CN116364913A - Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle - Google Patents
Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle Download PDFInfo
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- CN116364913A CN116364913A CN202310341664.3A CN202310341664A CN116364913A CN 116364913 A CN116364913 A CN 116364913A CN 202310341664 A CN202310341664 A CN 202310341664A CN 116364913 A CN116364913 A CN 116364913A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 27
- 239000002116 nanohorn Substances 0.000 title claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 150000001875 compounds Chemical class 0.000 title claims description 8
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229910001416 lithium ion Inorganic materials 0.000 claims description 8
- 238000010891 electric arc Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000010405 anode material Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 5
- 239000010406 cathode material Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000009831 deintercalation Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- H01M4/58—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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- 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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
-
- 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
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 load MoS 2 Preparation method and application of carbon nanohorn composite of nano particles, and MoS-loaded carbon nanohorn composite can be prepared by one-step method 2 Carbon nanohorns of nanoparticles using MoS 2 And carbon nanohorn, and has higher specific capacity, better cycle stability and excellent rate performance when used as a cathode material.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a load MoS 2 A preparation method and application of a carbon nanohorn composite of nano particles.
Background
Lithium-ion batteries (LIBs) have been widely used in the fields of portable electronic devices, electric vehicles, satellites, and the like, due to their advantages of higher energy density and longer service life. Graphite is used as a lithium ion negative electrode material commonly used in current commerce, and the theoretical specific capacity (372 mAh g -1 ) Smaller, limiting its further use in high performance lithium ions. Molybdenum disulfide (MoS) 2 ) Is considered as a graphite-substitutable LIBs negative electrode material. MoS (MoS) 2 (669mAh g -1 ) Has a specific graphite (372 mAh g) -1 ) Higher theoretical specific capacity, and MoS 2 The S-Mo-S three atomic layers are stacked together through Van der Waals force, the interlayer spacing is 0.62nm, and the intercalation and deintercalation of lithium ions are facilitated. However, moS 2 When the LIBs are used as anode materials, the problems of poor conductivity, volume expansion in the process of intercalation/deintercalation and the like still exist, so that the problems of rapid capacity attenuation in the process of discharging/charging are caused, and the commercial application of the LIBs is limited. The MoS-based material is prepared by introducing carbon materials such as graphene, carbon nano tube, carbon fiber and the like 2 Can effectively improve MoS 2 Electrochemical behavior (enhancing conductivity and slowing volume expansion during charge and discharge). Since Chemical Vapor Deposition (CVD) mostly requires the use of a metal catalyst in the preparation of graphene or carbon nanotubes, the cost for mass production of graphene or carbon nanotubes is excessive. In addition, the current literature reports a load MoS 2 The preparation method of the carbon nanocomposite material of (c) is complicated and time-consuming, including hydrothermal (or solvothermal) and subsequent annealing treatment for several or even several tens of hours.
Disclosure of Invention
In view of this, the present invention aims to provide a load MoS 2 Preparation method and application of carbon nanohorn composite of nano particles, and MoS-loaded carbon nanohorn composite can be prepared by one-step method 2 Carbon nanohorns of nanoparticles using MoS 2 And the synergistic effect of the carbon nanohorns, and the energy storage performance of the carbon nanohorns in the lithium ion battery is exerted.
The invention adopts the following specific technical scheme:
load MoS 2 A method for preparing a carbon nanohorn complex of nanoparticles, comprising the steps of:
(1) MoS is carried out 2 Mixing, grinding and uniformly mixing the powder and the graphite powder, filling the mixture into a hollow chromatographic pure graphite rod, and then mounting the filled graphite rod to the anode end of an electric arc furnace;
(2) Evacuating air of the electric arc furnace to the vacuum degree of 10Pa, then introducing carbon monoxide gas into the electric arc furnace to the pressure of 50kPa, and enabling carbon rods of the cathode and the anode to be in contact short circuit under the current of 110A; and then evacuating again to 10Pa, introducing carbon monoxide gas to 40kPa, discharging under the voltage of 40V and the current of 90A, controlling the distance between the anode and the cathode to be 0.1-1.0cm until the anode carbon rod is consumed, collecting the product, and obtaining the compound without impurity removal.
Further, moS used in step (1) 2 The mass ratio of the powder to the graphite powder is 4:1.
Further, in the step (2), the distance between the anode and the cathode is controlled by rotating the carbon rod of the cathode.
Further, the whole discharging process in the step (2) is 10-15 minutes.
Further, before the product is collected in the step (2), carbon monoxide gas in the furnace is pumped out of the chamber and is discharged into air to balance the air pressure in the furnace.
The invention also provides a load MoS 2 The carbon nanohorn composite of the nano particles is prepared by the preparation method.
The invention also provides the load MoS 2 The application of the carbon nanohorn compound of the nano particles in the anode material of the lithium ion battery.
The beneficial effects of the invention are as follows: the preparation method is simple and convenient, does not need impurity removal treatment, has high product purity, can be directly used, and has better production efficiency. And experiments prove that the supported MoS prepared by the invention 2 The carbon nanohorn complex of the nanoparticle has higher specific capacity, better cycle stability and excellent rate performance.
Drawings
FIG. 1 is MoS 2/ Transmission electron microscopy pictures of CNHs complexes.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto, and various substitutions and modifications can be made by those skilled in the art without departing from the technical spirit of the present invention, and are intended to be included in the scope of the present invention.
Example 1
Load MoS 2 Carbon nanohorn (MoS) of nanoparticle 2 CNHs) composite is assembled in situ by arc methodComprises the following steps: moS (MoS) 2 The powder and the graphite powder are mixed, ground and mixed uniformly according to the mass ratio of 4:1, then filled into a hollow chromatographic pure graphite rod (phi 8mm multiplied by 150mm, the hole diameter is phi 5mm multiplied by 125 mm), and then the filled graphite rod is mounted on the anode end of an electric arc furnace. The air of the arc furnace was evacuated to a vacuum degree of 10Pa, and then carbon monoxide gas was introduced into the arc furnace to a pressure of 50kPa, and the carbon rod contacts of the cathode and the anode were short-circuited at a current of 110A. Then, the mixture was evacuated again to 10Pa, and carbon monoxide gas was introduced to 40kPa. The discharge is carried out under the voltage of 40V and the current of 90A, and the distance between the cathode and the anode is controlled to be about 1mm by rotating the carbon rod of the cathode. The whole discharge process takes about 10 to 15 minutes. When the anode carbon rod is consumed, carbon monoxide gas in the furnace is pumped out of the chamber and is put into air to balance the air pressure in the furnace. Finally, collecting the products on the furnace wall and the furnace cover, wherein the obtained products can be directly used without further impurity removal process.
Prepared (MoS 2 CNHs) compound in the negative electrode material of lithium ion battery, the specific implementation method is as follows:
to active substance MoS 2 The CNHs compound, carbon black and sodium alginate are mixed according to the mass ratio of 6:2:2, and then a small amount of deionized water is added, and the mixture is stirred to prepare black slurry. The slurry was coated on a copper foil, followed by vacuum drying at 60 degrees for 8 hours, and then the copper foil coated with the slurry was cut into wafers having a diameter of 11 mm. Button cells are assembled in a glove box under the protection of argon, a counter electrode is a pure metal Li piece, and electrolyte contains 1mol L -1 LiPF of (a) 6 And 5wt% fluoroethylene carbonate (FEC) in a vinyl carbonate/dimethyl carbonate mixture (the volume ratio of vinyl carbonate to dimethyl carbonate is 1:1), the separator of the battery is a microporous polypropylene film Celgard 2400. In the experimental battery, metal lithium is used as a negative electrode, a carbon nanomaterial is used as a positive electrode, and constant-current charge and discharge tests are carried out. After 600 cycles, moS 2 CNHs still have 480.4mAhg -1 And an average CE of greater than 98% over a cycle range of 3-600, whereas pure MoS2 without any treatment has a specific capacity of only 245mAh g at the same current -1 。MoS 2 CNHs ratio pure MoS 2 Has higher specific capacity, better cycle stability and excellent rate performance.
While the embodiments have been described above, other variations and modifications will occur to those skilled in the art once the basic inventive concepts are known, and it is therefore intended that the foregoing description and drawings illustrate only embodiments of the invention and not limit the scope of the invention, and it is therefore intended that the invention not be limited to the specific embodiments described, but that the invention may be practiced with their equivalent structures or with their equivalent processes or with their use directly or indirectly in other related fields.
Claims (7)
1. Load MoS 2 The preparation method of the carbon nanohorn composite of the nano particles is characterized by comprising the following steps:
(1) MoS is carried out 2 Mixing, grinding and uniformly mixing the powder and the graphite powder, filling the mixture into a hollow chromatographic pure graphite rod, and then mounting the filled graphite rod to the anode end of an electric arc furnace;
(2) Evacuating air of the electric arc furnace to the vacuum degree of 10Pa, then introducing carbon monoxide gas into the electric arc furnace to the pressure of 50kPa, and enabling carbon rods of the cathode and the anode to be in contact short circuit under the current of 110A; and then evacuating again to 10Pa, introducing carbon monoxide gas to 40kPa, discharging under the voltage of 40V and the current of 90A, controlling the distance between the anode and the cathode to be 0.1-1.0cm until the anode carbon rod is consumed, collecting the product, and obtaining the compound without impurity removal.
2. The process according to claim 1, wherein MoS is used in step (1) 2 The mass ratio of the powder to the graphite powder is 4:1.
3. The method according to claim 1, wherein in the step (2), the distance between the cathode and the anode is controlled by rotating a carbon rod of the cathode.
4. The method of claim 1, wherein the total discharge in step (2) is 10 to 15 minutes.
5. The method according to claim 1, wherein the carbon monoxide gas in the furnace is evacuated outside the chamber and is introduced into the air to balance the air pressure in the furnace before the product is collected in the step (2).
6. Load MoS 2 A carbon nanohorn composite of nanoparticles, characterized by being prepared by the preparation method according to any one of claims 1 to 5.
7. The loaded MoS of claim 6 2 The application of the carbon nanohorn compound of the nano particles in the anode material of the lithium ion battery.
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CN202310341664.3A CN116364913A (en) | 2023-03-31 | 2023-03-31 | Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle |
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CN202310341664.3A CN116364913A (en) | 2023-03-31 | 2023-03-31 | Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle |
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- 2023-03-31 CN CN202310341664.3A patent/CN116364913A/en active Pending
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