CN109494368B - Preparation method and application of carbon nano composite material - Google Patents
Preparation method and application of carbon nano composite material Download PDFInfo
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- CN109494368B CN109494368B CN201811470997.1A CN201811470997A CN109494368B CN 109494368 B CN109494368 B CN 109494368B CN 201811470997 A CN201811470997 A CN 201811470997A CN 109494368 B CN109494368 B CN 109494368B
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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 and application of a carbonaceous nano composite material, and relates to a carbon material. A preparation method of a carbonaceous nano composite material comprises the following steps: respectively dissolving a boron-containing compound and a metallic antimony compound in a mixed solution of deionized water and absolute ethyl alcohol, adding a high polymer material, heating to 80-100 ℃, keeping the temperature for 0.5-2 hours, and cooling to obtain a gel-state substance; freeze-drying for 10-48 h to obtain dry gel; and (3) placing the carbon nano composite material in a tubular furnace, vacuumizing, introducing inert gas at the speed of 100-300 ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 600-1200 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2-5 h, and cooling to room temperature to obtain the carbon nano composite material. The preparation method has the advantages of simple preparation process, low raw material cost, no environmental pollution in the preparation process, controllable structure and performance and capability of obtaining the carbonaceous nano composite materials with different sodium storage performances.
Description
Technical Field
The invention relates to a carbon material, in particular to a preparation method and application of a carbon nano composite material prepared based on hydrothermal reaction and carbonization processes.
Background
The traditional graphite material has low efficiency of sodium ion deintercalation, slow kinetic rate and large volume expansion, so that the direct application of the graphite material in a sodium ion battery is limited, and the anode material of the sodium ion battery with high capacity, high sodium diffusivity and good cycle performance is seriously deficient. Because the size of sodium ions is larger than that of lithium, most lithium ion battery cathode materials have poor performance in sodium ion batteries, and have the problems of low intercalation efficiency, slow kinetic rate, serious volume expansion and the like, so that the design and preparation of the novel sodium ion battery cathode material are particularly critical.
In the existing sodium ion battery cathode material system (carbon material, alloy material, metal oxide, etc.), the carbon material exists: low cost, various structures, high reversible capacity, stable cycle performance and flexible space construction characteristics. Among them, hard carbon has a large carbon layer distance and disordered micropores, and has more sodium storage sites, so that hard carbon attracts great attention of many researchers as a sodium storage negative electrode material.
However, the sodium storage capacity, the cycle performance and the rate performance of the hard carbon still need to be improved, and the invention is to develop the carbon nano composite material with high sodium storage capacity.
Disclosure of Invention
The invention aims to provide a preparation method of a carbonaceous nano composite material.
It is another object of the present invention to provide the use of carbonaceous nanocomposites.
The invention idea is as follows: the carbon nano composite material with high reversible capacity and rate capability is prepared by hydrothermal reaction and high-temperature carbonization, and is used for preparing the cathode material of the sodium-ion battery.
The invention is realized by the following technical scheme:
a preparation method of a carbonaceous nano composite material comprises the following steps:
1) preparation of gel-state material: respectively dissolving a boron-containing compound and a metallic antimony compound in a mixed solution of deionized water and absolute ethyl alcohol, adding a high polymer material, uniformly stirring, heating to 80-100 ℃, keeping the temperature for 0.5-2 hours, and cooling to obtain a gel-state substance;
2) preparation of xerogel: freeze-drying the gel-state substance for 10-48 h to obtain dry gel;
3) preparing a carbonaceous nanocomposite: and (3) placing the dried gel in a tube furnace, vacuumizing, introducing inert gas at the speed of 100-300 ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 600-1200 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2-5 h, and cooling to room temperature to obtain the carbon nano composite material.
Further, the boron-containing compound is sodium tetraphenylborate, ammonium pentaborate or dimethylaminoborane.
The antimony compound is antimony acetate, antimony trichloride or antimony pentafluoride.
The volume ratio of the deionized water to the absolute ethyl alcohol is 3-6: 1.
the high polymer material is starch or cellulose.
The boron-containing compound: compounds of metallic antimony: the mass-volume ratio of the high polymer material is 12-26 g:18g:100 mL.
The inert gas is high-purity argon or nitrogen.
Furthermore, the invention also provides an application of the carbonaceous nano composite material, and the carbonaceous nano composite material can be used as a negative electrode material of a sodium-ion battery.
According to the invention, by utilizing hydrothermal reaction and high-temperature carbonization methods, heteroatom boron is introduced into a hard carbon structure and is used as a substitution site boron atom of an electron acceptor, so that electrons can be more easily obtained from sodium by the carbon structure, the adsorption effect on alkali metal ions is enhanced, a wider carbon layer interval is generated, more sodium ions are favorably adsorbed and rapidly de-intercalated, the energy density and rate characteristics of the hard carbon cathode material are further improved, and meanwhile, antimony with high sodium storage capacity is introduced into a boron-doped hard carbon material matrix, so that a carbon nano composite material with high sodium storage capacity, high reversible capacity and rate capability is formed, and the composite material can be used as a cathode material of a sodium ion battery.
In order to verify the performance of the carbonaceous nano composite material, the performance of the carbonaceous nano composite material is respectively measured through a scanning electron microscope, a transmission electron microscope, an X-ray photoelectron spectrum, an X-ray diffraction spectrum and a sodium storage; wherein, FIG. 2 is a scanning electron microscope picture of the carbonaceous nano composite material, and the microscopic morphology of the carbonaceous nano composite material obtained in the invention in a jellyfish shape can be clearly seen from the picture; FIG. 3 is a transmission electron micrograph of a carbonaceous nanocomposite, wherein transmission electron micrograph analysis of the carbonaceous nanocomposite shows that the carbonaceous nanocomposite has a jellyfish-like microstructure; FIG. 4 is an X-ray photoelectron spectrum of the carbonaceous nanocomposite, from which it can be derived that the carbonaceous nanocomposite contains five elements of carbon, boron, antimony, oxygen and nitrogen; FIG. 5 is an X-ray diffraction spectrum of a carbonaceous nanocomposite, which is proved to contain amorphous carbon and metallic elemental antimony by analyzing the phase composition of the material prepared in the present invention; fig. 6 shows the sodium storage performance of the carbonaceous nanocomposite, and it can be seen from the figure that the material prepared in the present invention has high specific capacity and excellent cycling stability.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation process is simple, the cost of the raw materials is low, the raw materials do not need to be pretreated, and the carbonaceous sodium ion battery cathode material can be obtained through hydrothermal reaction and high-temperature carbonization;
(2) the preparation process has no environmental pollution, the process is environment-friendly, and no waste gas, waste liquid, waste residue and the like are generated;
(3) the structure and the performance are controllable, and the carbon nano composite materials with different sodium storage performances can be obtained by simply adjusting the proportion of the high polymer material and the inert metal compound.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
FIG. 2 is a scanning electron microscope image of the carbonaceous nanocomposite prepared in example 1 of the present invention.
FIG. 3 is a transmission electron microscope image of the carbonaceous nanocomposite prepared in example 1 of the present invention.
FIG. 4 is an X-ray photoelectron spectrum of the carbonaceous nanocomposite prepared in example 1 of the present invention.
FIG. 5 is an X-ray diffraction pattern of the carbonaceous nanocomposite prepared in example 1 of the present invention.
FIG. 6 shows the sodium storage capacity of the carbonaceous nanocomposite prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and embodiments, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Respectively dissolving 5.300g of sodium tetraphenylborate and 4.500g of antimony acetate in 25ml of a mixed solution (volume ratio is 3: 1) of deionized water and absolute ethyl alcohol, then adding 13.500g of starch, uniformly stirring, heating the mixed solution to 80 ℃, keeping the temperature for 0.5h, and cooling to form a gel-state substance; then freeze-drying for 10h to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 100ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 600 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 2
Respectively dissolving 3.300g of ammonium pentaborate, 2.000g of dimethylamino borane and 4.500g of antimony acetate in 25ml of mixed solution (volume ratio is 3: 1) of deionized water and absolute ethyl alcohol, then adding 13.500g of starch, uniformly stirring, heating the mixed solution to 90 ℃, keeping the temperature for 1.5h, and cooling to form a gel-state substance; then freeze-drying for 24h to form xerogel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 150ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 900 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 3.5h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 3
Respectively dissolving 5.300g of dimethylamino borane, 2.000g of antimony pentafluoride and 2.500g of antimony acetate in 25ml of mixed solution (volume ratio is 4: 1) of deionized water and absolute ethyl alcohol, then adding 13.500g of cellulose, uniformly stirring, heating the mixed solution to 100 ℃, keeping the temperature for 2 hours, and cooling to form a gel-state substance; then dried by freezing for 48 hours to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 300ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 1200 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 5h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 4
Respectively dissolving 4.800g of dimethylamino borane and 4.500g of antimony acetate in 25ml of mixed solution (volume ratio is 5: 1) of deionized water and absolute ethyl alcohol, adding 12.500g of starch, uniformly stirring, heating the mixed solution to 100 ℃, keeping the temperature for 1.5h, and cooling to form a gel-state substance; then dried by freezing for 36 hours to form xerogel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 200 ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 1000 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 4h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 5
4.300g of ammonium pentaborate and 4.500g of antimony trichloride are respectively dissolved in 25ml of mixed solution (volume ratio is 6: 1) of deionized water and absolute ethyl alcohol, 4.500g of starch and 7.000 g of cellulose are added, the mixed solution is uniformly stirred, the temperature is raised to 95 ℃, the temperature is kept for 0.5h, and then the mixed solution is cooled to form a gel-state substance; then dried by freezing for 48 hours to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 300ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 1100 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 3h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 6
Respectively dissolving 3.500g of sodium tetraphenylborate and 4.500g of antimony acetate in 25ml of a mixed solution (volume ratio is 3: 1) of deionized water and absolute ethyl alcohol, adding 8.500g of starch, uniformly stirring, heating the mixed solution to 100 ℃, keeping the temperature for 0.5h, and cooling to form a gel-state substance; then dried by freezing for 48 hours to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 100ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 800 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 5h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 7
Respectively dissolving 3.000g of ammonium pentaborate and 4.500g of antimony pentafluoride in 25ml of mixed solution (volume ratio is 5: 1) of deionized water and absolute ethyl alcohol, adding 12.500g of cellulose, uniformly stirring, heating the mixed solution to 90 ℃, keeping the temperature for 1.5h, and cooling to form a gel-state substance; then dried by freezing for 36 hours to form xerogel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 200 ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 1000 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 8
Respectively dissolving 6.500g of ammonium pentaborate and 4.500g of antimony acetate in 25ml of mixed solution (volume ratio is 3: 1) of deionized water and absolute ethyl alcohol, then adding 13.500g of starch, uniformly stirring, heating the mixed solution to 80 ℃, keeping the temperature for 0.5h, and cooling to form a gel-state substance; then dried by freezing for 48 hours to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 300ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 700 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 3h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 9
Respectively dissolving 6.000g of ammonium pentaborate and 4.500g of antimony trichloride in 25ml of a mixed solution (volume ratio is 4: 1) of deionized water and absolute ethyl alcohol, adding 12.500g of cellulose, uniformly stirring, heating the mixed solution to 90 ℃, keeping the temperature for 1.5h, and cooling to form a gel-state substance; then freeze-drying for 24h to form xerogel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 100ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 900 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2-5 h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
Example 10
Respectively dissolving 5.500g of sodium tetraphenylborate and 4.500g of antimony acetate in 25ml of a mixed solution (volume ratio is 6: 1) of deionized water and absolute ethyl alcohol, then adding 13.500g of starch, uniformly stirring, heating the mixed solution to 100 ℃, keeping the temperature for 0.5h, and cooling to form a gel-state substance; then dried by freezing for 48 hours to form dry gel; placing the dried xerogel in a tubular furnace, vacuumizing, introducing inert gas at the speed of 300ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 1200 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 5h, and cooling to room temperature; and finally, obtaining the carbonaceous nano composite material, and using the carbonaceous nano composite material as an active material for manufacturing the cathode of the sodium-ion battery.
The above-mentioned embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be used, not restrictive; it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.
Claims (8)
1. A method for preparing a carbonaceous nanocomposite, characterized by comprising the steps of:
1) preparation of gel-state material: respectively dissolving a boron-containing compound and a metallic antimony compound in a mixed solution of deionized water and absolute ethyl alcohol, then adding a high polymer material, uniformly stirring, heating to 80-100 ℃, keeping the temperature for 0.5-2 hours, and cooling to obtain a gel-state substance;
2) preparation of xerogel: freeze-drying the gel-state substance for 10-48 h to obtain dry gel;
3) preparing a carbonaceous nanocomposite: and (3) placing the dried gel in a tube furnace, vacuumizing, introducing inert gas at the speed of 100-300 ml/min, repeatedly vacuumizing, introducing inert protective gas for several times, heating to 600-1200 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 2-5 h, and cooling to room temperature to obtain the carbon nano composite material.
2. The method for preparing a carbonaceous nanocomposite as claimed in claim 1, wherein the boron-containing compound is any one or a mixture of sodium tetraphenylborate, ammonium pentaborate and dimethylaminoborane.
3. The method for preparing a carbonaceous nanocomposite as claimed in claim 1 or 2, wherein the metallic antimony compound is any one or a mixture of antimony acetate, antimony trichloride and antimony pentafluoride.
4. The method for preparing the carbonaceous nanocomposite material according to claim 1 or 2, wherein the volume ratio of the deionized water to the absolute ethyl alcohol is 3-6: 1.
5. the method of claim 1 or 2, wherein the polymer material is starch, cellulose, or a mixture thereof.
6. The method of claim 1 or 2, wherein the boron-containing compound: compounds of metallic antimony: the mass-volume ratio of the high polymer material is 12-26 g:18g:100 mL.
7. The method of claim 1 or 2, wherein the inert gas is high purity argon or nitrogen.
8. Use of the carbonaceous nanocomposite material according to claim 1, wherein the carbonaceous nanocomposite material is used as a negative electrode material for sodium ion batteries.
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| CN115974045B (en) * | 2022-12-06 | 2024-02-13 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic alkaline metal oxide template method and application thereof |
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