CN113224275A - Graphene/clay nano composite electrode material and preparation method thereof - Google Patents
Graphene/clay nano composite electrode material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 41
- 239000004927 clay Substances 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 31
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 229910000273 nontronite Inorganic materials 0.000 claims abstract description 9
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000013736 caramel Nutrition 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 8
- 239000007774 positive electrode material Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 239000007773 negative electrode material Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000011049 filling Methods 0.000 description 3
- 229910018688 LixC6 Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- SBWRUMICILYTAT-UHFFFAOYSA-K lithium;cobalt(2+);phosphate Chemical compound [Li+].[Co+2].[O-]P([O-])([O-])=O SBWRUMICILYTAT-UHFFFAOYSA-K 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
Abstract
The invention discloses a preparation method of a graphene/clay nano composite electrode material, which mainly comprises the following steps: mixing caramel, layered clay and water and stirring to prepare a precursor; putting the precursor into a tube furnace, heating to 800-1000 ℃ in an inert gas atmosphere according to a certain heating rate, and keeping for 3-5 hours; and taking out the mixture, and grinding the mixture into powder to obtain the graphene composite nano electrode material. The graphene/clay nano composite electrode material provided by the invention integrates the excellent conductivity of the graphene material and the good chemical property stability of the nontronite, forms an ABAB type stacked layered structure, greatly improves the shuttling capacity and shuttling efficiency of lithium ions between the positive and negative electrode materials in the charging and discharging processes, and has excellent charging and discharging properties and high cycle times. Meanwhile, the electrode material is simple in preparation process and easy to industrialize.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and relates to a clay graphene/clay nano composite material and a preparation method thereof.
Background
Lithium ion batteries have become the main choice of rechargeable power sources for today's portable electronic products due to their advantages of high specific energy, high power density, long cycle life, low self-discharge, high cost performance, etc. Meanwhile, in order to relieve environmental stress, countries around the world compete to develop Hybrid Electric Vehicles (HEVs) that use both batteries and mechanical power. In the development process of the lithium ion battery, the positive electrode material may become a bottleneck restricting large-scale popularization and application of the lithium ion battery, so that the development of the positive electrode material with excellent performance and low price is a key factor in the commercialization process of the lithium ion battery.
The positive electrode of the lithium ion battery is a compound containing metallic lithium, typically a lithium iron phosphate (e.g., lithium iron phosphate LiFePO)4Lithium cobalt phosphate LiCoO2Etc.), the negative electrode is graphite or carbon (general graphite is used in many cases), and an organic solvent is used as an electrolyte between the positive and negative electrodes. When the battery is charged, lithium ions are generated by decomposition on the positive electrode, enter the negative electrode of the battery through the electrolyte and are embedded into micropores of the negative electrode carbon layer. During the use of the battery (corresponding to discharge), lithium ions embedded in the micropores of the negative electrode move back to the positive electrode. The more lithium ions that return to the positive electrode, the higher the discharge capacity, which we usually refer to as the battery capacity. In this way, during the charging and discharging of the battery, lithium ions run back and forth between the positive and negative electrodes, so the lithium ion battery is also called a rocking chair type battery. The electrochemical reaction equation is as follows:
and (3) positive electrode: li0.33Fe(3+)2〔(Al，Si)4O10〕(OH)2·nH2O<＝>
Li0.33-xFe(2+)2〔(Al，Si)4O10〕(OH)2·nH2O+xLi++xe-
Negative electrode: xLi + xe-+6C<＝>LixC6
And (3) total reaction: li0.33Fe(3+)2〔(Al，Si)4O10〕(OH)2·nH2O+6xC<＝>Li0.33·FePO4+LixC6
Graphene is a two-dimensional crystal with only one layer of carbon atoms thick. Graphene does not have the capacity of electricity storage, and is a novel nano material with excellent conductivity. In the charging and discharging process, the shuttling movement of graphene lithium ions between the graphene surface and the electrode is accelerated.
The clay has no very good conductive performance, but has excellent structure stability, and particularly contains divalent iron nontronite, and lithium ions can be guided to be de-intercalated and de-intercalated through electrochemical oxidation reduction in a battery.
The clay graphene composite nano electrode material is a novel electrode material which can be prepared by utilizing the excellent conductivity of graphene and the stable chemical property of the perpetual clay montmorillonite, and has good charge and discharge performance and higher cycle efficiency.
Disclosure of Invention
The present invention aims to provide an electrode material capable of having both excellent conductivity and chemical stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphene/clay nano composite electrode material is characterized by comprising the following steps:
(1) according to mCaramel∶mLayered clay∶mWater (W)Mixing caramel, layered clay and water in a ratio of 1: 2-3: 5-8, and stirring for 2-5 hours to obtain a precursor;
(2) putting the precursor obtained in the step (1) into a tube furnace, heating to 800-1000 ℃ in an inert gas atmosphere according to the heating rate of 5-10 ℃/min, and keeping for 3-5 hours;
(3) and (3) taking out the mixture obtained in the step (2) and grinding the mixture into powder to obtain the graphene composite nano electrode material.
Further, the layered clay in the step (1) is nontronite powder with the granularity of 200-400 meshes.
Further, the water in the step (1) is deionized water.
Further, the inert gas in the step (2) is nitrogen.
Further, in the step (3), the mixture is ground into powder with 200-400 meshes.
The invention also aims to provide the graphene/clay nano composite electrode material prepared by the preparation method, which is characterized in that the graphene/clay nano composite electrode material is an ABAB type stacked layered material doped with lithium ions.
Further, the lithium ion doped region is an interlayer region where graphene is located.
The graphene/clay nano composite electrode material integrates the excellent conductivity of the graphene material and the good chemical property stability of the nontronite, forms an ABAB type stacked layered structure (as shown in figure 1), greatly improves the shuttling capacity and shuttling efficiency of lithium ions between a positive electrode material and a negative electrode material in the charging and discharging process, and has excellent charging and discharging performance and high cycle number. Meanwhile, the electrode material is simple in preparation process and easy to industrialize.
Drawings
Fig. 1 is a structural view of a graphene composite nanoelectrode material according to the present invention.
Detailed Description
Example 1
Taking 10g of caramel, 20g of nontronite powder with the granularity of 200 meshes and 50g of deionized water, mixing, and placing in a high-speed stirrer to stir for 2.5 hours to prepare a precursor;
placing the precursor in a tube furnace, filling nitrogen, heating to 800 ℃ at the heating rate of 5 ℃/min, and continuously maintaining for 3 hours;
and taking out the obtained mixture, and grinding the mixture to 200 meshes to obtain the graphene/clay nano composite electrode material.
The structure of the graphene/clay nano composite electrode material is shown in fig. 1, and the graphene/clay nano composite electrode material has an ABAB type layered structure, and a lithium ion doped region is an inter-graphene region.
The charge and discharge properties of the obtained material are shown in the following table:
example 2
Taking 20g of caramel, 40g of nontronite powder with the granularity of 200 meshes and 120g of deionized water, mixing, and placing in a high-speed stirrer to stir for 3.5 hours to prepare a precursor;
placing the precursor in a tube furnace, filling nitrogen, heating to 800 ℃ at the heating rate of 8 ℃/min, and continuously maintaining for 3 hours;
and taking out the obtained mixture, and grinding the mixture to 300 meshes to obtain the graphene/clay nano composite electrode material.
The structure of the graphene/clay nano composite electrode material is shown in fig. 1, and the graphene/clay nano composite electrode material has an ABAB type layered structure, and a lithium ion doped region is an inter-graphene region.
The charge and discharge properties of the obtained material are shown in the following table:
example 3
Taking 40g of caramel, 80g of nontronite powder with the granularity of 200 meshes and 320g of deionized water, mixing and placing in a high-speed stirrer to stir for 5 hours to prepare a precursor;
placing the precursor in a tube furnace, filling nitrogen, heating to 900 ℃ at the heating rate of 5 ℃/min, and continuously maintaining for 5 hours;
and taking out the obtained mixture, and grinding the mixture to 400 meshes to obtain the graphene/clay nano composite electrode material.
The structure of the graphene/clay nano composite electrode material is shown in fig. 1, and the graphene/clay nano composite electrode material has an ABAB type layered structure, and a lithium ion doped region is an inter-graphene region.
The charge and discharge properties of the obtained material are shown in the following table:
the tests prove that the graphene/clay nano composite electrode material integrates the excellent conductivity of the graphene material and the good chemical property stability of the nontronite, greatly improves the shuttling capacity and shuttling efficiency of lithium ions between the positive and negative electrode materials in the charging and discharging processes, and has excellent charging and discharging properties and high cycle times.
Claims (7)
1. A preparation method of a graphene/clay nano composite electrode material is characterized by comprising the following steps:
(1) according to mCaramel∶mLayered clay∶mWater (W)Mixing caramel, layered clay and water in a ratio of 1: 2-3: 5-8, and stirring for 2-5 hours to obtain a precursor;
(2) putting the precursor obtained in the step (1) into a tube furnace, heating to 800-1000 ℃ in an inert gas atmosphere according to the heating rate of 5-10 ℃/min, and keeping for 3-5 hours;
(3) and (3) taking out the mixture obtained in the step (2) and grinding the mixture into powder to obtain the graphene composite nano electrode material.
2. The method according to claim 1, wherein the layered clay in the step (1) is nontronite powder having a particle size of 200-400 mesh.
3. The method according to claim 1, wherein the water in the step (1) is deionized water.
4. The method according to claim 1, wherein the inert gas in the step (2) is nitrogen.
5. The method as claimed in claim 1, wherein the mixture is ground into 400 mesh powder in step (3).
6. The graphene/clay nanocomposite electrode material prepared by the preparation method of any one of claims 1 to 5, wherein the structure of the graphene/clay nanocomposite electrode material is a lithium ion-doped ABAB type stacked layered material.
7. The graphene/clay nanocomposite electrode material according to claim 6, wherein the lithium ion doped region is an interlayer domain region where graphene is located.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157736A (en) * | 2011-03-23 | 2011-08-17 | 中银（宁波）电池有限公司 | Ferrous disulfide/carbon composite cathode material of primary lithium battery and preparation method and application thereof |
| WO2013103537A1 (en) * | 2012-01-04 | 2013-07-11 | Momentive Performance Materials Inc. | Silicone adhesive compositions |
| CN103950914A (en) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | Preparation method of conductive carbon material with graphene-like structure |
| CN107128903A (en) * | 2017-06-02 | 2017-09-05 | 扬州大学 | To crimp the method that the halloysite nanotubes of layer structure prepare graphene |
| US20180366280A1 (en) * | 2017-06-14 | 2018-12-20 | Nanotech Energy, Inc | Electrodes and electrolytes for aqueous electrochemical energy storage systems |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157736A (en) * | 2011-03-23 | 2011-08-17 | 中银（宁波）电池有限公司 | Ferrous disulfide/carbon composite cathode material of primary lithium battery and preparation method and application thereof |
| WO2013103537A1 (en) * | 2012-01-04 | 2013-07-11 | Momentive Performance Materials Inc. | Silicone adhesive compositions |
| CN103950914A (en) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | Preparation method of conductive carbon material with graphene-like structure |
| CN107128903A (en) * | 2017-06-02 | 2017-09-05 | 扬州大学 | To crimp the method that the halloysite nanotubes of layer structure prepare graphene |
| US20180366280A1 (en) * | 2017-06-14 | 2018-12-20 | Nanotech Energy, Inc | Electrodes and electrolytes for aqueous electrochemical energy storage systems |
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Denomination of invention: A graphene/clay nanocomposite electrode material and its preparation method Granted publication date: 20220719 Pledgee: Agricultural Bank of China Limited Yangyuan County Branch Pledgor: YANGYUAN COUNTY RENHENG FINE CLAY Co.,Ltd. Registration number: Y2024980003041 |