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 PDF

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Publication number
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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mos
carbon
anode
cathode
preparation
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CN202310341664.3A
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谭雪友
王海娇
祖士明
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Guangxi University of Science and Technology
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Guangxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/364Composites as mixtures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027Negative electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy 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

Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle
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.
CN202310341664.3A 2023-03-31 2023-03-31 Load MoS 2 Preparation method and application of carbon nanohorn compound of nanoparticle Pending CN116364913A (en)

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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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Application Number Priority Date Filing Date Title
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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CN116364913A true CN116364913A (en) 2023-06-30

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