CN108807000B - Preparation method of nano porous carbon for high-performance super capacitor - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for 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
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention provides a preparation method of nanoporous carbon for a high-performance supercapacitor, which comprises the following steps: step 1) preparation of a precursor nano metal organic framework Fe-BTT, and step 2) preparation of nano porous carbon, wherein the preparation comprises the following specific steps: calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600-800 ℃, the precursor nano metal organic frame Fe-BTT stays for 4 hours at the target temperature after reaching the target temperature at the heating rate of 5 ℃/min, then is naturally cooled, the black solid powder obtained after calcining treatment is soaked for 24 hours by using 5-20% hydrofluoric acid solution, HF is replaced twice and stirring is carried out continuously, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is obtained. The nano-porous carbon material prepared by the invention still maintains the capacity of up to 99.5 percent after being cycled for 1 ten thousand times under a high-current test of 10A/g, which shows that the material has excellent cycling stability.
Description
Technical Field
The invention belongs to the technical field of preparation of nano porous carbon, and particularly relates to a preparation method of nano porous carbon for a high-performance super capacitor.
Background
The modern society is rapidly developed, the support of energy and power cannot be avoided, and the problems of energy exhaustion, environmental pollution and the like are puzzling people gradually, for example, three fossil energy sources: coal, oil and natural gas, which are the primary energy sources, are used up by human beings, which forces people to continuously explore novel energy sources. On the other hand, effective utilization of new energy sources depends on energy storage equipment, and people urgently need to find advanced energy storage equipment. As the electronics industry has developed, various electronic devices need to provide high capacity, portable backup power sources, and the most promising energy storage devices, in addition to batteries, are now supercapacitors. The super capacitor has various advantages, the research of the super capacitor has become one of hot research projects in the research of the super capacitor by researchers in many countries including China, and the super capacitor has a large application market [2] in the aspects of electric vehicles, electronic products, national defense industry and the like. In the research field of super capacitors, electrode materials and electrolyte are always main factors, and the performance of a super capacitor is greatly dependent on the performance of the electrode materials.
Carbon materials were first applied in electric double layer supercapacitors. The carbon material has the advantages of very high specific surface area, adjustable pore size, good stability, long cycle life, abundant sources, low price and the like, so that the double-electric-layer capacitor using the carbon material as the electrode appears on the market in a large scale. Among them, carbon sources such as activated carbon, graphene, and carbon nanotubes have been studied in many cases. In recent years, research on carbon materials has focused on how to increase the capacitance and energy density by increasing the specific surface area and pore size of the carbon material. However, the carbon material having a high specific surface area does not necessarily have a high capacitance, and is only satisfied within a certain range and limit. The most widely studied carbon material is activated carbon, which is prepared by using some carbon-containing precursors such as: coconut shell, wood, coal and the like are subjected to heat treatment and activation to obtain the coconut shell-wood-coal composite material. Generally, the activation method is chemical activation of physical activation, and different activation methods and pore structures and sizes of the obtained carbon materials are different, which is the key to relate to the size of the capacitance value. In general, the performance of supercapacitors with different carbon materials as electrode materials varies, and researchers are constantly searching for and improving carbon electrode materials.
A Metal-Organic framework (MOFs) is an Organic-inorganic hybrid material which is rapidly developed in the last two decades, and is a porous crystal material which is constructed by a Metal center/Metal cluster and a multidentate Organic ligand in a self-assembly form and has a one-dimensional, two-dimensional or three-dimensional network structure. The diversity of the organic ligands enables the pore channels of the MOFs to have the characteristics of strong chemical modification, size adjustability and the like, so that the MOFs has wide potential application in the fields of fluorescence, sensing, gas adsorption separation, catalysis and the like. In recent years, materials prepared by calcining MOFs serving as templates or precursors under different conditions, such as MOFs-based porous carbon materials, metal oxide and carbon composite materials, metal oxides and the like, have excellent performance in the fields of lithium ion batteries, supercapacitors and the like.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a method for preparing nanoporous carbon for high-performance supercapacitor.
The technical scheme adopted by the invention is as follows:
a preparation method of nanoporous carbon for a high-performance supercapacitor comprises the following steps:
step 1) preparing a precursor nano metal organic frame Fe-BTT, specifically comprising ①, weighing ferrous chloride and 1,3, 5-tetrazole-mesitylene with a molar ratio of (0.5-1.5) to (0.8-1.2), and adding a mixed solvent of an organic solvent N, N-dimethylformamide and water with a molar ratio of (5-8) to (0.5-2);
②, reacting the mixed solution in a microwave reactor for 5 minutes under the condition that the power is 300-600W to obtain light yellow powder;
③, respectively washing the light yellow powder with N, N-dimethylformamide and anhydrous methanol, and drying to obtain a precursor Fe-BTT (nano metal organic framework);
step 2) preparation of the nanoporous carbon, which comprises the following specific steps:
calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600-800 ℃, the temperature is raised to a target temperature at a heating rate of 5 ℃/min, the precursor nano metal organic frame Fe-BTT stays at the target temperature for 4 hours, then the precursor nano metal organic frame Fe-BTT is naturally cooled, black solid powder obtained after calcining treatment is soaked in a hydrofluoric acid solution with the concentration of 5-20% for 24 hours, the hydrofluoric acid solution with the concentration of 5-20% is replaced twice during the process, the stirring is continuously carried out, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is.
In step ①, the molar ratio of ferrous chloride to 1,3, 5-tetrazole-mesitylene is (0.8-1.2): (0.8-1).
In step ①, the molar ratio of ferrous chloride to 1,3, 5-tetrazole-mesitylene is 1: 1.
In step ①, the ratio of N, N-dimethylformamide to water is 6: 1.
In the step 2), the preparation of the nanoporous carbon comprises the following specific steps:
calcining the precursor Fe-BTT of the nano metal organic framework obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600-800 ℃, the temperature is raised to a target temperature at a heating rate of 5 ℃/min, the precursor Fe-BTT stays at the target temperature for 4 hours, then the precursor Fe-BTT is naturally cooled, black solid powder obtained after calcining treatment is soaked in 10% hydrofluoric acid solution for 24 hours, the 10% hydrofluoric acid solution is replaced twice and continuously stirred, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is obtained.
The invention has the following advantages: the nano-porous carbon material prepared by the invention still maintains the capacity of up to 99.5 percent after being cycled for 1 ten thousand times under a high-current test of 10A/g, which shows that the material has excellent cycling stability.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is an SEM image of a precursor nano metal organic framework Fe-BTT in the invention;
FIG. 2 is another SEM image of a precursor nano metal organic framework Fe-BTT in the present invention;
FIG. 3 is a plot of cyclic voltammetry for NC-800 at different scan rates in the present invention;
FIG. 4 is a graph of chronopotentiometric curves for different current densities in accordance with the present invention;
FIG. 5 is a graph of current density at 10A/g cycle life in the present invention.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
Example 1
Referring to fig. 1 to 2, the present invention provides a method for preparing nanoporous carbon for a high-performance supercapacitor, comprising the steps of:
step 1) preparation of a precursor nano metal organic framework Fe-BTT, which comprises the following steps:
①, weighing ferrous chloride and 1,3, 5-tetrazole-mesitylene with the molar ratio of 0.5: 0.8, adding a mixed solvent of an organic solvent N, N-dimethylformamide and water, wherein the ratio of the two solvents is 5: 0.5;
②, reacting the mixed solution in a microwave reactor for 5 minutes under the condition that the power is 300W to obtain light yellow powder;
③, respectively washing the yellowish powder with N, N-dimethylformamide and anhydrous methanol, and drying to obtain a precursor Fe-BTT (nano metal organic framework);
step 2) preparation of the nanoporous carbon, which comprises the following specific steps:
calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600 ℃, after reaching the target temperature at the heating rate of 5 ℃/min, staying for 4h at the target temperature, naturally cooling, soaking black solid powder obtained after calcining treatment for 24h by using 5% hydrofluoric acid solution, replacing HF twice and continuously stirring, and then washing by using a large amount of water until the black solid powder is neutral to obtain the nano porous carbon.
Example 2
Referring to fig. 1 to 2, the present invention provides a method for preparing nanoporous carbon for a high-performance supercapacitor, comprising the steps of:
step 1) preparing a precursor nano metal organic framework Fe-BTT, specifically comprising ①, weighing ferrous chloride and 1,3, 5-tetrazole-mesitylene with a molar ratio of 1: 1, and adding a mixed solvent of an organic solvent N, N-dimethylformamide and water, wherein the ratio of the ferrous chloride to the 1: 1 to the mixed solvent is 6: 1;
②, reacting the mixed solution in a microwave reactor for 5 minutes under the condition that the power is 400W to obtain light yellow powder;
③, respectively washing the yellowish powder with N, N-dimethylformamide and anhydrous methanol, and drying to obtain a precursor Fe-BTT (nano metal organic framework);
step 2) preparation of the nanoporous carbon, which comprises the following specific steps:
calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 700 ℃, the precursor nano metal organic frame Fe-BTT stays for 4 hours at the target temperature after reaching the target temperature at the heating rate of 5 ℃/min, then is naturally cooled, the black solid powder obtained after calcining treatment is soaked for 24 hours by using 10% hydrofluoric acid solution, HF is replaced twice during the soaking process and is continuously stirred, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is obtained.
Example 3
Referring to fig. 1 to 2, the present invention also provides a preparation method of nanoporous carbon for a high-performance supercapacitor, comprising the steps of:
step 1) preparing a precursor nano metal organic framework Fe-BTT, specifically comprising ①, weighing ferrous chloride and 1,3, 5-tetrazole-mesitylene with a molar ratio of 1.5:1.2, and adding a mixed solvent of an organic solvent N, N-dimethylformamide and water, wherein the ratio of the ferrous chloride to the mixed solvent to the water is 8: 2;
②, reacting the mixed solution in a microwave reactor for 5 minutes under the condition that the power is 300-600W to obtain light yellow powder;
③, respectively washing the yellowish powder with N, N-dimethylformamide and anhydrous methanol, and drying to obtain a precursor Fe-BTT (nano metal organic framework);
step 2) preparation of the nanoporous carbon, which comprises the following specific steps:
calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 800 ℃, the precursor nano metal organic frame Fe-BTT stays for 4 hours at the target temperature after reaching the target temperature at the heating rate of 5 ℃/min, then is naturally cooled, the black solid powder obtained after calcining treatment is soaked for 24 hours by using 20% hydrofluoric acid solution, HF is replaced twice during the soaking period and stirring is carried out continuously, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is obtained.
Test example: (3) the preparation and electrochemical performance test of the electrode comprise the following specific experimental steps:
taking the synthesized nano porous carbon, weighing 1mg of carbonized nano porous carbon black powder by using an electronic analytical balance, mixing the carbonized nano porous carbon black powder with 1mL of absolute ethyl alcohol and 10 microliters of binder, performing ultrasonic treatment for 2min to fully mix the mixture, coating the mixture in the range of 1 x 1 cm2 of a stainless steel sheet (current collector) for multiple times, and drying the mixture to prepare the carbon electrode material. And testing the prepared electrode in an electrochemical workstation by using a three-electrode system, using a saturated calomel electrode as a reference electrode, a platinum electrode as a counter electrode and 1mol/L electrolyte of sulfuric acid solution, and respectively performing cyclic voltammetry, timed potential and alternating current impedance tests to obtain relevant data of the electrochemical performance.
According to the invention, organic ligands rich in nitrogen heteroatoms are selected to construct a porous nitrogen-rich metal organic frame-Fe-BTT, and the metal organic frame is calcined at high temperature and acid-washed to remove metal elements to obtain a nitrogen-doped porous carbon material, so that the high-specific-capacity super-electricity material is obtained. As shown in FIG. 3, N-C-800 shows good rectangular shape at different scanning speeds in a voltage window of-0.5V to 0.5V, which shows that the rate capability of the porous nitrogen-doped carbon material is good. In addition, as shown in FIG. 4, the NC-800 material was subjected to chronopotentiometric scanning at different currents, and when the current gradually increased from 1A/g to 30A/g, the capacitance of the NC-800 material still maintained a high specific capacity, which changed from 365F/g to 212F/g, indicating that the material had good rate capability. Meanwhile, the electrode material also has excellent cycling stability, and as shown in FIG. 5, the material still maintains the capacity of 99.5 percent after being cycled for 1 ten thousand times under a high-current test of 10A/g, which shows that the material has excellent cycling stability.
The technical solutions disclosed in the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained in the present document by using specific embodiments, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (5)
1. A preparation method of nanoporous carbon for a high-performance supercapacitor is characterized by comprising the following steps:
step 1) preparing a precursor nano metal organic frame Fe-BTT, specifically comprising ①, weighing ferrous chloride and 1,3, 5-tetrazole-mesitylene with a molar ratio of (0.5-1.5) to (0.8-1.2), and adding a mixed solvent of an organic solvent N, N-dimethylformamide and water with a molar ratio of (5-8) to (0.5-2);
②, reacting the mixed solution in a microwave reactor for 5 minutes under the condition that the power is 300-600W to obtain light yellow powder;
③, respectively washing the light yellow powder with N, N-dimethylformamide and anhydrous methanol, and drying to obtain a precursor Fe-BTT (nano metal organic framework);
step 2) preparation of the nanoporous carbon, which comprises the following specific steps:
calcining the precursor nano metal organic frame Fe-BTT obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600-800 ℃, the temperature is raised to a target temperature at a heating rate of 5 ℃/min, the precursor nano metal organic frame Fe-BTT stays at the target temperature for 4 hours, then the precursor nano metal organic frame Fe-BTT is naturally cooled, black solid powder obtained after calcining treatment is soaked in a hydrofluoric acid solution with the concentration of 5-20% for 24 hours, the hydrofluoric acid solution with the concentration of 5-20% is replaced twice during the process, the stirring is continuously carried out, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is.
2. The method for preparing the nanoporous carbon for the high-performance supercapacitor according to claim 1, wherein in the step ①, the molar ratio of the ferrous chloride to the 1,3, 5-tetrazole-mesitylene is (0.8-1.2): 0.8-1.
3. The preparation method of nanoporous carbon for high-performance supercapacitors as claimed in claim 1 or 2, wherein in step ①, the molar ratio of ferrous chloride and 1,3, 5-tetrazole-mesitylene is 1: 1.
4. The method for preparing nanoporous carbon for high-performance supercapacitors according to claim 1, wherein in step ① the ratio of N, N-dimethylformamide to water is 6: 1.
5. The preparation method of nanoporous carbon for high-performance supercapacitor according to claim 1, wherein in step 2), the specific steps of the preparation of nanoporous carbon are:
calcining the precursor Fe-BTT of the nano metal organic framework obtained in the step 1) in a nitrogen atmosphere, wherein the calcining temperature range is 600-800 ℃, the temperature is raised to a target temperature at a heating rate of 5 ℃/min, the precursor Fe-BTT stays at the target temperature for 4 hours, then the precursor Fe-BTT is naturally cooled, black solid powder obtained after calcining treatment is soaked in 10% hydrofluoric acid solution for 24 hours, the 10% hydrofluoric acid solution is replaced twice and continuously stirred, and then a large amount of water is used for washing until the black solid powder is neutral, so that the nano porous carbon is obtained.
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| CN112592484B (en) * | 2020-11-27 | 2022-07-19 | 江苏科技大学 | MOF material constructed by taking 5-mercapto-1-phenyl-1H-tetrazole as ligand and preparation method and application of derivative thereof |
| CN115331978B (en) * | 2022-09-02 | 2024-07-26 | 河北工业大学 | Preparation method and application of anode-cathode matching material of lithium ion hybrid capacitor |
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