CN109920654B - Preparation method of graphene/carbon nanosheet electrode - Google Patents
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Abstract
The invention belongs to the field of preparation of electrode materials, and particularly relates to a preparation method of a graphene/carbon nanosheet electrode, which comprises the steps of dissolving graphene oxide and foamed nickel in methanol, carrying out ultrasonic treatment, standing for multiple times, and drying to obtain the foamed nickel with pre-loaded graphene oxide; placing the mixture into a methanol solution containing graphene oxide and 4, 4' -biphenyl diboronic acid, and reacting for 24 hours at 90 ℃; washing with methanol, drying and weighing; washing with trimethylbenzene and dioxane solution, directly dispersing in the trimethylbenzene and dioxane solution, adding 1, 4-benzene diboronic acid, reacting at 120 ℃ for 72h, washing with acetone, drying and weighing; calcining at 600 ℃ under the protection of molten salt, washing for a plurality of times in a deionized water bath, and drying in vacuum to obtain the electrode. The graphene/carbon nanosheet electrode prepared by the method has the advantage of large specific surface area, is good in stability in an electrochemical test, and can be further loaded with a pseudocapacitance substance to obtain a supercapacitor electrode with higher specific capacitance.
Description
Technical Field
The invention belongs to the field of preparation of electrode materials, and particularly relates to a preparation method of a graphene/carbon nanosheet electrode.
Background
In the modern society, energy and environment are the common concerns of human beings, and the development of novel energy storage devices is urgent. The super capacitor is a green energy storage device with fast charge and discharge, high power density and long cycle time, and has received extensive attention of researchers. The graphene has great potential in the application of super capacitor electrodes due to excellent conductivity and extremely excellent charge storage capacity brought by a relatively large theoretical specific surface area, and the research of the graphene super capacitor becomes a hot spot of domestic and foreign research. The graphene composite material is an important research direction of graphene in the application of the energy field, and the graphene is compounded with other materials, so that the performance of the material is improved, and the application range of the material is expanded.
Covalent Organic Framework (COFs) materials have high specific surface area and low framework density, and have permanently open pore channel structures capable of synthesizing diversification, for example, two-dimensional COFs materials such as COF-1 and the like have porous graphite laminated structures, so that the COFs have wide application in the field of energy.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene/carbon nanosheet electrode. The super capacitor electrode with excellent double electric layer capacitance is prepared by combining the advantages of excellent graphene conductivity and charge storage capacity with the advantages of high specific surface area and open pore channels of the covalent organic framework material, and the preparation is made for further preparing the composite electrode loaded with pseudo-capacitance substances.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphene/carbon nanosheet electrode specifically comprises the following steps:
(1) preparing graphene oxide by adopting a modified Hummers method;
(2) pre-loading graphene oxide on the foamed nickel: dissolving the graphene oxide obtained in the step (1) in methanol to prepare a methanol solution of the graphene oxide, immersing the solution in foamed nickel, performing ultrasonic treatment for 1 hour, standing for 2 hours, drying at 60 ℃, standing for multiple times and drying to improve the loading capacity of the graphene oxide on the foamed nickel;
(3) placing the foamed nickel pre-loaded with graphene oxide obtained in the step (2) and 80 mg of graphene oxide in 16 mL of methanol, standing for 12h, adding 4, 4' -biphenyl diboronic acid, performing ultrasonic treatment for 2h, transferring the solution to a reaction kettle, and adding N2Sealing, reacting at 90 deg.C for 24 hr, centrifuging the product with methanol, washing, vacuum drying at 60 deg.C, and weighing;
(4) washing the product prepared in the step (3) with trimethylbenzene and dioxane solution, directly soaking the product in 16 mL of trimethylbenzene and dioxane solution without drying, adding 1, 4-benzene diboronic acid, transferring the solution to a reaction kettle, and adding N2Sealing, reacting at 120 deg.C for 72h, washing the product with acetone, vacuum drying at 60 deg.C, and weighing;
(5) vacuum drying the product obtained in step (4) at 220 ℃ for 4 h, and ZnCl2Mixing with acetone solution, soaking for 12 hr, centrifuging to remove acetone, vacuum drying at 60 deg.C, transferring to crucible, and heating to 600 deg.C N2And calcining for 3 hours. Soaking the obtained product in deionized water, performing water bath at 70 deg.C, vacuum filtering, repeating for several times, and vacuum drying at 60 deg.C to obtain the electrode.
The preparation method of the graphene oxide in the step (1) comprises the following steps: adding 3 g of graphite into a mixed acid of 360 mL of concentrated sulfuric acid and 40 mL of phosphoric acid, stirring in an ice bath at 0 ℃, slowly adding 18 g of potassium permanganate into 4 batches of the mixed acid within 3 hours, keeping the temperature below 35 ℃, heating to 50 ℃, stirring for 12 hours, cooling to room temperature, slowly adding 400 mL of ice water, slowly dropwise adding 30vol% of hydrogen peroxide until the solution turns into golden yellow, adding 100 mL of 5vol% of hydrochloric acid, standing overnight, removing supernatant, centrifugally washing the precipitate with deionized water to be neutral, and freeze-drying to obtain the graphene oxide.
The concentration of the methanol solution of the graphene oxide in the step (2) is 1-5 mg/mL.
The mass ratio of the 4, 4' -biphenyl diboronic acid to the total amount of the graphene oxide in the step (3) is 0.5-5: 1.
The volume ratio of the trimethylbenzene to the dioxane in the trimethylbenzene and dioxane solution in the step (4) is 1: 1.
In the step (4), the mass ratio of the 1, 4-phenyl diboronic acid to the total amount of the graphene oxide modified by the 4, 4' -biphenyl diboronic acid is 0.5-5: 1.
ZnCl described in step (5)2ZnCl with acetone solution2The mass ratio to acetone was 1: 15.
The experimental mechanism is as follows: an OH group on the graphene oxide is connected with a 4,4 '-biphenyl diboronic acid monomer molecule through a chemical bond, and a boric acid group at the other end of the 4, 4' -biphenyl diboronic acid monomer molecule is continuously connected with a 1, 4-benzene diboronic acid monomer; and the 1, 4-phenyl diboronic acid monomers are subjected to dehydration condensation and are connected by chemical bonds to form the COFs material. And calcining the composite material of the graphene oxide and the COFs to obtain the graphene/carbon nano sheet composite material. The reaction equation involved is shown in FIG. 4.
The invention has the beneficial effects that:
(1) the carbon nanosheets compounded with the graphene prevent the graphene from overlapping, the spacing between graphene layers is increased, and the specific surface area of the composite material is increased, so that the pseudo capacitance of the electrode material is improved;
(2) the graphene/carbon nanosheet electrode prepared by the method is good in stability and can be used as a supercapacitor electrode for further loading pseudo-capacitance substances;
(3) the electrode material prepared by the invention directly loads the pseudocapacitance substance on the foamed nickel without using acetylene black and a binder.
Drawings
FIG. 1 is an XRD pattern of a material support prepared in example 1 of the present invention at each reaction stage;
FIG. 2 is a scanning electron micrograph of a material prepared according to example 1 of the present invention;
FIG. 3 is an electrochemical cycling stability of the material prepared in example 1 of the present invention;
FIG. 4 shows the chemical reaction scheme of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
A preparation method of a graphene/carbon nanosheet electrode comprises the following specific steps:
(1) preparing graphene oxide by adopting a modified Hummers method: adding 3 g of graphite into a mixed acid of 360 mL of concentrated sulfuric acid and 40 mL of phosphoric acid, stirring in an ice bath at 0 ℃, slowly adding 18 g of potassium permanganate in 4 batches (within 3 h), keeping the temperature below 35 ℃, heating to 50 ℃, stirring for 12h, cooling to room temperature, slowly adding 400 mL of ice water, slowly dropwise adding 30vol% of hydrogen peroxide until the solution turns into golden yellow, adding 100 mL of 5vol% of hydrochloric acid, standing overnight, removing supernatant, centrifugally washing the precipitate with deionized water to be neutral, and freeze-drying to obtain graphene oxide;
(2) pre-loading graphene oxide on the foamed nickel: dissolving 60 mg of the graphene oxide obtained in the step (1) in 30 mL of methanol to prepare a methanol solution (2 mg/mL) of the graphene oxide, immersing the graphene oxide in foamed nickel, performing ultrasonic treatment for 1 h, standing for 2h, drying at 60 ℃, standing and drying for 3 times in total to improve the loading capacity of the graphene oxide on the foamed nickel;
(3) placing the nickel foam pre-loaded with graphene oxide obtained in the step (2) and 80 mg of graphene oxide in 16 mL of methanol, and standing12h, adding 4,4 '-biphenyl diboronic acid (the mass ratio of the 4, 4' -biphenyl diboronic acid to the total amount of the graphene oxide is 3: 1), carrying out ultrasonic treatment for 2h, transferring the solution to a reaction kettle, and carrying out N2Sealing, reacting at 90 deg.C for 24 hr, centrifuging and washing the product with methanol, and vacuum drying at 60 deg.C;
(4) washing the product prepared in the step (3) by using a trimethylbenzene and dioxane solution (the volume ratio is 1: 1), directly soaking the product in 16 mL of the trimethylbenzene and dioxane solution (the volume ratio is 1: 1) without drying, adding 1, 4-benzene diboronic acid (the mass ratio of the 1, 4-benzene diboronic acid to the total amount of the 4, 4' -biphenyl diboronic acid modified graphene oxide is 5: 1), transferring the solution to a reaction kettle, and transferring N2Sealing, reacting at 120 deg.C for 72h, washing the product with acetone, vacuum drying at 60 deg.C, and weighing;
(5) vacuum drying the product obtained in step (4) at 220 ℃ for 4 h, and ZnCl2With acetone solution (ZnCl)2Mixing with acetone at a mass ratio of 1: 15), soaking for 12 hr, centrifuging to remove acetone, vacuum drying at 60 deg.C, transferring to crucible, and heating to 600 deg.C under N2And calcining for 3 hours. Soaking the obtained product in deionized water, performing water bath at 70 deg.C, vacuum filtering, repeating for several times, and vacuum drying at 60 deg.C to obtain the electrode.
Example 2
A preparation method of a graphene/carbon nanosheet electrode comprises the following specific steps:
(1) preparing graphene oxide by adopting a modified Hummers method: adding 3 g of graphite into a mixed acid of 360 mL of concentrated sulfuric acid and 40 mL of phosphoric acid, stirring in an ice bath at 0 ℃, slowly adding 18 g of potassium permanganate into the mixed acid in 4 batches (within 3 h), keeping the temperature below 35 ℃, heating to 50 ℃, stirring for 12h, cooling to room temperature, slowly adding 400 mL of ice water, slowly dropwise adding 30vol% of hydrogen peroxide until the solution turns into golden yellow, adding 100 mL of 5vol% of hydrochloric acid, standing overnight, removing supernatant, centrifugally washing the precipitate with deionized water to be neutral, and freeze-drying to obtain the graphene oxide.
(2) Pre-loading graphene oxide on the foamed nickel: dissolving 60 mg of the graphene oxide obtained in the step (1) in 30 mL of methanol to prepare a methanol solution (2 mg/mL) of the graphene oxide, immersing the graphene oxide in foamed nickel, performing ultrasonic treatment for 1 h, standing for 2h, drying at 60 ℃, standing and drying for 3 times in total to improve the loading capacity of the graphene oxide on the foamed nickel;
(3) placing the foamed nickel pre-loaded with graphene oxide obtained in the step (2) and 80 mg of graphene oxide in 16 mL of methanol, standing for 12h, adding 4,4 '-biphenyl diboronic acid (the mass ratio of 4, 4' -biphenyl diboronic acid to the total amount of the graphene oxide is 3: 1), carrying out ultrasonic treatment for 2h, transferring the solution to a reaction kettle, and carrying out N2Sealing, reacting at 90 deg.C for 24 hr, centrifuging and washing the product with methanol, and vacuum drying at 60 deg.C;
(4) washing the product prepared in the step (3) by using a trimethylbenzene and dioxane solution (the volume ratio is 1: 1), directly soaking the product in 16 mL of the trimethylbenzene and dioxane solution (the volume ratio is 1: 1) without drying, adding 1, 4-benzene diboronic acid (the mass ratio of the 1, 4-benzene diboronic acid to the total amount of the 4, 4' -biphenyl diboronic acid modified graphene oxide is 3: 1), transferring the solution to a reaction kettle, and transferring N2Sealing, reacting at 120 deg.C for 72h, washing the product with acetone, vacuum drying at 60 deg.C, and weighing;
(5) vacuum drying the product obtained in step (4) at 220 ℃ for 4 h, and ZnCl2With acetone solution (ZnCl)2Mixing with acetone at a mass ratio of 1: 15), soaking for 12 hr, centrifuging to remove acetone, vacuum drying at 60 deg.C, transferring to crucible, and heating to 600 deg.C under N2And calcining for 3 hours. Soaking the obtained product in deionized water, performing water bath at 70 deg.C, vacuum filtering, repeating for several times, and vacuum drying at 60 deg.C to obtain the electrode.
Example 3
A preparation method of a graphene/carbon nanosheet electrode comprises the following specific steps:
(1) preparing graphene oxide by adopting a modified Hummers method: adding 3 g of graphite into a mixed acid of 360 mL of concentrated sulfuric acid and 40 mL of phosphoric acid, stirring in an ice bath at 0 ℃, slowly adding 18 g of potassium permanganate into the mixed acid in 4 batches (within 3 h), keeping the temperature below 35 ℃, heating to 50 ℃, stirring for 12h, cooling to room temperature, slowly adding 400 mL of ice water, slowly dropwise adding 30vol% of hydrogen peroxide until the solution turns into golden yellow, adding 100 mL of 5vol% of hydrochloric acid, standing overnight, removing supernatant, centrifugally washing the precipitate with deionized water to be neutral, and freeze-drying to obtain the graphene oxide.
(2) Pre-loading graphene oxide on the foamed nickel: dissolving 60 mg of the graphene oxide obtained in the step (1) in 30 mL of methanol to prepare a methanol solution (2 mg/mL) of the graphene oxide, immersing the graphene oxide in foamed nickel, performing ultrasonic treatment for 1 h, standing for 2h, drying at 60 ℃, standing and drying for 3 times in total to improve the loading capacity of the graphene oxide on the foamed nickel;
(3) placing the foamed nickel pre-loaded with graphene oxide obtained in the step (2) and 80 mg of graphene oxide in 16 mL of methanol, standing for 12h, adding 4,4 '-biphenyl diboronic acid (the mass ratio of 4, 4' -biphenyl diboronic acid to the total amount of the graphene oxide is 5: 1), performing ultrasonic treatment for 2h, transferring the solution to a reaction kettle, and carrying out N2Sealing, reacting at 90 deg.C for 24 hr, centrifuging and washing the product with methanol, and vacuum drying at 60 deg.C;
(4) washing the product prepared in the step (3) by using a trimethylbenzene and dioxane solution (the volume ratio is 1: 1), directly soaking the product in 16 mL of the trimethylbenzene and dioxane solution (the volume ratio is 1: 1) without drying, adding 1, 4-benzene diboronic acid (the mass ratio of the 1, 4-benzene diboronic acid to the total amount of the 4, 4' -biphenyl diboronic acid modified graphene oxide is 5: 1), transferring the solution to a reaction kettle, and transferring N2Sealing, reacting at 120 deg.C for 72h, washing the product with acetone, vacuum drying at 60 deg.C, and weighing;
(5) vacuum drying the product obtained in step (4) at 220 ℃ for 4 h, and ZnCl2With acetone solution (ZnCl)2Mixing with acetone at a mass ratio of 1: 15), soaking for 12 hr, centrifuging to remove acetone, vacuum drying at 60 deg.C, transferring to crucible, and heating to 600 deg.C under N2And calcining for 3 hours. Soaking the obtained product in deionized water, performing water bath at 70 deg.C, vacuum filtering, repeating for several times, and vacuum drying at 60 deg.C to obtain the electrode.
The obtained electrode was subjected to electrochemical performance test, and the results are shown in table 1.
TABLE 1 electrochemical Performance and specific surface area of graphene/carbon nanoplate electrodes
In FIG. 1, b is an XRD spectrum of GO; c is an XRD spectrogram of 4,4 '-biphenyl diboronic acid connected to GO, compared with GO, the peak position of the XRD spectrogram is shifted to the left, which shows that the interlayer spacing of GO is increased after 4, 4' -biphenyl diboronic acid is connected to GO; d is an XRD spectrum of the COFs grown continuously, and a series of peak positions of the COFs appear (the crystal plane indexes are (100) (110) (200) (101) (201) (211) (002) (112) from left to right), which indicates that the COFs are grown successfully; a is a spectrogram after calcination, only the peak position of graphene appears, and the successful thermal reduction of GO and COFs is demonstrated;
fig. 2 illustrates that the electrode has been uniformly coated with a graphene composite;
FIG. 3 illustrates that the electrode has better electrochemical cycling stability;
FIG. 4 is a reaction equation involved in the present invention.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of a graphene/carbon nanosheet electrode is characterized by comprising the following steps: dissolving graphene oxide and foamed nickel in methanol, performing ultrasonic treatment, standing for multiple times, and drying to obtain the foamed nickel pre-loaded with graphene oxide; placing the mixture into a methanol solution containing graphene oxide and 4, 4' -biphenyl diboronic acid for reaction; washing with methanol and drying; washing with trimethylbenzene and dioxane solution, directly dispersing in the trimethylbenzene and dioxane solution, adding 1, 4-benzene diboronic acid for reaction, washing with acetone, drying, calcining under the protection of molten salt, washing with deionized water bath for several times, and drying in vacuum to obtain an electrode; the method specifically comprises the following steps:
(1) preparing graphene oxide by adopting a modified Hummers method;
(2) pre-loading graphene oxide on the foamed nickel: dissolving the graphene oxide obtained in the step (1) in methanol to prepare a methanol solution of the graphene oxide, immersing the solution in foamed nickel, performing ultrasonic treatment for 1 hour, standing for 2 hours, drying at 60 ℃, standing for multiple times and drying to improve the loading capacity of the graphene oxide on the foamed nickel;
(3) pre-treating the mixture obtained in the step (2)Placing foamed nickel loaded with graphene oxide and 80 mg of graphene oxide in 16 mL of methanol, standing for 12h, adding 4, 4' -biphenyl diboronic acid, performing ultrasonic treatment for 2h, transferring the solution to a reaction kettle, and performing N2Sealing, reacting at 90 deg.C for 24 hr, centrifuging the product with methanol, washing, vacuum drying at 60 deg.C, and weighing;
(4) washing the product prepared in the step (3) with trimethylbenzene and dioxane solution, directly soaking the product in 16 mL of trimethylbenzene and dioxane solution without drying, adding 1, 4-benzene diboronic acid, transferring the solution to a reaction kettle, and adding N2Sealing and reacting, washing the product with acetone, vacuum drying at 60 ℃, and weighing;
(5) vacuum drying the product obtained in step (4) at 220 ℃ for 4 h, and ZnCl2Mixing with acetone solution, soaking for 12h, centrifuging to remove acetone, vacuum drying at 60 deg.C, and transferring to crucible for calcining; soaking the obtained product in deionized water, performing water bath at 70 deg.C, vacuum filtering, repeating for several times, and vacuum drying at 60 deg.C to obtain the electrode.
The mass ratio of the 4, 4' -biphenyl diboronic acid to the total amount of the graphene oxide in the step (3) is 0.5-5: 1;
in the step (4), the mass ratio of the 1, 4-phenyl diboronic acid to the total amount of the graphene oxide modified by the 4, 4' -biphenyl diboronic acid is 0.5-5: 1.
2. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: the preparation method of the graphene oxide in the step (1) comprises the following steps: adding 3 g of graphite into a mixed acid of 360 mL of concentrated sulfuric acid and 40 mL of phosphoric acid, stirring in an ice bath at 0 ℃, slowly adding 18 g of potassium permanganate into 4 batches of the mixed acid within 3 hours, keeping the temperature below 35 ℃, heating to 50 ℃, stirring for 12 hours, cooling to room temperature, slowly adding 400 mL of ice water, slowly dropwise adding 30vol% of hydrogen peroxide until the solution turns into golden yellow, adding 100 mL of 5vol% of hydrochloric acid, standing overnight, removing supernatant, centrifugally washing the precipitate with deionized water to be neutral, and freeze-drying to obtain the graphene oxide.
3. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: the concentration of the methanol solution of the graphene oxide in the step (2) is 1-5 mg/mL.
4. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: the volume ratio of the trimethylbenzene to the dioxane in the trimethylbenzene and dioxane solution in the step (4) is 1: 1.
5. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: step (4) N2The lower sealing reaction is carried out for 72 hours at 120 ℃.
6. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: ZnCl described in step (5)2ZnCl with acetone solution2The mass ratio to acetone was 1: 15.
7. The method for producing a graphene/carbon nanosheet electrode of claim 1, wherein: the calcination in the step (5) is specifically as follows: 600 ℃ N2And calcining for 3 hours.
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| CN106139923A (en) * | 2015-04-16 | 2016-11-23 | 中国科学院上海高等研究院 | A kind of graphene oxide framework material composite membrane and its preparation method and application |
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