CN111170303A - Preparation method and application of carbon fluoride material - Google Patents

Preparation method and application of carbon fluoride material Download PDF

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Publication number
CN111170303A
CN111170303A CN202010048761.XA CN202010048761A CN111170303A CN 111170303 A CN111170303 A CN 111170303A CN 202010048761 A CN202010048761 A CN 202010048761A CN 111170303 A CN111170303 A CN 111170303A
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carbon
carbon fluoride
producing
fluoride material
gas
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CN111170303B (en
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岳红军
钟贵明
陈慧鑫
卢灿忠
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Xiamen Zhongke Xifu Technology Co ltd
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Xiamen Institute of Rare Earth Materials
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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
    • C01B32/10—Carbon fluorides, e.g. [CF]nor [C2F]n
    • 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
    • H01M4/5835—Comprising fluorine or fluoride salts
    • 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
    • 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
    • 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 carbon fluoride material, which comprises the following steps: s1, weighing 70-98% by mass of a soft carbon raw material and 2-30% by mass of a graphite carbon material, mixing in a solvent, uniformly stirring, and sintering at 300-1500 ℃ in a protective atmosphere for 1-24 hours to obtain a pretreatment material; s2, grinding the pretreatment material obtained in the step S1 and preparing a powdery product; s3, putting the powdery product obtained in the step S2 into fluorination equipment, introducing fluorination gas, keeping the pressure at 90-120 kPa, and reacting at 350-450 ℃ for 8-16 h to obtain the carbon fluoride material. The carbon fluoride material prepared by the invention has high specific power and high specific energy, can realize discharge under the current of 10A/g, has the specific energy of more than 850 Wh/kg and the specific power of more than 17000W/kg, and can be applied to the anode material of the lithium carbon fluoride battery.

Description

Preparation method and application of carbon fluoride material
Technical Field
The invention belongs to the field of electrochemical energy storage of power supply technology, and particularly relates to a preparation method and application of a carbon fluoride material.
Background
When the carbon fluoride is used as the positive electrode material of the lithium primary battery, the theoretical specific energy of mass is as high as 2180 Wh kg-1, and the carbon fluoride is the commercial lithium primary battery material with the highest theoretical specific energy at present. The lithium fluorocarbon battery is widely applied to various civil and military fields such as electronic radio frequency identification systems, cardiac pacemakers, missile ignition systems, small satellites or space weapons and the like for maneuvering orbital transfer launching, kinetic energy interception missiles, space stations and the like. The specific energy of the carbon fluoride material is determined by the fluorination degree of the material, the higher the fluorination degree is, the higher the theoretical specific energy is, but the higher the fluorination degree is, the poorer the electronic conductance of the material is, when the fluorine-carbon ratio is close to 1, the carbon fluoride is equivalent to an electronic insulator, the large-rate discharge performance of the material is limited, the specific capacity and the rate performance are mutually restricted, and the two are difficult to simultaneously achieve the optimization.
In order to improve the rate capability of carbon fluoride materials, researchers have developed various material modification approaches. For example, the measure of coating the surface with the high-conductivity material plays a certain role in improving the rate capability of the material. The direct addition of highly conductive carbon nanotubes, graphene, and the like in the positive electrode formulation is also a traditional modification measure. In addition, it is also a way to improve the discharge performance of the material by compounding a second phase positive electrode active material having a good rate capability or a higher discharge voltage with carbon fluoride. However, the methods are difficult to achieve the optimization of the specific capacity and the rate capability of the carbon fluoride material at the same time, and how to achieve the property of high specific energy while obtaining the performance of high specific power puts requirements on the structural design of the carbon fluoride material.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for producing a carbon fluoride material having both high specific power and high specific energy, and use thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a carbon fluoride material, comprising the steps of:
s1, weighing 70-98% by mass of soft carbon raw materials and 2-30% by mass of graphite carbon materials, mixing in a solvent, uniformly stirring, and sintering at 300-1500 ℃ in a protective atmosphere for 1-24 hours to obtain the pretreatment material.
S2, grinding the pretreatment material obtained in the step S1 and preparing a powdery product.
S3, putting the powdery product obtained in the step S2 into fluorination equipment, introducing fluorination gas, keeping the pressure at 90-120 kPa, and reacting at 350-450 ℃ for 8-16 h to obtain the carbon fluoride material.
Further, in the step S2, the pretreatment material is ground until the particle size reaches below 60 um, and then the powder is sequentially sieved through a 200-mesh sieve, a 400-mesh sieve and a 800-mesh sieve to obtain a powdery product.
Further, the fluorocarbon material prepared in step S3 has a fluorocarbon ratio of 0.7 to 1.0.
Further, the soft carbon raw material is one or a combination of more of petroleum coke, petroleum needle coke, coal needle coke and non-graphitized intermediate carbon microspheres.
Further, the graphite-like carbon material is one or a combination of natural graphite, artificial graphite, graphene and carbon nanotubes.
Further, the solvent is one or more of water, ethanol, acetone, methyl methacrylate, butyl acrylate, acrylic acid, isopropanol, butyl glycol ether, tetrahydrofuran, benzene, toluene, xylene and dimethylformamide.
Further, the protective atmosphere is one or a combination of nitrogen, argon, neon and helium.
Further, the fluoridizing gas is one or a combination of more of xenon difluoride, nitrogen trifluoride, fluorine gas, boron trifluoride and mixed gas of fluorine gas and argon gas.
The invention also discloses an application of the carbon fluoride material prepared by the preparation method in preparation of a lithium carbon fluoride battery.
The invention has the following beneficial effects: the carbon fluoride material prepared by the preparation method has high specific power and high specific energy, can realize discharge under the current of 10A/g, has the specific energy of more than 850 Wh/kg and the specific power of more than 17000W/kg, and can be applied to the anode material of the lithium carbon fluoride battery.
Drawings
FIG. 1 is a diagram illustrating the electrochemical performance test results of the carbon fluoride material prepared in the first embodiment.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example one
A method for preparing a carbon fluoride material, comprising the steps of:
the method comprises the following steps: the mass ratio of the non-graphitized mesocarbon microbeads of the soft carbon raw material to the graphene material is 98%: 2 percent, mixing the non-graphitized mesocarbon microbeads and the graphene material in methyl methacrylate, uniformly stirring, and sintering for 12 hours in a protective atmosphere at 900 ℃ to obtain the pretreatment material.
And step two, grinding the pretreated product obtained in the step one until the particle size reaches below 60 microns, and sequentially sieving the ground product with 200-mesh, 400-mesh and 800-mesh sieves to obtain a powdery product.
Step three: and (3) putting the powder material obtained in the step two into fluorination equipment, introducing a fluorination gas NF3, keeping the pressure at 120KPa, and reacting for 12 h at the temperature of 450 ℃ to obtain the carbon fluoride material with the bulk phase containing grapheme carbon and the fluorine-carbon ratio of 0.8.
The carbon fluoride material prepared by the method is used as a lithium battery anode material to be assembled into a button cell to be tested for electrochemical performance: (1) the working electrode is a bulk phase containing graphene carbon, the mass ratio of the carbon fluoride to the acetylene black to the polyvinylidene fluoride is 0.8: 1: 1, mixing materials; (2) the counter electrode is a lithium metal sheet; (3) the electrolyte is 1M lithium tetrafluoroborate solution dissolved in ethylene carbonate and dimethyl carbonate (volume ratio is 1: 1); (4) the discharge cut-off voltage is 1.5V; (5) the discharge current was 10A/g.
The performance results obtained from the above tests are shown in fig. 1, and the material shows excellent rate performance, and at 10A/g, the discharge is 1.5V, the discharge time is 184s, the specific energy is 1073 Wh/kg, and the specific power is 20993W/kg.
Example two
A method for preparing a carbon fluoride material, comprising the steps of:
the method comprises the following steps: according to the mass ratio of the non-graphitized mesocarbon microbeads of the soft carbon raw material to the graphene material of 70%: 30 percent, mixing the non-graphitized mesocarbon microbeads and the graphene material in methyl methacrylate, uniformly stirring, and sintering for 24 hours in a protective atmosphere at 300 ℃ to obtain the pretreatment material.
And step two, grinding the pretreated product obtained in the step one until the particle size reaches below 60 microns, and sequentially sieving the ground product with 200-mesh, 400-mesh and 800-mesh sieves to obtain a powdery product.
Step three: and (3) putting the powder material obtained in the step two into fluorination equipment, introducing a fluorination gas NF3, keeping the pressure at 90KPa, and reacting for 24 hours at 350 ℃ to obtain the carbon fluoride material with the bulk phase containing grapheme carbon and the fluorine-carbon ratio of 0.7.
The carbon fluoride material prepared in the embodiment is tested, and the material shows excellent rate performance, and is discharged to 1.5V at 10A/g, the discharge time is 175 s, the specific energy is 852Wh/kg, and the specific power is 17526W/kg.
EXAMPLE III
A method for preparing a carbon fluoride material, comprising the steps of:
the method comprises the following steps: the mass ratio of the non-graphitized mesocarbon microbeads of the soft carbon raw material to the graphene material is 85%: 15 percent, mixing the non-graphitized mesocarbon microbeads and the graphene material in methyl methacrylate, uniformly stirring, and sintering for 3 hours in a protective atmosphere at 1500 ℃ to obtain the pretreatment material.
And step two, grinding the pretreated product obtained in the step one until the particle size reaches below 60 microns, and sequentially sieving the ground product with 200-mesh, 400-mesh and 800-mesh sieves to obtain a powdery product.
Step three: and (3) putting the powder material obtained in the step two into fluorination equipment, introducing a fluorinated gas NF3, keeping the pressure at 100KPa, and reacting for 10 hours at the temperature of 400 ℃ to obtain the carbon fluoride material with the bulk phase containing grapheme carbon and the fluorine-carbon ratio of 0.75.
The carbon fluoride material prepared in the embodiment is tested, and the material shows excellent rate capability, and is discharged to 1.5V at 10A/g, the discharge time is 178 s, the specific energy is 881 Wh/kg, and the specific power is 17817W/kg.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. A method for producing a carbon fluoride material, characterized by comprising the steps of:
s1, weighing 70-98% by mass of a soft carbon raw material and 2-30% by mass of a graphite carbon material, mixing in a solvent, uniformly stirring, and sintering at 300-1500 ℃ in a protective atmosphere for 1-24 hours to obtain a pretreatment material;
s2, grinding the pretreatment material obtained in the step S1 and preparing a powdery product;
s3, putting the powdery product obtained in the step S2 into fluorination equipment, introducing fluorination gas, keeping the pressure at 90-120 kPa, and reacting at 350-450 ℃ for 8-16 h to obtain the carbon fluoride material.
2. The method for producing a carbon fluoride material according to claim 1, wherein: in the step S2, the pretreatment material is ground until the particle size is below 60 um, and then the powder is sequentially sieved by a 200-mesh sieve, a 400-mesh sieve and a 800-mesh sieve to obtain a powdery product.
3. The method for producing a carbon fluoride material according to claim 1, wherein: the fluorocarbon material prepared in the step S3 has a fluorine-carbon ratio of 0.7-1.0.
4. The method for producing a carbon fluoride material according to claim 1, wherein: the soft carbon raw material is one or a combination of more of petroleum coke, petroleum needle coke, coal needle coke and non-graphitized intermediate carbon microspheres.
5. The method for producing a carbon fluoride material according to claim 1, wherein: the graphite carbon material is one or a combination of natural graphite, artificial graphite, graphene and carbon nanotubes.
6. The method for producing a carbon fluoride material according to claim 1, wherein: the solvent is one or more of water, ethanol, acetone, methyl methacrylate, butyl acrylate, acrylic acid, isopropanol, ethylene glycol butyl ether, tetrahydrofuran, benzene, toluene, xylene and dimethylformamide.
7. The method for producing a carbon fluoride material according to claim 1, wherein: the protective atmosphere is one or a combination of more of nitrogen, argon, neon and helium.
8. The method for producing a carbon fluoride material according to claim 1, wherein: the fluoridizing gas is one or a combination of more of xenon difluoride, nitrogen trifluoride, fluorine gas, boron trifluoride and fluorine gas and argon gas mixed gas.
9. Use of the carbon fluoride material produced by the production method according to any one of claims 1 to 8 for producing a lithium carbon fluoride cell.
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CN112158832A (en) * 2020-10-08 2021-01-01 天津大学 Method for improving specific capacity of carbon fluoride and discharge voltage through boron-doped graphene
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
CN113675385A (en) * 2021-07-13 2021-11-19 厦门理工学院 Nanoscale silicon-carbon composite negative electrode material, preparation method and lithium ion battery
CN114335455A (en) * 2021-12-06 2022-04-12 电子科技大学长三角研究院(湖州) Method for precisely fluorinating soft carbon with adjustable crystallinity and research on performance of primary battery

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112158832A (en) * 2020-10-08 2021-01-01 天津大学 Method for improving specific capacity of carbon fluoride and discharge voltage through boron-doped graphene
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
CN113675385A (en) * 2021-07-13 2021-11-19 厦门理工学院 Nanoscale silicon-carbon composite negative electrode material, preparation method and lithium ion battery
CN113675385B (en) * 2021-07-13 2022-12-09 厦门理工学院 Nanoscale silicon-carbon composite negative electrode material, preparation method and lithium ion battery
CN114335455A (en) * 2021-12-06 2022-04-12 电子科技大学长三角研究院(湖州) Method for precisely fluorinating soft carbon with adjustable crystallinity and research on performance of primary battery
CN114335455B (en) * 2021-12-06 2023-11-10 电子科技大学长三角研究院(湖州) Method for precisely fluorinating soft carbon with adjustable crystallinity and primary battery performance research

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