CN110148713B - Carbon-coated nitrogen-rich g-C3N4And anode material and preparation method thereof - Google Patents

Carbon-coated nitrogen-rich g-C3N4And anode material and preparation method thereof Download PDF

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CN110148713B
CN110148713B CN201810148357.2A CN201810148357A CN110148713B CN 110148713 B CN110148713 B CN 110148713B CN 201810148357 A CN201810148357 A CN 201810148357A CN 110148713 B CN110148713 B CN 110148713B
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潘晖
钟熊伟
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University of Macau
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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
    • 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
    • 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
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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 carbon-coated nitrogen-rich g-C3N4And a negative electrode material and a preparation method thereof, relating to the technical field of lithium battery materials. Carbon-coated nitrogen-rich g-C3N4Has high active site and conductivity, and is coated with nitrogen-rich g-C3N4The lithium ion battery also has a micro-nano structure, effectively prevents agglomeration and ensures high-efficiency lithium storage performance.

Description

Carbon-coated nitrogen-rich g-C3N4And anode material and preparation method thereof
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to carbon-coated nitrogen-rich g-C3N4And a negative electrode material and a method for producing the same.
Background
With the rapid development of science and technology and economy, environmental problems are increasingly prominent, so that the development of high-energy-density energy storage devices becomes an important link for the development of new energy. Among energy storage devices, lithium ion batteries have high energy density and are currently a focus of research. The lithium ion battery cathode material mainly adopts graphite and silicon, wherein the capacity of the graphite material is close to the theoretical capacity (372mAh/g), the promotion space is small, and the manufacturing cost is high; in addition, silicon-based negative electrode materials have high theoretical capacity (4200mAh/g) and low delithiation potential (<0.5V) and are paid extensive attention, but silicon is a semiconductor material and has low self conductivity, lithium ion intercalation and deintercalation can cause the volume of the material to expand and contract by more than 300% in the electrochemical cycling process, and the generated mechanical force can cause the material to be gradually pulverized to cause structural collapse, and finally, electrode active substances are separated from a current collector to lose electric contact, so that the cycling performance of the battery is greatly reduced. Therefore, development of a negative electrode material with high energy density, high stability and low cost has been the research direction of the next generation of negative electrode materials.
Graphite phase carbon nitride (g-C)3N4) Is a novel low-cost,The graphene-like two-dimensional material has rich lithium storage active sites and higher theoretical energy density, but g-C3N4Is a semiconductor, has poor conductivity, and is not widely used in the end.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide carbon-coated nitrogen-rich g-C3N4The preparation method of (1). The preparation method can improve g-C3N4Lithium storage active sites and electrical conductivity.
Another object of the present invention is to provide a carbon-coated nitrogen-rich g-C3N4. The carbon-coated nitrogen-rich g-C3N4Has good conductivity.
The invention also aims to provide a preparation method of the anode material. The preparation method can know the negative electrode material with good conductivity.
Another object of the present invention is to provide a negative electrode material. The negative electrode material has good conductivity.
Another object of the present invention is to provide a negative electrode sheet. The negative plate has good conductivity.
Another object of the present invention is to provide a battery. The battery has good conductivity, can be charged and discharged circularly for many times, and has stable specific capacity.
Another object of the present invention is to provide an electrically powered device. The battery can be charged and discharged circularly for many times, and has stable specific capacity and long service life.
The invention is realized by the following steps:
in one aspect, the invention provides a carbon-coated nitrogen-rich g-C3N4The production method of (1), which comprises: g to C3N4Calcining in ammonia gas to obtain nitrogen-enriched g-C3N4(abbreviated as N-g-C)3N4)。
Further, in some embodiments of the present invention, the calcination temperature in the ammonia gas is 450 to 600 ℃, the calcination time is 0.5 to 36 hours, and the flow rate of the ammonia gas is 5 to 900 sccm.
Further, in some embodiments of the present invention, the above preparation method further comprises:
nitrogen-rich g-C3N4Mixing with organic solvent and carbon source, heating, maintaining temperature, cleaning, and oven drying to obtain powder.
Further, in some embodiments of the invention, the heating temperature is 120-200 ℃, the heat preservation time is 1-36h, and the drying temperature is 40-80 ℃.
Further, in some embodiments of the present invention, the carbon source is a hydrocarbon dissolved in water.
Further, in some embodiments of the present invention, the water-soluble hydrocarbon is selected from the group consisting of glucose, sucrose, fructose, maltose, starch, and cellulose.
Further, in some embodiments of the present invention, the organic solvent is insoluble g-C3N4But an organic solvent that dissolves hydrocarbons.
Further, in some embodiments of the present invention, the organic solvent is selected from one or more of methanol, ethanol, N-methylpyrrolidone, and acetone.
Further, in some embodiments of the present invention, the above preparation method further comprises:
heating and carbonizing the powder under the protection of inert gas to obtain carbon-coated nitrogen-rich g-C3N4(abbreviated as: C/N-g-C3N4)。
Further, in some embodiments of the present invention, the inert gas is selected from any one of helium, neon, argon, krypton, and xenon.
Further, in some embodiments of the invention, the temperature for heat carbonization is 450 to 600 ℃.
Further, in some embodiments of the present invention, the above preparation method further comprises: preparation of g-C3N4A step of;
preparation of g-C as described above3N4The method comprises the following steps: heating the carbon nitride compound to 450-600 ℃ at a heating rate of 1-10 ℃/min in an air atmosphere, and keeping the temperature for 1-20 h.
After the heat preservation is finished, the room temperature is cooled to obtain g-C3N4And (3) powder.
Further, in some embodiments of the present invention, the carbon-nitrogen compound is selected from any one or more of urea, melamine, hexamethylenetetramine, dicyandiamide, cyanamide, dicyandiamide, and the like.
In another aspect, the invention provides a carbon-coated nitrogen-rich g-C3N4Which is prepared by the preparation method as described above.
In another aspect, the present invention provides a method for preparing an anode material, including: nitrogen-rich g-C coated with the above carbon3N4Mixing with a binder and a conductive agent to prepare slurry.
Further, in some embodiments of the invention, 60 wt% to 90 wt% of the carbon-coated nitrogen-rich g-C is present in weight percent3N45 to 20 weight percent of binder and 0.05 to 20 weight percent of conductive agent are mixed to prepare slurry.
Further, in some embodiments of the present invention, the above binder is selected from one or more of asphalt, polyvinylidene fluoride, polytetrafluoroethylene, hydroxypropyl methylcellulose, polyvinyl alcohol, styrene-butadiene rubber latex, polyethylene oxide, and sodium alginate.
Further, in some embodiments of the present invention, the conductive agent is selected from one or more of natural flake graphite, microcrystalline graphite, and conductive carbon black.
In another aspect, the invention provides a negative electrode material, which is prepared by the preparation method of the negative electrode material.
In another aspect, the present invention provides a negative electrode sheet, the surface of which is coated with the negative electrode material.
In another aspect, the present invention provides a battery, which includes the negative electrode sheet described above.
In another aspect, the present invention provides an electric device mounted with the battery described above.
The invention has the following beneficial effects:
the carbon-coated nitrogen-rich g-C provided by the invention3N4By NH3Calcining, solvothermal and carbonizing to obtain carbon-coated nitrogen-rich g-C3N4On the one hand, C/N-g-C is increased3N4On the other hand, the active site of (A) is increased by C/N-g-C3N4The conductivity of (a);
the carbon-coated nitrogen-rich g-C provided by the invention3N4Has high active site and conductivity, and is coated with nitrogen-rich g-C3N4The lithium ion battery also has a micro-nano structure, effectively prevents agglomeration and ensures high-efficiency lithium storage performance;
the cathode material provided by the invention is prepared from the carbon-coated nitrogen-rich g-C3N4The prepared product has good conductivity.
The surface of the negative plate provided by the invention is coated with the negative material, so that the negative plate has good conductivity.
The battery provided by the invention is assembled by the negative electrode plates, has good conductivity, can be charged and discharged repeatedly, and has stable specific capacity.
The electric equipment provided by the invention is provided with the battery, can be charged and discharged repeatedly, and has stable specific capacity and long service life.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows C/N-g-C provided in example 1 of the present invention3N4SEM picture of (1);
FIG. 2 shows C/N-g-C provided in example 1 of the present invention3N4The lithium battery thus obtained was subjected to a cycle chart at a current density of 0.1A/g (in the chart, 1st represents the 1st time, 50 th time)thRepresenting the 50 th time, 100th representing the 100th time).
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
1) 5g of melamine were calcined at 550 ℃ for 2h to give a yellow powder, which was then NH-powdered at 550 ℃3Calcining for 4h under atmosphere to obtain N-g-C3N4。
2) Taking 1g N-g-C3N4Adding 30ml of water and 5ml of methanol into a beaker, ultrasonically stirring for 30min, adding 0.2g of glucose, stirring for 1min, placing the mixture into a polytetrafluoroethylene reaction kettle, heating to 140 ℃, preserving heat for 24h, collecting precipitates, cleaning, and drying at 60 ℃.
3) Heating the dried powder to 600 deg.C under argon gas for carbonization to obtain C/g-C3N4 flower-shaped nanosphere compound (i.e. carbon-coated nitrogen-rich g-C)3N4) The SEM image is shown in FIG. 1.
The results in FIG. 1 show that the composite has the morphology of flower-shaped nanospheres with the diameter of 2-3 μm and a sheet-shaped structure, and the material has more active sites and larger specific surface area on lithium storage.
4) 80 wt% of C/g-C3N4Mixing the flower-shaped nanosphere compound, 10 wt% of sodium alginate and 10 wt% of Ketjen black to prepare slurry; coating the slurry on copper foil, drying, and testing with lithium battery, wherein the active substance mass is 2.58mg, and the electrolyte is New Zea corporationElectrolyte LBC 3707F. The capacity of the lithium battery is shown in table 1 and fig. 2.
Example 2
1) Calcining 3g of a mixture of dicyanodiamine and melamine at 500 ℃ for 12h to give a yellow powder, then calcining the powder at 480 ℃ in NH3Calcining for 10 hours under atmosphere to obtain N-g-C3N4。
2) Taking 2g N-g-C3N4Adding 35ml of NMP solvent (N-methyl derivative of 2-pyrrolidone) into a beaker, ultrasonically stirring for 5min, adding 0.5g of cane sugar, stirring for 5min, placing in a polytetrafluoroethylene reaction kettle, heating to 200 ℃, preserving heat for 10h, collecting precipitate, cleaning, and drying at 180 ℃.
3) Heating the dried powder to 500 ℃ under argon gas for carbonization to obtain C/g-C3N4Flower-shaped nanosphere complexes.
4) 60 wt% of C/g-C3N4Mixing the flower-shaped nanosphere compound, 20 wt% of sodium alginate and 20 wt% of Ketjen black to prepare slurry; and coating the slurry on a copper foil, drying, and assembling a lithium battery for testing, wherein the mass of the active material is 2.62mg, and the electrolyte is LBC315T9 of New Zenation company. The capacity of the lithium battery is shown in table 1.
Example 3
1) Calcining 10g mixture of dicyanodiamine, hexamethylenetetramine and urea at 450 deg.C for 24h to obtain yellow powder, and calcining the yellow powder at 520 deg.C in the presence of NH3Calcining for 8 hours under atmosphere to obtain N-g-C3N4。
2) Taking 2g N-g-C3N4Adding 35ml of acetone solvent into a beaker, ultrasonically stirring for 3min, adding 0.4g of a mixture of sucrose and glucose (wherein the mass ratio of sucrose to glucose is 2:1), stirring for 3min, placing in a polytetrafluoroethylene reaction kettle, heating to 150 ℃, preserving heat for 16h, collecting precipitates, cleaning, and drying at 200 ℃.
3) Heating the dried powder to 550 ℃ under argon gas for carbonization to obtain C/g-C3N4Flower-shaped nanosphere complexes.
4) 75 wt% of C/g-C3N4Flower-shaped nanosphere complex, 10 wt% sodium alginate and 15 wt%Mixing the Keqin black to prepare slurry; and coating the slurry on a copper foil, drying, and assembling a lithium battery for testing, wherein the mass of the active material is 2.56mg, and the electrolyte is LBC315T9 of New Zenation company. The capacity of the lithium battery is shown in table 1.
Example 4
1) 4g of dicyanodiamine are calcined at 490 ℃ for 5h and then the powder is NH at 600 ℃3Calcining for 6 hours under atmosphere to obtain N-g-C3N4。
2) Taking 3g N-g-C3N4Adding 35ml of ethanol solvent into a beaker, ultrasonically stirring for 15min, adding 0.4g of a mixture of glucose and starch (mass ratio is 1:3), stirring for 1min, placing in a polytetrafluoroethylene reaction kettle, heating to 160 ℃, preserving heat for 5h, collecting precipitates, cleaning, and drying at 120 ℃.
3) Heating the dried powder to 525 ℃ under argon gas for carbonization to obtain C/g-C3N4Flower-shaped nanosphere complexes.
4) 85 wt% of C/g-C3N4Mixing the flower-shaped nanosphere compound, 10 wt% of sodium alginate and 5 wt% of Ketjen black to prepare slurry; and coating the slurry on a copper foil, drying, and assembling a lithium battery for testing, wherein the mass of the active material is 2.68mg, and the electrolyte is LBC3508C of New Zebra company. The capacity of the lithium battery is shown in table 1.
Example 5
1) 20g of cyanamide are calcined at 580 ℃ for 15h, and then the powder is treated with NH at 570 DEG C3Calcining for 9 hours under atmosphere to obtain N-g-C3N4。
2) Taking 6g N-g-C3N4Adding 25ml of water and 10ml of acetone solvent into a beaker, ultrasonically stirring for 20min, adding 0.2g of a mixture of sucrose and cellulose (the mass ratio is 5:1), stirring for 2min, placing in a polytetrafluoroethylene reaction kettle, heating to 190 ℃, keeping the temperature for 14h, collecting precipitates, cleaning, and drying at 80 ℃.
3) Heating the dried powder to 580 ℃ under argon gas for carbonization to obtain C/g-C3N4Flower-shaped nanosphere complexes.
4) Mixing 90 wt% of C/g-C3N4Flower-shaped nanosphere complex, 6 wt% sodium alginateMixing with Ketjen black at a ratio of 4 wt% to prepare a slurry; and coating the slurry on a copper foil, drying, and assembling a lithium battery for testing, wherein the mass of the active material is 2.60mg, and the electrolyte is LBC3508C of New Zebra company. The capacity of the lithium battery is shown in table 1.
TABLE 1C/N-g-C provided by examples 1-53N4Manufactured battery test related data
Specific capacity of 50 th cycle charge (mAh/g) Current Density (A/g)
Example 1 480 0.1
Example 2 468 0.1
Example 3 470 0.1
Example 4 460 0.1
Example 5 475 0.1
According to the results in table 1, it can be seen that the C/N-g-C3N4 obtained in examples 1-5 has a higher capacity, which is larger than the theoretical 375mAh/g of graphite, and the 50 th specific capacity is selected, which indicates that the material has stable capacity and no obvious attenuation, and the capacities obtained by different carbon sources are not different greatly, indicating that the method is easy to be industrialized.
Comparative example 1
Using g-C which has not undergone a carbon-rich step3N4The experiment for assembling the lithium battery is as follows:
20g of melamine is calcined for 15h at 550 ℃ to obtain g-C3N4；
Mixing 90 wt% of g-C3N4Mixing the flower-shaped nanosphere compound, 6 wt% of sodium alginate and 4 wt% of Ketjen black to prepare slurry; the slurry is coated on a copper foil, and a lithium battery is assembled for testing after drying, wherein the mass of the active material is 2.56mg, and the capacity of the electrolyte is LBC322-01 lithium battery of New Zenation company is shown in Table 2.
Comparative example 2
N-g-C enriched with nitrogen but not coated with carbon3N4The experiment for assembling the lithium battery is as follows:
calcining 20g of urea at 550 ℃ for 4h to obtain g-C3N4Then NH of the powder at 550 ℃3Calcining for 5h under atmosphere to obtain N-g-C3N4；
85 wt% of N-g-C3N4Mixing the flower-shaped nanosphere compound, 5 wt% of sodium alginate and 10 wt% of Ketjen black to prepare slurry; the slurry is coated on a copper foil, and a lithium battery is assembled after drying for testing, wherein the mass of the active material is 2.56mg, and the capacity of the electrolyte is LBC315T9 lithium battery of New Zenation company is shown in Table 2.
Table 2 data relating to testing of cells made from comparative examples 1-2
Comparative example Material Specific capacity of 50 th cycle charge (mAh/g) Current Density (A/g)
1 g-C3N4 30 0.1
2 N-g-C3N4 20 0.1
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A method for preparing an anode material, comprising:
preparation of carbon-coated Nitrogen-enriched g-C3N4Preparation of carbon-coated nitrogen-rich g-C3N4The method comprises the following steps: g to C3N4Calcining in ammonia gas to obtain nitrogen-enriched g-C3N4Then the nitrogen enriched g-C3N4Mixing with an organic solvent and a carbon source, thermally preserving the temperature of the solvent, cleaning and drying to prepare powder;
then the carbon-coated nitrogen-rich g-C3N4Mixing with a binder and a conductive agent to prepare slurry.
2. The method according to claim 1, wherein the calcination in the ammonia gas is carried out at a temperature of 450 to 600 ℃, for a time of 0.5 to 36 hours, and at a flow rate of 5 to 900 sccm.
3. The method of claim 1, wherein the nitrogen-rich g-C is3N4The temperature of the solvent after mixing with the organic solvent and the carbon source is 120-200 ℃, the heat preservation time is 1-36h, and the drying temperature is 40-80 ℃.
4. The method of claim 1, wherein the producing carbon-coated nitrogen-rich g-C3N4Further comprising:
heating and carbonizing the powder under the protection of inert gas to obtain carbon-coated nitrogen-rich g-C3N4。
5. The method according to claim 4, wherein the temperature for the carbonization by heating is 450 to 600 ℃.
6. The production method according to claim 1 or 2, characterized by further comprising: preparation of g-C3N4A step of;
preparation g to C3N4The method comprises the following steps: heating the carbon nitride compound in air atmosphere to 450-600 ℃ at a heating rate of 1-10 ℃/min, and preserving the heat for 1-20 h.
7. A negative electrode material, characterized in that it is produced by the production method according to any one of claims 1 to 6.
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Synergistic effect of 2D Ti2C and g-C3N4 for efficient photocatalytic hydrogen production;Mengmeng Shao，et al.;《Journal of Materials Chemistry A》;20170710;第16748-16756页 *

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