CN109961966B - Preparation method of porous carbon/ferroferric oxide composite electrode material of peanut shell - Google Patents
Preparation method of porous carbon/ferroferric oxide composite electrode material of peanut shell Download PDFInfo
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- CN109961966B CN109961966B CN201711452761.0A CN201711452761A CN109961966B CN 109961966 B CN109961966 B CN 109961966B CN 201711452761 A CN201711452761 A CN 201711452761A CN 109961966 B CN109961966 B CN 109961966B
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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
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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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- 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
- H01G11/84—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
Abstract
The invention discloses a novel preparation method of a peanut shell porous carbon/ferroferric oxide composite electrode material, and introduces application of the peanut shell porous carbon/ferroferric oxide composite electrode material in a supercapacitor electrode. Is prepared from peanut shell (FeKMnO)4The composite material with large specific surface area and excellent performance is prepared by adopting ultrasonic treatment and high-temperature carbonization treatment as raw materials, and the size of the ferroferric oxide nano sheet is 500-700 nm. The nano-sheets grown on the surface of the carbon material not only increase the specific surface area of the material, but also provide a certain pseudocapacitance, thereby greatly increasing the capacitance performance of the material. In addition, the preparation method is simple to operate, environment-friendly, low in cost, easy to control and scale, and capable of recycling domestic wastes and changing wastes into valuables.
Description
Technical Field
The invention relates to a preparation method of a supercapacitor electrode material, in particular to a novel preparation method of a porous carbon composite electrode material based on biomass peanut shells. The method has the advantages of simple operation, low cost, good repeatability and easy control.
Background
With the increase of the demand of human beings on clean and sustainable energy, the electrochemical super capacitor has become one of the main emerging energy storage devices due to the advantages of high power density, long cycle life, safe use and the like. However, low energy density is the most important obstacle to its practical application in the field of energy storage. In order to increase the energy density, many studies are focused on developing new materials with high specific capacitance and asymmetric architectures with wider operating voltage windows.
In the double-layer capacitor electrode material, the carbon material has the characteristics of abundant raw materials, cleanness and environmental protection, so the carbon material is most widely applied, and the production process is mature day by day. Activated carbon is most common in commercial supercapacitors today. However, the activated carbon material itself has a problem that the electrolyte and the electrode material cannot be in sufficient contact with each other due to the uneven distribution of pore sizes. The ideal carbon material should satisfy: the material has the advantages of ultrahigh specific surface area, reasonable pore volume and pore size distribution, good conductivity and wettability, and active substances capable of generating pseudo-capacitance reaction are preferably present on the surface of the material besides the double electric layer capacitance.
China is a big agricultural country and has a large amount of shells and woods every year. The peanut shells are used as daily domestic waste, and if the activated carbon with high electrochemical performance can be prepared by using the peanut shells, the peanut shells have good application value, and waste is changed into valuable. According to the invention, peanut shells are used as raw materials, special high-valence metal ions are introduced by using a potassium ferrate solution, and then the mixture is directly carbonized at high temperature to prepare the porous carbon/ferroferric oxide composite electrode material with excellent performance. By controlling the concentration of the potassium ferrate solution, the shape of the ferroferric oxide nano structure can be adjusted, so that the energy storage performance of the electrode is optimized.
Disclosure of Invention
The purpose of the invention is as follows: the method is characterized in that the method takes biological fiber waste as a raw material, utilizes a strong oxidant potassium ferrate solution to combine with ultrasound to treat peanut shells, introduces special high-valence metal ions into the potassium ferrate, and then directly carries out high-temperature carbonization to prepare the porous carbon/ferroferric oxide composite electrode material with excellent performance. The invention aims to change waste peanut shells in daily life into valuable and ensure that the peanut shells have good application value; the defect of low capacitance of a single carbon material is overcome, and the specific capacitance of the porous carbon/ferroferric oxide composite material is optimized to the greatest extent.
1. The technical scheme of the invention is as follows: cutting peanut shells with clean surfaces and complete structures into pieces, mechanically grinding the peanut shells into powder, adding absolute ethyl alcohol, stirring the mixture uniformly, then ultrasonically dispersing the mixture for 10min, and washing the mixture clean by deionized water; adding a proper amount of peanut shell powder into a potassium ferrate solution with a certain concentration, performing ultrasonic dispersion for 30min, and standing the suspension solution for more than 6 h; repeatedly cleaning the pretreated peanut shell powder by using deionized water, and then putting the peanut shell powder into a vacuum drying oven to be dried at the temperature of 80 ℃; and (3) putting the dried powder into a vacuum tube furnace, heating to a certain temperature within the range of 600-900 ℃ at the speed of 5 ℃/min in an argon atmosphere, and carrying out carbonization treatment for 2h in the constant temperature atmosphere to obtain a final product.
Before the peanut shells are treated, the peanut shells with clean surfaces and complete structures are required to be cut into pieces, mechanically ground into powder, so that the peanut shells are more easily soaked in subsequent treatment, then absolute ethyl alcohol is added, the mixture is stirred uniformly, then ultrasonic dispersion is carried out for 10min, the mixture is washed clean by deionized water, and the dried mixture is dried.
As the best scheme, the concentration range of the peanut shell powder in the potassium ferrate solution is 20 g/L-25 g/L, and the concentration range of the potassium ferrate solution is 1-5M.
As the best scheme, the peanut shell powder suspended and dispersed by the potassium ferrate solution is ultrasonically dispersed for 30min under the power of 100W;
as the best scheme, standing the suspension solution after ultrasonic treatment for more than 6 hours;
as the best scheme, the pretreated peanut shell powder is repeatedly cleaned by deionized water, and then is put into a vacuum drying oven for drying at 80 ℃ for more than 2 hours.
The best proposal is that the dried powder is put into a vacuum tube furnace, heated to a certain temperature within the range of 600-900 ℃ at the speed of 5 ℃/min under the protection of inert gas, and carbonized under the atmosphere of constant temperature for 2 h.
The prepared peanut shell porous carbon/ferroferric oxide can be applied to electrode materials of super capacitors. The composite material based on the biomass activated carbon and the nano metal oxide is prepared for the first time, and has excellent electrochemical performance. Compared with other methods, the preparation method provided by the invention does not need any template, is low in cost, environment-friendly and easy to control and scale.
The invention has the beneficial effects that:
(1) the invention provides a composite material with a biomass porous carbon-supported metal oxide nano structure and a one-step preparation method thereof.
(2) The composite electrode material with the peanut shell porous carbon-supported ferroferric oxide nano structure can be prepared only by surface treatment of strong oxidant, physical means ultrasonic and heat treatment.
(3) Compared with other methods, the preparation method has the following unique advantages:
firstly, the experimental device, experimental conditions and preparation process are very simple and easy to operate;
secondly, the controllability is good, and the shape and the nano structure of the ferroferric oxide are controlled by adjusting the concentration;
the cost is low, and the method has good industrial application prospect;
and fourthly, the applicability is strong, and the preparation method can be popularized to the preparation of other biomass activated carbon/nano metal oxide composite materials.
Drawings
Fig. 1 is a picture of a material preparation process. (a) Raw peanut shells and a peanut shell powder diagram; (b) adding potassium ferrate solution; 2. carrying out ultrasonic reaction for 30 min; 3. drying the product after treatment; 4. and (4) carbonizing to obtain the final product.
FIG. 2 is a SEM and TG picture of the products obtained in examples 1-5. The concentration of the potassium ferrate solution is (a) 1M; (b) 2M; (c) 3M; (d) 4M; (e) 5M; (f) TG picture of products prepared from potassium ferrate solutions with different concentrations
FIG. 3 is an SEM image of the product obtained using a 3M potassium ferrate solution (example 3) at different magnifications.
FIG. 4 is an XRD pattern of electrode materials prepared in examples 1-5.
Fig. 5 is an EDS diagram of the electrode material prepared in example 3.
FIG. 6 is a graph showing the electrochemical performance test of various electrode materials prepared in examples 1 to 5. Preparing CV curves of materials (a) by using potassium ferrate with different concentrations; (b) a CD curve; preparing a CV curve of the material by using the optimized 3M potassium ferrate solution; (d) CD curve.
FIG. 7 is a graph of rate capability of electrode materials prepared in examples 1-5 and a graph of cycling performance of materials prepared with 3M potassium ferrate solution.
Detailed Description
The specific implementation mode of successfully preparing the peanut shell-based porous carbon supercapacitor material loaded with the metal oxide nanostructure by adopting the high-temperature carbonization method is as follows:
example 1
Preparing a peanut shell-based porous active carbon material: cutting peanut shells with clean surfaces and complete structures into pieces, mechanically grinding the peanut shells into powder, adding absolute ethyl alcohol, stirring the mixture uniformly, then ultrasonically dispersing the mixture for 10min under the power of 100W, washing the mixture clean by deionized water, and drying the mixture; adding a proper amount of peanut shell powder into a 1M potassium ferrate solution, and then performing ultrasonic dispersion for 30min in an ultrasonic reactor under the power of 100W; then standing the suspension solution for 6 hours; repeatedly cleaning the pretreated peanut shell powder by using deionized water, and then putting the peanut shell powder into a vacuum drying oven to be dried at the temperature of 80 ℃; and (3) putting the dried powder into a vacuum tube furnace, heating to 800 ℃ at the speed of 5 ℃/min in an argon atmosphere, and carrying out carbonization treatment for 2h in the constant-temperature atmosphere to obtain a final product.
FIG. 1a is a graph of peanut shells and peanut shell powder from the preparation of example 1, the raw peanut shell powder having a yellowish brown color. FIG. 1b is a graph of the process and carbonization products of potassium ferrate-treated peanut hulls during the preparation of example 1, wherein: 1. immediately after the addition of the potassium ferrate solution, the dispersion appeared orange; 2. after 30min of ultrasound treatment, the dispersion liquid is brown yellow; 3. drying the peanut shell powder treated by the potassium ferrate to turn the powder into orange; 4. the carbonized product is black powder.
Example 2
The concentration of potassium ferrate solution was 2M, and the other conditions were the same as in example 1.
Example 3
The potassium ferrate solution was 3M in concentration, and the other conditions were the same as in example 1.
Example 4
The potassium ferrate solution was concentrated at 4M under the same conditions as in example 1.
Example 5
The potassium ferrate solution was 5M in concentration, and the other conditions were the same as in example 1.
As can be seen in FIG. 2, the sheet-like structure or spherical structure is generated on the surface of the carbonized material, and in the cases a to c (examples 1 to 3), the sheet-like structure is gradually increased and densified at low concentration; from d-e (examples 4-5), it can be seen that the concentration continues to increase, spherical structures grow on the carbon surface, the concentration continues to increase, the spherical structures increase, and the spherical structures agglomerate; the thermogram of the products obtained in examples 1-5 is shown as f, the mass ratio of the surface materials is as follows: 5%, 11%, 13.3%, 17%, 19.4%.
FIG. 3 is an SEM image of materials made with the optimized concentration of 3M potassium ferrate solution (example 3) at different magnifications. It can be seen that uniform and compact nano flaky structures grow on the surface of the material, the size of the nano sheet is 500nm-700nm, the flaky structures greatly increase the specific surface area of the material, and the active ferroferric oxide has the pseudocapacitance energy storage characteristic, so that the specific capacitance of the composite material is enhanced.
FIG. 4 is an XRD pattern of materials prepared from different concentrations of potassium ferrate solutions (examples 1-5). It can be seen that there are distinct diffraction characteristic peaks at 43.37 deg., 57.4 deg., 63.1 deg., and no other distinct impurity peaks, indicating that the component of the surface-grown product is Fe3O4。
FIG. 5 is an EDS chart of materials prepared from the optimal concentration of 3M potassium ferrate solution. From these three figures, it can be seen that the distribution of the Fe and O elements on the surface of the material is very uniform, and their atomic ratio is Fe: O43: 56, which is close to 3: 4.
Example 6
After the carbonized product is taken out, acetylene black and PTFE are respectively added according to the proportion of 7: 2: 1, a small amount of ethanol is added, the mixture is uniformly ground in an agate mortar until the mixture is in a film shape, a glass rod is used for pressurizing the mixture, the mixture is cut into a rectangular film with the size of 2cm multiplied by 1cm, and the rectangular film is pressed on foamed nickel; the adopted foam nickel matrix is rectangular, and the size is 2cm multiplied by 1cm, so that the capacitive performance test is facilitated.
FIG. 6a is a plot of cyclic voltammograms of materials obtained from different concentrations of potassium ferrate solutions (examples 1-5) at a scan rate of 10mVs-1. As can be seen from the figure, the CV curves all deviate from the rectangle to some extent, because the pseudo-capacitance behavior exists in the electrode charging and discharging process; at the same scan rate, the CV curve of the carbon material of the peanut shell has the smallest area of enclosure, and the optimal concentration is 3M highThe area enclosed by the CV curve of the material prepared by the potassium ferrite solution is the largest. Compared with a pure peanut shell carbon material, the specific capacitance of the composite material is obviously improved. FIG. 6b is the constant current charge and discharge curve of the material obtained from different concentrations of potassium ferrate solution, the current density is 0.5Ag-1(ii) a The charging and discharging curves are symmetrically distributed in a triangular mode, the slope is basically kept constant, and the material has good capacitance characteristics. It was calculated that the specific capacitance of the composite material prepared in example 3 was the highest at the same current density. FIGS. 6c and 6d are the cyclic voltammetry curve and the charge-discharge curve, respectively, for the optimized composite material at 0.5Ag-1The specific capacitance of the material at the current density was 260F/g.
FIG. 7a is a graph of the rate capability of materials obtained from different concentrations of potassium ferrate solutions (examples 1-5). As seen from the figure, after the potassium ferrate solution is introduced, the overall specific capacitance of the material is greatly improved, and the higher specific capacitance can be maintained under the condition of high current density; fig. 7b is a graph of the cycle performance of the composite material prepared in example 3, and it can be seen that the capacitance of the material is still maintained above 82% after 5000 charge-discharge cycles, indicating that the composite electrode material has good cycle stability.
Claims (5)
1. A preparation method of a porous carbon/ferroferric oxide composite supercapacitor electrode material based on peanut shells is characterized in that the peanut shells with clean surfaces and complete structures are cut into fragments, mechanically ground into powder, added with absolute ethyl alcohol and stirred uniformly, then ultrasonically dispersed for 10min, and washed clean by deionized water; adding a proper amount of peanut shell powder into a potassium ferrate solution with a certain concentration, performing ultrasonic dispersion for 30min, and standing the suspension solution for more than 6 h; repeatedly cleaning the pretreated peanut shell powder by using deionized water, and then putting the peanut shell powder into a vacuum drying oven to be dried at the temperature of 80 ℃; and (3) putting the dried powder into a vacuum tube furnace, heating to a certain temperature within the range of 600-900 ℃ at the speed of 5 ℃/min under the protection of inert gas, and carrying out carbonization treatment for 2h under the constant temperature atmosphere to obtain a final product.
2. The preparation method of claim 1, wherein a proper amount of peanut shell powder is added into the potassium ferrate solution for surface treatment, the concentration range of the peanut shell powder in the solution is 20 g/L-25 g/L, and the concentration range of the potassium ferrate solution is 1-5M.
3. The method according to claim 1, wherein the peanut shell powder dispersed in suspension in the potassium ferrate solution is subjected to ultrasonic dispersion at a power of 100W for 30 min; standing the suspension solution after ultrasonic treatment for more than 6 h.
4. The preparation method of claim 1, wherein the pretreated peanut shell powder is repeatedly washed with deionized water, and then dried in a vacuum drying oven at 80 ℃ for more than 2 hours.
5. The application of the peanut shell porous carbon/ferroferric oxide composite supercapacitor electrode material prepared by the preparation method according to claim 1 in supercapacitor electrode materials.
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