CN111180214A - Bamboo-based porous carbon/manganese dioxide nano composite electrode material for supercapacitor and preparation method thereof - Google Patents
Bamboo-based porous carbon/manganese dioxide nano composite electrode material for supercapacitor and preparation method thereof Download PDFInfo
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- CN111180214A CN111180214A CN201811348924.5A CN201811348924A CN111180214A CN 111180214 A CN111180214 A CN 111180214A CN 201811348924 A CN201811348924 A CN 201811348924A CN 111180214 A CN111180214 A CN 111180214A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/46—Metal oxides
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- 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
Abstract
The invention relates to a bamboo-based porous carbon/manganese dioxide nano composite electrode material for a super capacitor and a preparation method thereof. Selecting moso bamboo as a raw material, processing the moso bamboo into small blocks, drying the small bamboo blocks, putting the small bamboo blocks into an inert atmosphere for high-temperature carbonization, soaking a carbonized product into an alkali metal hydroxide solution, then putting the carbonized product into the inert atmosphere for high-temperature activation, washing the activated product to be neutral, and drying to obtain bamboo-based porous carbon; manganese dioxide nanospheres are generated by taking potassium permanganate and manganese sulfate as raw materials through a low-temperature hydrothermal method and loaded on the surface of the bamboo-based porous carbon, so that the bamboo-based porous carbon/manganese dioxide nanocomposite for the supercapacitor is obtained. The method has the advantages of simple operation, low requirement on equipment and wide raw material source, and the bamboo wood is a renewable green material with biocompatibility and has excellent electrochemical performance when used as the electrode material of the super capacitor.
Description
Technical Field
The invention relates to a preparation method of a bamboo-based porous carbon/manganese dioxide nanocomposite and application of the nanocomposite in a supercapacitor, and belongs to the technical field of electrode materials of supercapacitors.
Background
With the increase of global energy crisis and environmental pollution problems, the development and utilization of new clean energy sources has become one of the important issues facing people. People increasingly have an increasing demand for portable energy storage devices with high energy density, excellent cycle performance, safety and no pollution, and the super capacitor becomes one of the most potential energy storage devices. The super capacitor is also called as a large-capacity capacitor or an electrochemical capacitor, is a novel energy storage device between a battery and a common power supply, has the advantages of ultrahigh power, high charging speed, long service life, excellent low-temperature performance, small leakage current and the like, and is widely applied to the fields of portable electronic equipment, electric automobiles, hybrid power automobiles, industry and military at present. The electrode material is an important component of the super capacitor, and the composition and the structure of the electrode material play an important role in the performance of the super capacitor. The traditional electrode materials of the super capacitor mainly comprise three main categories of porous carbon materials, metal oxides and conducting polymers.
Porous carbon materials, such as activated carbon, graphene, carbon aerogel and the like, are preferred materials for preparing the super capacitor due to the advantages of ultrahigh specific surface area, abundant pore structures, good conductivity, stable charge and discharge performance and the like. Natural biomass materials, such as wood, coconut shells, seaweed, agricultural wastes, and the like, have received considerable attention in the field of energy storage due to the advantages of abundant resources, low cost, simple manufacturing process, environmental friendliness, and the like. Dangbegnon et al reported the use of three-dimensional porous Carbon Derived from Renewable Pine cone biomass for supercapacitor electrode Materials (Renewable Pine cone biomass Derived Carbon Materials for supercapacitor application. RSC adv.2016, 6, 1800-1809). However, although electric double layer capacitors based on porous carbon electrodes are available, their energy density is limited and, therefore, more attention and expectations have been given to hybrid electrodes combining electric double layers and pseudocapacitance.
MnO2As a pseudocapacitance material, the material has higher theoretical capacitance (-1370F g)-1) Cost-effectiveness and environmental friendliness are considered as potential supercapacitor electrode Materials, however, the poor conductivity of MnO2 limits its application as electrode material (mangase Oxide-Based Materials as Electrochemical supercapacitor electrodes. chem. soc. rev. 2011, 40, 1697-1721). Therefore, when the pseudocapacitance material is added into the three-dimensional conductive carbon carrier, the synergistic effect between the electrode materials is beneficial to the transfer of electronic charges, and higher electrochemical capacity is provided.
Therefore, there is a need to develop a method for preparing a three-dimensional porous carbon/pseudocapacitance composite material from a biomass precursor so as to solve the problems of high cost, environmental pollution, single product structure, low capacitance performance and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the bamboo-based porous carbon is obtained by taking biomass bamboo as a precursor and performing high-temperature carbonization and activation with alkali metal hydroxide; the bamboo-based porous carbon loaded with manganese dioxide nanospheres is obtained by combining a low-temperature hydrothermal method with a manganese source and is used as an electrode material of a super capacitor. The technical scheme adopted by the invention is as follows: a preparation method of a bamboo-based porous carbon/manganese dioxide nanocomposite comprises the following specific steps:
1. processing bamboo into small blocks, cleaning to remove impurities, and drying;
2. placing the bamboo blocks dried in the step 1 in an inert atmosphere for high-temperature carbonization;
3. soaking the carbonized product obtained in the step (2) in a potassium hydroxide solution at a certain temperature for a certain time, then placing the soaked product in an inert atmosphere for high-temperature activation, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon;
4. adding the bamboo-based porous carbon obtained in the step (3) into a potassium permanganate/manganese sulfate mixed solution with a certain concentration, placing the mixture into a high-pressure reaction kettle, and reacting for several hours at a certain temperature;
5. and (4) centrifugally washing the product cooled in the step (4) to be neutral, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite for the super capacitor.
The bamboo-based porous carbon/manganese dioxide nanocomposite prepared by the method has the advantages of easily available raw materials, wide sources, good biocompatibility and simple synthesis process. The bamboo-based porous carbon in the prepared composite material has a large number of pore structures and good conductivity, and can provide a double electric layer effect for a super capacitor; the manganese dioxide nanospheres have higher theoretical specific capacity and can provide a pseudocapacitance effect for the super capacitor. The composite material can effectively improve the performance of the electrode material of the super capacitor.
Drawings
Fig. 1 is a scanned image of the bamboo-based porous carbon prepared in example 1.
Fig. 2 is a scanned image of the bamboo-based porous carbon/manganese dioxide nanocomposite prepared in example 1.
Fig. 3 is a scanned image of the bamboo-based porous carbon/manganese dioxide nanocomposite prepared in example 4.
Fig. 4 is a constant current charge-discharge curve of the bamboo-based porous carbon and the bamboo-based porous carbon/manganese dioxide nanocomposite prepared in example 1.
Fig. 5 is a graph showing rate capability of the bamboo-based porous carbon/manganese dioxide nanocomposite prepared in example 1.
Detailed Description
The present invention will be further described below by way of examples, but the present invention is not limited thereto.
Example 1
Processing bamboo into small blocks, cleaning to remove impurities, drying, placing about 2 g of small bamboo blocks in a boat-shaped crucible, and carbonizing in a tube furnace under nitrogen atmosphere at a temperature rise rate of 5 ℃/min and a carbonization temperature of 800 ℃ for 120 min. Mixing the carbonized product with a potassium hydroxide solution, wherein the alkali-carbon ratio is 1: and 4, soaking at 90 ℃ for 5h, then placing in a nickel crucible, performing high-temperature activation in a nitrogen atmosphere at the heating rate of 5 ℃/min, the activation temperature of 800 ℃ and the activation time of 120min, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon. Soaking the bamboo-based porous carbon in a solution with a molar ratio of 1: 3, placing the potassium permanganate/manganese sulfate solution in a high-pressure reaction kettle, heating to 150 ℃, reacting for 24 hours, naturally cooling the product to room temperature, centrifugally washing to neutrality, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite.
Observing the obtained bamboo-based porous carbon by scanning electron microscope, as shown in figure 1, allowing a large number of pores to exist in the original structure of bamboo, and subjecting the bamboo-based porous carbon to N treatment2The specific surface area of the adsorption-desorption isothermal test is 2857 m2g-1. The obtained bamboo-based porous carbon/manganese dioxide nanocomposite is observed by a scanning electron microscope, as shown in fig. 2, wherein the diameter distribution of the manganese dioxide nanospheres is 0.25-1.25 μm, the surfaces of the nanospheres are rough, and the nanospheres have more pores. The electrochemical performance test results are shown in FIGS. 4-5 and are at 0.1A g-1The charging and discharging curve of the bamboo-based porous carbon is in an isosceles triangle shape under the current density, the typical double electric layer effect is achieved, the charging and discharging curve of the bamboo-based porous carbon/manganese dioxide composite material can reflect the obvious pseudo-capacitance effect, and the pseudo-capacitance effect is 0.1A g in the rate performance test-1Has a specific discharge capacity of 387F g-1And has better capacity retention rate.
Example 2
Processing bamboo into small blocks, cleaning to remove impurities, drying, placing about 2 g of small bamboo blocks in a boat-shaped crucible, and carbonizing in a tube furnace under nitrogen atmosphere at a temperature rise rate of 5 ℃/min and a carbonization temperature of 800 ℃ for 120 min. Mixing the carbonized product with a potassium hydroxide solution, wherein the alkali-carbon ratio is 1: 2, soaking at 90 ℃ for 5h, then placing in a nickel crucible, performing high-temperature activation in a nitrogen atmosphere at a heating rate of 5 ℃/min, an activation temperature of 800 ℃ and an activation time of 120min, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon. Soaking the bamboo-based porous carbon in a solution with a molar ratio of 1: 3, placing the potassium permanganate/manganese sulfate solution in a high-pressure reaction kettle, heating to 150 ℃, reacting for 24 hours, naturally cooling the product to room temperature, centrifugally washing to neutrality, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite.
Subjecting the obtained bamboo-based porous carbon to N2Adsorption-desorption isothermal test, the specific surface area is 1404 m2g-1The alkali content reduction activation was insufficient.
Example 3
Processing bamboo into small blocks, cleaning to remove impurities, drying, placing about 2 g of small bamboo blocks in a boat-shaped crucible, and carbonizing in a tube furnace under nitrogen atmosphere at a temperature rise rate of 5 ℃/min and a carbonization temperature of 800 ℃ for 120 min. Mixing the carbonized product with a potassium hydroxide solution, wherein the alkali-carbon ratio is 1: and 4, soaking at 90 ℃ for 5h, then placing in a nickel crucible, performing high-temperature activation in a nitrogen atmosphere at the heating rate of 5 ℃/min, the activation temperature of 700 ℃, the activation time of 120min, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon. Soaking the bamboo-based porous carbon in a solution with a molar ratio of 1: 3, placing the potassium permanganate/manganese sulfate solution in a high-pressure reaction kettle, heating to 150 ℃, reacting for 24 hours, naturally cooling the product to room temperature, centrifugally washing to neutrality, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite.
The obtained bamboo-based porous carbon/manganese dioxide nanocomposite is observed by a scanning electron microscope, so that the bamboo-based porous carbon has a smooth surface and a small amount of manganese dioxide attached.
Example 4
Processing bamboo into small blocks, cleaning to remove impurities, drying, placing about 2 g of small bamboo blocks in a boat-shaped crucible, and carbonizing in a tube furnace under nitrogen atmosphere at a temperature rise rate of 5 ℃/min and a carbonization temperature of 800 ℃ for 120 min. Mixing the carbonized product with a potassium hydroxide solution, wherein the alkali-carbon ratio is 1: and 4, soaking at 90 ℃ for 5h, then placing in a nickel crucible, performing high-temperature activation in a nitrogen atmosphere at the heating rate of 5 ℃/min, the activation temperature of 800 ℃ and the activation time of 120min, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon. Soaking the bamboo-based porous carbon in a solution with a molar ratio of 1: 6, placing the potassium permanganate/manganese sulfate solution in a high-pressure reaction kettle, heating to 150 ℃, reacting for 24 hours, naturally cooling the product to room temperature, centrifugally washing to neutrality, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite.
The obtained bamboo-based porous carbon/manganese dioxide nanocomposite is observed by a scanning electron microscope, as shown in fig. 3, wherein the diameter distribution of the manganese dioxide nanospheres is 1.5-2.5 μm, and the surface has pores but is smooth. In the rate capability test, 0.1A g-1Current density of 312F g-1。
Example 5
Processing bamboo into small blocks, cleaning to remove impurities, drying, placing about 2 g of small bamboo blocks in a boat-shaped crucible, and carbonizing in a tube furnace under nitrogen atmosphere at a temperature rise rate of 5 ℃/min and a carbonization temperature of 800 ℃ for 120 min. Mixing the carbonized product with a potassium hydroxide solution, wherein the alkali-carbon ratio is 1: and 4, soaking at 90 ℃ for 5h, then placing in a nickel crucible, performing high-temperature activation in a nitrogen atmosphere at the heating rate of 5 ℃/min, the activation temperature of 800 ℃ and the activation time of 120min, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon. Soaking the bamboo-based porous carbon in a solution with a molar ratio of 1: 3, placing the potassium permanganate/manganese sulfate solution in a high-pressure reaction kettle, heating to 180 ℃ for reaction for 24 hours, naturally cooling the product to room temperature, centrifugally washing to neutrality, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite.
The sphere diameter distribution of manganese dioxide in the obtained composite material is 0.5-3 mu m, the distribution is wide, and the surface is rough. In the rate capability test, 0.1A g-1Current density of 296F g-1
Although some embodiments of the present invention have been described in detail, the present invention is not limited to the above-described embodiments, and those skilled in the art can make equivalent modifications or substitutions without departing from the spirit of the present invention, and such equivalent modifications or substitutions are included in the scope of the present invention defined by the claims.
Claims (7)
1. A bamboo-based porous carbon/manganese dioxide nano composite electrode material for a supercapacitor and a preparation method thereof are characterized by comprising the following steps:
(1) processing bamboo into small blocks, cleaning to remove impurities, and drying;
(2) placing the dried bamboo blocks in the step (1) in an inert atmosphere for high-temperature carbonization;
(3) soaking the carbonized product obtained in the step (2) in a potassium hydroxide solution at a certain temperature, placing the soaked product in an inert atmosphere for high-temperature activation after certain time of soaking, washing the activated product to be neutral, and drying to obtain the bamboo-based porous carbon;
(4) adding the bamboo-based porous carbon obtained in the step (3) into a potassium permanganate/manganese sulfate mixed solution with a certain concentration, placing the mixture into a high-pressure reaction kettle, and reacting for several hours at a certain temperature;
(5) and (4) centrifugally washing the product cooled in the step (4) to be neutral, and drying to obtain the bamboo-based porous carbon/manganese dioxide nanocomposite material for the super capacitor.
2. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1 are characterized in that: the bamboo material is annual moso bamboo which grows normally and has no plant diseases and insect pests.
3. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1, characterized in that the inert atmosphere in the step (2) is nitrogen or argon, the carbonization temperature is 700-1000 ℃, the activation time is 60-180 min, and the heating rate is 5-10 ℃/min.
4. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1, wherein in the step (3), the ratio of alkali to carbon is 1: 1-1: 4, soaking for 1-5 h at 90 ℃.
5. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1, characterized in that the inert atmosphere in the step (3) is nitrogen or argon, the activation temperature is 700-800 ℃, the carbonization time is 60-180 min, and the temperature rise rate is 5-10 ℃/min.
6. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1, wherein the ratio of the mixed solution of potassium permanganate and manganese sulfate in step (4) is potassium permanganate/manganese sulfate = 1: 1-1: 6, molar ratio.
7. The bamboo-based porous carbon/manganese dioxide nanocomposite electrode material for the supercapacitor and the preparation method thereof according to claim 1 are characterized in that the reaction temperature of a high-pressure reaction kettle in the step (4) is 120-180 ℃, and the reaction time is 12-48 h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174136A (en) * | 2020-08-20 | 2021-01-05 | 浙江大学 | High-nitrogen biochar composite material and preparation method and application thereof |
| CN112447417A (en) * | 2020-11-10 | 2021-03-05 | 同济大学 | Manganese dioxide-loaded pine cone electrode material, and preparation method and application thereof |
| CN112927954A (en) * | 2021-01-25 | 2021-06-08 | 北华大学 | Method for preparing carbon electrode material by constructing wood pore structure based on fungus method |
| CN112951618A (en) * | 2021-01-29 | 2021-06-11 | 中国矿业大学 | Biomass-based activated carbon loaded CuO nano-particle composite material and application thereof |
| CN114890453A (en) * | 2022-06-10 | 2022-08-12 | 南京林业大学 | Method for preparing self-supporting electrode by using MXene modified carbonized wood/metal oxide composite |
| WO2024000175A1 (en) * | 2022-06-28 | 2024-01-04 | 皖西学院 | Preparation method for porous carbon and manganese dioxide composite supercapacitor electrode material |
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| CN103594254A (en) * | 2013-11-26 | 2014-02-19 | 华东理工大学 | Method for preparing manganese dioxide/mesoporous carbon nanometer graded composite electrode material |
| CN106145283A (en) * | 2015-04-02 | 2016-11-23 | 北京化工大学 | The bamboo matrix activated carbon being applied in capacitance method desalting technology and material modified preparation thereof and test |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112174136A (en) * | 2020-08-20 | 2021-01-05 | 浙江大学 | High-nitrogen biochar composite material and preparation method and application thereof |
| CN112174136B (en) * | 2020-08-20 | 2022-12-02 | 浙江大学 | High-nitrogen biochar composite material and preparation method and application thereof |
| CN112447417A (en) * | 2020-11-10 | 2021-03-05 | 同济大学 | Manganese dioxide-loaded pine cone electrode material, and preparation method and application thereof |
| CN112927954A (en) * | 2021-01-25 | 2021-06-08 | 北华大学 | Method for preparing carbon electrode material by constructing wood pore structure based on fungus method |
| CN112951618A (en) * | 2021-01-29 | 2021-06-11 | 中国矿业大学 | Biomass-based activated carbon loaded CuO nano-particle composite material and application thereof |
| CN114890453A (en) * | 2022-06-10 | 2022-08-12 | 南京林业大学 | Method for preparing self-supporting electrode by using MXene modified carbonized wood/metal oxide composite |
| WO2024000175A1 (en) * | 2022-06-28 | 2024-01-04 | 皖西学院 | Preparation method for porous carbon and manganese dioxide composite supercapacitor electrode material |
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Application publication date: 20200519 |