CN112047329A - Preparation method of fluorinated modified graphene negative electrode long-cycle battery and product thereof - Google Patents
Preparation method of fluorinated modified graphene negative electrode long-cycle battery and product thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 32
- 239000010439 graphite Substances 0.000 claims abstract description 32
- -1 hydroxide ions Chemical class 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000003792 electrolyte Substances 0.000 claims abstract description 14
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 239000011737 fluorine Substances 0.000 claims abstract description 14
- 239000007773 negative electrode material Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 239000007774 positive electrode material Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052744 lithium Inorganic materials 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 239000010405 anode material Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- 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
-
- 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
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 preparation method of a fluorinated modified graphene cathode long-cycle battery and a product thereof.A high-purity graphene powder can be obtained by utilizing an electrochemical corrosion method, generating alkaline hydroxide ions and oxygen as external force for stripping after external voltage is applied, controlling the number of C-F bonds in a system through the concentration of fluorine ions in a solution, and cleaning and drying precipitates; then adding graphite and mixing according to a certain proportion to obtain a negative electrode material, and matching and assembling the negative electrode material with the positive electrode, the electrolyte and the diaphragm to obtain the long-cycle lithium ion battery. The method is suitable for large-scale batch preparation, and has the advantages of short time consumption and high purity. The powder prepared by the method can be used for preparing the high-performance lithium battery field.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a manufacturing method of a fluorinated modified graphene negative electrode long-cycle battery and a product thereof.
Background
With the rapid development of lithium battery technology, innovations in miniaturization, flexibility and long endurance are urgently needed. High capacity lithium batteries are commercially important power sources, but have limited cycle life, low power density, poor low temperature kinetics, and safety issues. Recently, the high power density, the strong flexibility and the high safety of the graphene modified negative electrode become research hotspots in the field of lithium batteries, but the cyclicity is still a technical difficulty to be solved.
The fluorocarbon-containing nano material has good chemical stability and high-temperature stability in organic electrolyte, can not be decomposed when the temperature is up to 400 ℃, has the characteristics of stable voltage, wide working temperature, small self-discharge, long service life and the like, and can meet the requirements of extreme environments such as aerospace and the like. When the battery discharges, the fluorine-containing carbon material is converted into the nano carbon material with stronger conductivity, so that the overall conductivity of the electrode is increased, and the stable discharge voltage and the improvement of the discharge efficiency are facilitated.
The method for stripping by electrochemical corrosion uses aqueous solution containing fluoride as electrolyte, applies a certain voltage, allows the reduction of water, generates strong nucleophilic hydroxyl ions (OH-), continuously corrodes the interlayer bonds of graphite, and simultaneously generates oxygen by the continuous oxidation of water, and all of the above provide great force for separating weakly bonded graphite layers. The fluorine ions in the solution simultaneously polarize to form C-F bonds.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a fluorinated modified graphene negative electrode long-cycle battery.
Yet another object of the present invention is to: the fluorinated modified graphene negative electrode long-cycle battery product prepared by the method is provided.
The purpose of the invention is realized by the following scheme: a preparation method of a fluorinated modified graphene cathode long-cycle battery comprises a one-step method for synthesizing a fluorine-containing modified graphene material, and is characterized in that an electrochemical corrosion method is utilized, after external voltage is applied, alkaline hydroxyl ions and oxygen are generated to serve as external force for stripping, the number of C-F bonds in a system is controlled through the concentration of fluorine ions in a solution, and precipitates are cleaned and dried to obtain high-purity graphene powder; then adding graphite and mixing according to a certain proportion to obtain a negative electrode material, and matching and assembling the negative electrode material with a positive electrode, electrolyte and a diaphragm to obtain the long-cycle lithium ion battery, wherein the method comprises the following steps:
(1) weighing a proper amount of fluoride, dissolving the fluoride in deionized water to prepare a solution with the concentration of 0.1-1mol/l, and adjusting the pH value to 7;
(2) the electrochemical system uses inert material as anode and graphite as cathode, the areas of the anode and cathode are the same and are 4cm2；
(3) Applying voltage to allow water to be reduced to generate hydroxyl ions, corroding the graphite layer, and enabling the fluorine ions and the graphite to form C-F bonds;
the prepared graphene layer is ultrasonically cleaned and dried, and is mechanically mixed with graphite, wherein the mixing ratio is graphene: graphite = 5-30%: 95-70% of the active carbon to be used as a negative electrode;
(4) the cylinder and the soft package battery are made of a ternary positive electrode material, the diaphragm and the electrolyte are commercial products, and the design capacity is 0.5-2.5 Ah.
The fluoride in the step (1) is one of sodium fluoride, potassium hexafluorophosphate and ammonium fluoride.
The inert material in the step (2) is one of platinum and gold electrode.
The voltage applied in the step (3) is 10 mV-2V.
The ternary positive electrode material selected in the step (4) is Li [ Ni ]1/3Co1/3Mn1/3]O2And Li [ Ni ]0.5Co0.2Mn0.3]O2The electrolyte is one of the conventional electrolytes of Tiancio and Huarong of the Thailand, and the diaphragm is one of the specifications of a star source and Enjie of 10 microns.
The invention provides a fluorinated modified graphene negative electrode long-cycle battery which is prepared according to any one of the methods.
The present invention proposes to exfoliate graphite by utilizing hydroxyl and oxygen generated by electrode reaction as driving forces, on the basis of the full recognition of the electrochemical reaction principle. The method is simple in preparation, short in time consumption and strong in controllability, and can be used for producing high-quality graphene materials. The powder prepared by the method can be used for preparing long-circulating cathode materials.
Drawings
FIG. 1 is an AFM spectrum of a powder sample obtained in example 1 of the present invention;
fig. 2 is a battery cycle life curve obtained in example 1 of the present invention.
Detailed Description
Example 1
A fluorinated modified graphene cathode long-cycle battery comprises a one-step method for synthesizing a fluorine-containing modified graphene material, and is characterized in that an electrochemical corrosion method is utilized, after external voltage is applied, alkaline hydroxyl ions and oxygen are generated to serve as external force for stripping, the number of C-F bonds in a system is controlled through the concentration of fluorine ions in a solution, and precipitates are cleaned and dried to obtain high-purity graphene powder; then adding graphite and mixing according to a certain proportion to obtain a negative electrode material, matching and assembling the negative electrode material with a positive electrode, an electrolyte and a diaphragm to obtain the long-cycle lithium ion battery, and preparing according to the following steps:
(1) weighing sodium fluoride, dissolving the sodium fluoride in 500ml of deionized water to prepare a solution with the concentration of 0.1mol/l, and adjusting the pH value to 7;
(2) the electrochemical system uses inert material platinum sheet as positive electrode, graphite as negative electrode, the areas of positive and negative electrodes are identical and are 4cm2；
(3) Applying a voltage of 10mV to reduce water to generate hydroxyl ions, corroding the graphite layer, and enabling fluorine ions and graphite to form a C-F bond; the prepared graphene layer is ultrasonically cleaned and dried, as shown in figure 1, and is mechanically mixed with graphite, wherein the mixed molar ratio is graphene: graphite = 5%: 95% of the solution to be used as a negative electrode;
(4) selection of Li [ Ni ]1/3Co1/3Mn1/3]O2As the anode material, Njie 20 microns is used as a diaphragm, a cylindrical battery with 0.5Ah is prepared by using a Tiancio conventional electrolyte, the cycle life is as long as more than 1000 times, and the figure 2 shows.
Example 2
Similar to example 1, a fluorinated modified graphene negative electrode long-cycle battery is prepared by the following steps:
(1) weighing potassium hexafluorophosphate, dissolving in 500ml deionized water to prepare a solution with the concentration of 1mol/l, and adjusting the pH value to 7;
(2) an electrochemical system uses a platinum sheet as a positive electrode, graphite as a negative electrode, and the areas of the positive electrode and the negative electrode are 4cm2；
(3) Applying 2V voltage to reduce water to generate hydroxyl ions, corroding a graphite layer, forming C-F bonds by the fluorine ions and graphite, ultrasonically cleaning and drying the prepared graphene layer, and mechanically mixing the graphene layer with the graphite, wherein the mixed molar ratio is graphene: graphite = 30%: 70% for standby;
(4) selection of Li [ Ni ]1/3Co1/3Mn1/3]O2As the anode material, the star source 20 microns is used as a diaphragm, and the cylindrical lithium battery with 2.5Ah is prepared from the general electrolyte of the Thailand gorgeon, and the cycle life is as long as more than 800 times.
Example 3
Similar to example 1, a fluorinated modified graphene negative electrode long-cycle battery is prepared by the following steps:
(1) weighing a proper amount of ammonium fluoride, dissolving the ammonium fluoride in 500ml of deionized water to prepare a solution with the concentration of 0.5mol/l, and adjusting the pH value to 7;
(2) gold sheet is used as the positive electrode, graphite is used as the negative electrode, and the area of the positive electrode and the negative electrode is 4cm2；
(3) The method comprises the following steps of applying 1V voltage to reduce water to generate hydroxyl ions, corroding a graphite layer, forming C-F bonds by fluorine ions and graphite, ultrasonically cleaning and drying the prepared graphene layer, and mechanically mixing the graphene layer with the graphite, wherein the mixed ratio is graphene: graphite = 15%: 85% for standby;
(4) selection of Li [ Ni ]1/3Co1/3Mn1/3]O2As the anode material, the star source 20 microns is used as a diaphragm, the Tianci conventional electrolyte is made into a cylindrical lithium battery of 1.5Ah, and the cycle life is as long as more than 900 times.
Claims (6)
1. A preparation method of a fluorinated modified graphene cathode long-cycle battery comprises a one-step method for synthesizing a fluorine-containing modified graphene material, and is characterized in that an electrochemical corrosion method is utilized, after external voltage is applied, alkaline hydroxide ions and oxygen are generated to serve as external force for stripping, the number of C-F bonds in a system is controlled through the concentration of fluorine ions in a solution, and precipitates are cleaned and dried to obtain high-purity graphene powder; then adding graphite and mixing according to a certain proportion to obtain a negative electrode material, and matching and assembling the negative electrode material with a positive electrode, electrolyte and a diaphragm to obtain the long-cycle lithium ion battery, wherein the method comprises the following steps:
(1) weighing a proper amount of fluoride, dissolving the fluoride in deionized water to prepare a solution with the concentration of 0.1-1mol/l, and adjusting the pH value to 7;
(2) the electrochemical system uses inert material as anode and graphite as cathode, the areas of the anode and cathode are the same and are 4cm2；
(3) Applying voltage to reduce water to generate hydroxyl ions, corroding the graphite layer, and enabling the fluorine ions and the graphite to form a C-F bond;
the prepared graphene layer is ultrasonically cleaned and dried, and is mechanically mixed with graphite, wherein the mixed molar ratio is graphene: graphite = 5-30%: 95-70% of the active carbon to be used as a negative electrode;
(4) the cylinder and the soft package battery are made of a ternary positive electrode material, the diaphragm and the electrolyte are commercial products, and the design capacity is 0.5-2.5 Ah.
2. The preparation method of the fluorinated modified graphene cathode long-cycle battery according to claim 1, which is characterized by comprising the following steps: the fluoride in the step (1) is one of sodium fluoride, potassium hexafluorophosphate and ammonium fluoride.
3. The preparation method of the fluorinated modified graphene cathode long-cycle battery according to claim 1, which is characterized by comprising the following steps: the inert material in the step (2) is one of platinum and gold electrode.
4. The preparation method of the fluorinated modified graphene cathode long-cycle battery according to claim 1, which is characterized by comprising the following steps: the voltage applied in the step (3) is 10 mV-2V.
5. As set forth in claim 1The preparation method of the fluorinated modified graphene cathode long-cycle battery is characterized by comprising the following steps of: the ternary positive electrode material selected in the step (4) is Li [ Ni ]1/3Co1/3Mn1/3]O2And Li [ Ni ]0.5Co0.2Mn0.3]O2The electrolyte is one of the conventional electrolytes of Tiancio and Huarong of the Thailand, and the diaphragm is one of the specifications of a star source and Enjie of 10 microns.
6. A fluorinated modified graphene negative electrode long-cycle battery, which is characterized by being prepared according to the method of any one of claims 1 to 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112687873A (en) * | 2020-12-23 | 2021-04-20 | 湖南永盛新材料股份有限公司 | Preparation method of high-specific-energy lithium battery |
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| CN111899983A (en) * | 2020-07-15 | 2020-11-06 | 铜仁学院 | Preparation method of graphene, prepared graphene, application of graphene and super capacitor |
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Cited By (1)
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| CN112687873A (en) * | 2020-12-23 | 2021-04-20 | 湖南永盛新材料股份有限公司 | Preparation method of high-specific-energy lithium battery |
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Application publication date: 20201208 |