CN111994898A - Carbon material and preparation method and application thereof - Google Patents

Carbon material and preparation method and application thereof Download PDF

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CN111994898A
CN111994898A CN202010922788.7A CN202010922788A CN111994898A CN 111994898 A CN111994898 A CN 111994898A CN 202010922788 A CN202010922788 A CN 202010922788A CN 111994898 A CN111994898 A CN 111994898A
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carbon
carbon material
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王接喜
李广超
李新海
颜果春
王志兴
郭华军
戴雨晴
胡启阳
彭文杰
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Central South University
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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
    • 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
    • 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
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/22—Electronic properties
    • 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

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  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a carbon material and a preparation method and application thereof, wherein the carbon material comprises carbon nano tubes and nano carbon ring points, the nano carbon ring points comprise one or two of carbon nano rings and carbon nano points, and the mass ratio of the carbon nano tubes to the nano carbon ring points is 1: 100-10: 1. The carbon material is prepared by taking organic quantum dots as a precursor through one-step pyrolysis catalysis. The carbon nano tube and the carbon nano-ring are uniformly distributed and organically combined together, the surface contact and the long-range conductivity among active material particles are considered, and a high-efficiency conductive network is constructed; the conductive capacity of the battery electrode is improved through the synergistic effect of the two components.

Description

Carbon material and preparation method and application thereof
Technical Field
The invention relates to the technical field of conductive materials, in particular to a carbon material and a preparation method and application thereof.
Background
The conductive agent material is an important component in the battery assembly process and has an important influence on the electrochemical performance of the battery. The addition of a proper amount of conductive agent in the electrode material can obviously enhance the electronic conductivity of the material and can also construct contact sites between particles of the material. At present, conductive carbon black is mainly used, but the granular structure of the conductive carbon black causes point contact between granules, and an effective long-range conductive network cannot be formed.
The carbon nano tube is a carbon nano material with a one-dimensional linear structure and has excellent mechanical, optical and electrical properties. In recent years, with the continuous progress of energy storage technology, the application of carbon nanotubes in the field of energy storage also shows explosive development, and has wide application prospects, for example, the carbon nanotubes are mixed with graphene to prepare multilevel carbon nanomaterials (such as chinese patent CN110021745A), the carbon nanotubes are mixed with polymer macromolecules (such as chinese patent CN107325421A), the carbon nanotubes are mixed with metal oxides (such as chinese patent CN106024412A), the carbon nanotubes are mixed with metal sulfides (such as chinese patent CN108615620A), and the like, and the excellent performance is shown. However, the carbon nanotube preparation process is complicated and has high requirements for equipment.
Disclosure of Invention
The invention provides a carbon material and a preparation method and application thereof, aiming at overcoming the structural defects of the current battery conductive material, making up the deficiency of the conductivity of the battery conductive material, improving the electron transmission performance of the battery conductive carbon and preparing the carbon nanotube/nano carbon ring dot composite material by a simple and effective method.
In order to achieve the purpose, the carbon material comprises carbon nano tubes and nano carbon ring points, wherein the nano carbon ring points comprise one or two of carbon nano rings and carbon nano points, and the mass ratio of the carbon nano tubes to the nano carbon ring points is 1: 100-10: 1.
Preferably, the outer diameter of the carbon nanotube is 10-100 nm, the thickness of the tube wall is 5-20 nm, and the length is 0.1-1000 um; the diameter of the nano carbon ring point is 2-50 nm.
The invention also provides a preparation method of the carbon material, which comprises the following steps:
s1: mixing a carbon source and a heteroatom source, adding water to dissolve the mixture, carrying out hydrothermal reaction, and evaporating a solvent in a product after the reaction is finished to obtain an organic quantum dot precursor;
wherein the heteroatom source is a-NH containing2or-C ═ S or-C — S bond;
s2: mixing the organic quantum dot precursor obtained in the step S1 with metal salt, then sintering, and carrying out acid washing and drying to obtain a carbon material containing carbon nanotubes and nano carbon ring dots;
the mass ratio of the organic quantum dot precursor to the metal elements in the metal salt is 30: 1-1: 10.
The invention also provides another preparation method of the carbon material, which comprises the following steps:
s1: mixing a carbon source, a heteroatom source and metal salt, adding water to dissolve, carrying out hydrothermal reaction, and evaporating a solvent in a product after the reaction is finished to obtain a metal organic quantum dot precursor;
wherein the heteroatom source is a-NH containing2or-C ═ S or-C — S bond;
the mass ratio of the carbon source to the metal elements in the metal salt is 30: 1-1: 10;
s2: sintering the metal organic quantum dot precursor obtained in the step S1, and performing acid washing and drying to obtain a carbon material containing the carbon nano tube and the nano carbon ring dot;
preferably, the carbon source comprises a carbon source comprising-COOH or-COO-The compound of (1) comprises one or more of hydrated citric acid, anhydrous citric acid, amino acid, citrate, tartaric acid and sodium carboxymethylcellulose; the heteroatom source comprises one or more of urea, thiourea, amino acid and ethylenediamine.
Preferably, the carbon source is hydrated citric acid, anhydrous citric acid or citrate and the heteroatom source is urea or thiourea.
Preferably, the molar ratio of the carbon source to the heteroatom source is 10: 1-1: 5, and the concentration of the carbon source in the reactant is 1-100 g/L.
Preferably, the molar ratio of the carbon source to the heteroatom source is 5: 1-1: 5, and the concentration of the carbon source in the reactant is 30-70 g/L.
Preferably, the temperature of the hydrothermal reaction is 100-220 ℃, and the time of the hydrothermal reaction is 1-10 h.
Preferably, the temperature of the hydrothermal reaction is 150-200 ℃, and the time of the hydrothermal reaction is 3-7 h.
Preferably, the metal salt comprises one or more of nitrate, sulfate, chloride and acetate of iron, cobalt, nickel and chromium.
Preferably, the metal salt is an iron salt.
Preferably, in the step S2, the sintering temperature is 700-1300 ℃, the sintering time is 1-10 hours, and the sintering atmosphere is an inert atmosphere and comprises nitrogen or argon.
Preferably, in S2, the sintering temperature is 720-1000 ℃, the sintering time is 3-7 h,
the invention also provides a lithium ion battery, wherein the carbon material is used as a conductive agent in an electrode of the lithium ion battery; the electrode prepared by using the carbon material as a conductive agent has excellent conductivity, the conductivity is more than 1.1S/cm), the internal resistance of the obtained lithium ion battery is small, and the minimum internal resistance of the battery is 15 omega.
The scheme of the invention has the following beneficial effects:
1. the carbon nano tube and the nano carbon ring dot prepared by the method can realize the advantage combination of the carbon nano tube and the nano carbon ring dot. The linear structure of the carbon nano tube can provide a channel for long-range transportation of electrons, and the nano carbon ring point can realize point contact between particles of the electrode material, so that the defects of the carbon nano tube are overcome. The carbon nano tube and the carbon nano-ring are uniformly distributed and organically combined together, the surface contact and the long-range conductivity among active material particles are considered, and a high-efficiency conductive network is constructed; the conductive capacity of the battery electrode is improved through the synergistic effect of the two components.
2. The preparation method of the carbon nanotube/nano carbon ring dot composite carbon material can realize the preparation of the carbon nanotube/nano carbon ring dot composite carbon material by using the zero-dimensional quantum dots as precursors through a simple one-step catalytic reaction, has obvious advantages, and omits the steps of preparation, uniform dispersion and the like of the carbon material with a single size in the traditional process;
3. the invention can realize the proportion control of the carbon nano tube and the nano carbon ring point by controlling the reaction conditions, such as the particle size of the quantum dot precursor, the proportion of the quantum dot precursor and the catalyst, the type of the catalyst, the heat treatment temperature and the like, thereby realizing the regulation and control of the conductivity of the material.
4. The carbon material prepared by the invention can be used as a lithium ion battery electrode conductive agent, the electrode conductivity can be obviously improved, and the battery multiplying power performance can be improved.
Drawings
Fig. 1 is a transmission electron microscope image of a carbon nanotube and carbon nanoring dot composite material in example 1 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Example 1
A method of making a carbon material, comprising the steps of:
(1) respectively weighing 10mmol and 30mmol of citric acid monohydrate and urea according to the molar ratio of 1:3, adding 100ml of deionized water for dissolving, transferring into a reaction kettle for hydrothermal reaction at 180 ℃ for 8h, and evaporating the solvent in the product after the reaction is finished to obtain a carbon quantum dot precursor;
(2) respectively weighing 2g of the organic quantum dot precursor obtained in the step (1) and 20g of ferric nitrate, adding 50ml of deionized water, dissolving, and freeze-drying;
(3) and (3) sintering the material dried in the step (2) at 700 ℃ for 3h to obtain a composite of the carbon nano tube containing the iron simple substance and the carbon nano ring points, pickling to remove the iron simple substance, washing with water to be neutral, and drying to obtain the composite of the carbon nano tube and the carbon nano ring points. As shown in fig. 1.
Example 2
The same as example 1 except that the sintering temperature was 1000 ℃.
Example 3
The same as example 1 except that the sintering temperature was 1300 ℃.
Example 4
Substantially the same as in example 1, except that the sintering temperature was 1700 ℃.
Example 5
Basically the same as example 1, except that: the hydrothermal reaction temperature is 160 ℃, and the hydrothermal reaction time is 10 hours; the sintering temperature is 900 ℃; the metal salt is manganese nitrate.
Example 6
A method of making a carbon material, comprising the steps of:
(1) respectively weighing 10mmol and 30mmol of anhydrous citric acid and urea according to the mol ratio of 1:3, weighing nickel nitrate according to the mass ratio of the anhydrous citric acid to the nickel of 5:1, adding 100ml of deionized water for dissolving, transferring into a reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 8 hours, and freeze-drying a solvent in a product to obtain a metal organic quantum dot precursor;
(2) and (2) sintering the dried material in the step (1) at 800 ℃ for 3h to obtain a composite of the carbon nano tube containing the nickel simple substance and the carbon nano ring/dot, removing the nickel simple substance by acid washing, washing with water to be neutral, and drying to obtain the composite material of the carbon nano tube and the carbon nano ring dot.
Example 7
The composite material obtained in examples 1 to 6 was used as a conductive agent, and 94% of lithium iron phosphate, 5% of polyvinylidene fluoride, and 1% of the conductive agent were dissolved in N-methylpyrrolidone to obtain positive electrode slurry.Coating the slurry on the surface of an aluminum foil, and baking and compacting to obtain a positive pole piece; the mass surface density of the pole piece is 2mgcm-2(ii) a Lithium sheet as negative electrode, LiPF6Button cells are prepared by using/EC + DEC (volume ratio of 1:1) as electrolyte and Celgard2400 membrane as separator, and the performance of the button cells is tested, and the results are shown in Table 1:
TABLE A test result of the performance of button cell using the carbon material obtained in examples 1 to 6 as a conductive agent
Figure BDA0002667302780000051
From the test results, the carbon material prepared by the preparation method provided by the invention can effectively improve the electrical conductivity of the lithium battery electrode and reduce the internal resistance of the battery, the sintering temperature is too high or the internal resistance of the battery is increased during the preparation process, and when the sintering temperature is 1700 ℃, the carbon nano tube cannot be formed, and the internal resistance of the battery is increased. It can be seen that the sintering temperature also has a large effect on the properties of the carbon material produced.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The carbon material is characterized by comprising carbon nanotubes and carbon nanoring dots, wherein the carbon nanoring dots comprise one or two of carbon nanorings and carbon nanodots, and the mass ratio of the carbon nanotubes to the carbon nanoring dots is 1: 100-10: 1.
2. The carbon material according to claim 1, wherein the carbon nanotube has an outer diameter of 10 to 100nm, a tube wall thickness of 5 to 20nm, and a length of 0.1 to 1000 um; the diameter of the nano carbon ring point is 2-50 nm.
3. A method for producing a carbon material, characterized by comprising the steps of:
s1: mixing a carbon source and a heteroatom source, adding water to dissolve the mixture, carrying out hydrothermal reaction, and evaporating a solvent in a product after the reaction is finished to obtain an organic quantum dot precursor;
wherein the heteroatom source is a-NH containing2or-C ═ S or-C — S bond;
s2: mixing the organic quantum dot precursor obtained in the step S1 with metal salt, then sintering, and carrying out acid washing and drying to obtain a carbon material containing carbon nanotubes and nano carbon ring dots;
the mass ratio of the organic quantum dot precursor to the metal elements in the metal salt is 30: 1-1: 10.
4. A method for producing a carbon material, characterized by comprising the steps of:
s1: mixing a carbon source, a heteroatom source and metal salt, adding water to dissolve, carrying out hydrothermal reaction, and evaporating a solvent in a product after the reaction is finished to obtain a metal organic quantum dot precursor;
wherein the heteroatom source is a-NH containing2or-C ═ S or-C — S bond;
the mass ratio of the carbon source to the metal elements in the metal salt is 30: 1-1: 10;
s2: and sintering the metal organic quantum dot precursor obtained in the step S1, and performing acid washing and drying to obtain the carbon material containing the carbon nano tube and the nano carbon ring dot.
5. The method for producing a carbon material as claimed in any one of claims 3 and 4, wherein the carbon source comprises a carbon source containing-COOH or-COO-The compound of (1) comprises one or more of hydrated citric acid, anhydrous citric acid, amino acid, citrate, tartaric acid and sodium carboxymethylcellulose; the heteroatom source comprises one or more of urea, thiourea, amino acid and ethylenediamine.
6. The method for producing a carbon material as claimed in any one of claims 3 and 4, wherein the molar ratio of the carbon source to the heteroatom source is 10:1 to 1:5, and the concentration of the carbon source in the reactant is 1 to 100 g/L.
7. The method for producing a carbon material as claimed in any one of claims 3 and 4, wherein the temperature of the hydrothermal reaction is 100 to 220 ℃ and the time of the hydrothermal reaction is 1 to 10 hours.
8. The method for producing a carbon material as claimed in any one of claims 3 and 4, wherein the metal salt comprises one or more of nitrate, sulfate, chloride and acetate salts of iron, cobalt, nickel and chromium.
9. The method for producing a carbon material as claimed in any one of claims 3 and 4, wherein the sintering temperature in S2 is 700 to 1300 ℃, the sintering time is 1 to 10 hours, and the sintering atmosphere is an inert atmosphere.
10. A lithium ion battery characterized in that the carbon material according to claim 1 is used as a conductive agent in an electrode of the lithium ion battery.
CN202010922788.7A 2020-09-04 2020-09-04 Carbon material and preparation method and application thereof Pending CN111994898A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2607383A (en) * 2021-06-03 2022-12-07 Univ South China Tech Test strip containing nitrogen-doped carbon quantum dots, preparation method and application thereof
CN115611266A (en) * 2022-10-28 2023-01-17 河北宝力工程装备股份有限公司 Preparation method of oxygen-nitrogen metal doped nano carbon material and application of oxygen-nitrogen metal doped nano carbon material in rubber
CN115986127A (en) * 2022-12-29 2023-04-18 湖北亿纬动力有限公司 Composite aluminum foil current collector, positive plate using same and battery

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CN106276847A (en) * 2016-07-20 2017-01-04 苏州顾氏新材料有限公司 A kind of preparation method of CNT
CN108565131A (en) * 2018-05-23 2018-09-21 中南大学 A method of preparing N doping graphitized carbon
CN108689398A (en) * 2017-04-12 2018-10-23 南京理工大学 A kind of preparation method of controllable nitrogen-doped carbon nanometer pipe

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US20120058889A1 (en) * 2009-03-04 2012-03-08 Hidekazu Nishino Composition containing carbon nanotubes, catalyst for producing carbon nanotubes, and aqueous dispersion of carbon nanotubes
CN101661858A (en) * 2009-08-31 2010-03-03 福州大学 Surface chemical metal plating carbon nanotube field-emission cathode preparation method
US20150217274A1 (en) * 2009-10-21 2015-08-06 Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences Platinum/carbon nanotube catalyst, the preparation process and use thereof
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CN106276847A (en) * 2016-07-20 2017-01-04 苏州顾氏新材料有限公司 A kind of preparation method of CNT
CN108689398A (en) * 2017-04-12 2018-10-23 南京理工大学 A kind of preparation method of controllable nitrogen-doped carbon nanometer pipe
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2607383A (en) * 2021-06-03 2022-12-07 Univ South China Tech Test strip containing nitrogen-doped carbon quantum dots, preparation method and application thereof
GB2607383B (en) * 2021-06-03 2024-02-07 Univ South China Tech Test strip containing nitrogen-doped carbon quantum dots, preparation method and application thereof
CN115611266A (en) * 2022-10-28 2023-01-17 河北宝力工程装备股份有限公司 Preparation method of oxygen-nitrogen metal doped nano carbon material and application of oxygen-nitrogen metal doped nano carbon material in rubber
CN115611266B (en) * 2022-10-28 2023-06-23 河北宝力工程装备股份有限公司 Preparation method of oxygen-nitrogen metal doped nano carbon material and application of oxygen-nitrogen metal doped nano carbon material in rubber
CN115986127A (en) * 2022-12-29 2023-04-18 湖北亿纬动力有限公司 Composite aluminum foil current collector, positive plate using same and battery

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Application publication date: 20201127