aluminum current collector to achieve high energy density and high power. density.
- FIG. 1 is a cycle life diagram of a lithium ion supercapacitor of the present invention.
- the negative electrode sheet, the separator and the positive electrode sheet of the present invention are formed into a battery core by laminating according to a preparation process of a usual lithium ion battery, and then an electrolyte is injected into the battery case, and the injected electrolyte is 1 mol/L.
- LiPF 6 DOL-DME solution (DOL and DME volume ratio is 1:1), sealed to obtain lithium ion supercapacitor
- the negative electrode sheet, the separator and the positive electrode sheet of the present invention are formed into a battery cell by lamination according to a preparation process of a usual lithium ion battery, and then an electrolyte is injected into the battery case, and the injected electrolyte is 1 mol/L.
- LiPF 6 DOL-DME solution (DOL and DME volume ratio is 1:1), sealed to obtain lithium ion supercapacitor
- the negative electrode sheet, the separator and the positive electrode sheet of the present invention are formed into a battery cell by lamination according to a preparation process of a usual lithium ion battery, and then an electrolyte is injected into the battery case, and the injected electrolyte is 1 mol/L.
- LiPF 6 DOL-DME solution (DOL and DME volume ratio is 1:1), sealed to obtain lithium ion supercapacitor
- the negative electrode sheet, the separator and the positive electrode sheet of the present invention are formed into a battery core by laminating according to a preparation process of a usual lithium ion battery, and then an electrolyte is injected into the battery case, and the injected electrolyte is 1 mol/L.
- LiPF 6 DOL-DME solution (DOL and DME volume ratio is 1:1), sealed to obtain lithium ion supercapacitor
- the lithium ion supercapacitor prepared by the present invention is charged and discharged 1000 times, and the energy is not significantly attenuated.
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
La présente invention concerne un procédé de fabrication d'une électrode positive d'un supercondensateur lithium-ion. Le procédé comprend les étapes suivantes consistant : étape (1) à ajouter un oxyde de graphite et un polyacrylonitrile dans un broyeur à boulets destiné au broyage à boulets, à ajouter un mélange broyé aux boulets dans une solution mixte d'éthanol et d'eau permettant une dispersion ultrasonore afin de former une suspension; étape (2) à immerger une mousse de nickel dans la suspension, à sécher à la vapeur le solvant et à ajouter un mélange gazeux d'hydrogène et d'azote afin de protéger une réaction dans un four à moufle, puis à faire réagir jusqu'à l'achèvement de la réaction, suivie d'un refroidissement naturel; étape (3) à immerger un produit de l'étape précédente dans de l'acide chlorhydrique, à effectuer une réaction, puis à faire réagir jusqu'à l'achèvement de la réaction pour obtenir une mousse de graphène; et étape (4) à ajouter du Li2MoO3 à l'échelle nanométrique dans un toluène, à utiliser des ultrasons pour former une suspension, puis à revêtir par goutte-à-goutte la suspension de toluène contenant du Li2MoO3 sur la mousse de graphène, à sécher et à placer dans un four à moufle pour le recuit, à refroidir, puis à laminer pour obtenir une électrode. L'électrode positive de matériau composite de mousse de graphène-Li2MoO3 présente une densité d'énergie élevée et une puissance volumique élevée.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2016/095454 WO2018032322A1 (fr) | 2016-08-16 | 2016-08-16 | Procédé de fabrication d'électrode positive de condensateur lithium-ion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2016/095454 WO2018032322A1 (fr) | 2016-08-16 | 2016-08-16 | Procédé de fabrication d'électrode positive de condensateur lithium-ion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2018032322A1 true WO2018032322A1 (fr) | 2018-02-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CN2016/095454 WO2018032322A1 (fr) | 2016-08-16 | 2016-08-16 | Procédé de fabrication d'électrode positive de condensateur lithium-ion |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2018032322A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112713277A (zh) * | 2020-12-30 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | 一种硬炭材料及其制备方法和应用、锂离子电池 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103515110A (zh) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Li2MoO3/石墨烯复合材料及其制备方法和锂离子电容器 |
| CN103682368A (zh) * | 2012-09-20 | 2014-03-26 | 中国科学院金属研究所 | 一种快充的柔性锂离子电池及其电极的制备方法 |
| CN104157467A (zh) * | 2014-08-22 | 2014-11-19 | 东莞市迈科新能源有限公司 | 一种碳基锂离子超级电容器 |
| CN105609736A (zh) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | 一种三维碳纳米管/氮掺杂石墨烯/硫电极片的制备方法 |
| CN106229150A (zh) * | 2016-08-16 | 2016-12-14 | 肖丽芳 | 一种锂离子电容器正极片的制备方法 |
-
2016
- 2016-08-16 WO PCT/CN2016/095454 patent/WO2018032322A1/fr active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103515110A (zh) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Li2MoO3/石墨烯复合材料及其制备方法和锂离子电容器 |
| CN103682368A (zh) * | 2012-09-20 | 2014-03-26 | 中国科学院金属研究所 | 一种快充的柔性锂离子电池及其电极的制备方法 |
| CN104157467A (zh) * | 2014-08-22 | 2014-11-19 | 东莞市迈科新能源有限公司 | 一种碳基锂离子超级电容器 |
| CN105609736A (zh) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | 一种三维碳纳米管/氮掺杂石墨烯/硫电极片的制备方法 |
| CN106229150A (zh) * | 2016-08-16 | 2016-12-14 | 肖丽芳 | 一种锂离子电容器正极片的制备方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112713277A (zh) * | 2020-12-30 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | 一种硬炭材料及其制备方法和应用、锂离子电池 |
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