CN110610820A - Preparation method of porous carbon flexible self-supporting electrode based on melamine foam and metal organic framework material - Google Patents
Preparation method of porous carbon flexible self-supporting electrode based on melamine foam and metal organic framework material Download PDFInfo
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- CN110610820A CN110610820A CN201910906340.3A CN201910906340A CN110610820A CN 110610820 A CN110610820 A CN 110610820A CN 201910906340 A CN201910906340 A CN 201910906340A CN 110610820 A CN110610820 A CN 110610820A
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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
- H01G11/26—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 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
- H01G11/84—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 preparation method of a porous carbon flexible self-supporting electrode based on melamine foam and a metal organic framework material, wherein the preparation method of the melamine foam flexible self-supporting electrode comprises the steps of immersing the melamine foam in a cobalt salt solution; adding dimethyl imidazole, standing and drying; washing with alkali liquor, drying, and washing and drying after activation to obtain the porous carbon flexible self-supporting electrode material; the BET specific surface area of the flexible self-supporting electrode of the melamine foam can reach 1136m2(ii) in terms of/g. The carbon material with the hierarchical pore structure maintains flexibility, and simultaneously improves the specific surface area, micropore specific gravity and conductivity of the material, thereby showing excellent electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of super capacitors, and particularly relates to a preparation method of a porous carbon flexible self-supporting electrode based on melamine foam and a metal organic framework material.
Background
The energy storage element is one of the hot spots of research and research, especially a super capacitor, and has been widely applied in the fields of electric vehicle power supplies, portable electronic devices and the like due to its high-efficiency and practical energy storage characteristics and the advantages of large energy density, high power density and the like. With the emergence of the requirements of human beings on flexible and bendable electronic equipment and the like, the preparation of the flexible all-solid-state electrode is concerned by the majority of researchers.
The melamine foam is a cheap and environment-friendly porous material, and can maintain the original three-dimensional porous structure and excellent mechanical properties after carbonization. However, the directly carbonized melamine foam has poor electrochemical performance due to the low specific surface area and the lack of micropores.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the invention, the invention overcomes the defects in the prior art and provides a preparation method of a porous carbon flexible self-supporting electrode based on melamine foam and metal organic framework materials.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a melamine foam flexible self-supporting electrode comprises the steps of immersing melamine foam in a cobalt salt solution; adding dimethyl imidazole, standing and drying; washing with alkali liquor, drying, and washing and drying after activation to obtain the porous carbon flexible self-supporting electrode material.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: the melamine foam is treated at constant temperature for 1-2h under the carbonization condition of hydrogen and argon atmosphere, the temperature rise rate is 5 ℃/min, the carbonization temperature is 700-900 ℃.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: and immersing the melamine foam into a cobalt salt solution, wherein the cobalt salt solution is a cobalt nitrate hexahydrate solution, the concentration of the cobalt nitrate hexahydrate solution is 10-30mg/mL, the solvent is water, and the standing time is 6-12 h.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: and washing with alkali liquor, wherein the alkali liquor comprises one or more of potassium hydroxide and sodium hydroxide, the solute concentration is 2-4mol/L, and the ratio of the sample to the solute is 1:3 (mass ratio) and the standing time is 3-5 h.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: the secondary carbonization is carried out under the carbonization conditions of argon, the temperature rising rate is 5 ℃/min, the carbonization temperature is 900 ℃ and the constant temperature is 3 hours.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: and (3) drying after standing, wherein the standing time is 6-12h, the drying temperature is 60-80 ℃, and the drying temperature is 60-80 ℃ and the drying time is 12-24 h.
The preferable scheme of the preparation method of the melamine foam flexible self-supporting electrode is as follows: and (3) after activation, washing and drying, namely standing in hydrochloric acid for 10h, washing with distilled water to be neutral, and drying at the drying temperature of 60-80 ℃ for 12-24 h.
In one aspect, the present invention overcomes the disadvantages of the prior art by providing a flexible self-supporting electrode made by the method of any one of claims 1 to 7, wherein: the BET specific surface area can reach 1136m2/g。
As a preferable scheme of the melamine foam flexible self-supporting electrode, the invention comprises the following components: the specific volume reaches 238F/g, and after 10000 cycles, the specific volume retention rate is 94 percent.
As a preferable scheme of the melamine foam flexible self-supporting electrode, the invention comprises the following components: bending 180 degrees, and the specific volume retention rate is 90 percent.
The invention has the beneficial effects that:
the invention provides a preparation method of porous carbon based on melamine foam and a metal organic framework material, which is used as an all-solid-state electrode for a super capacitor, the carbonized melamine foam is loaded, activated/carbonized through a metal organic framework material (Co-ZIF-L) with a sheet structure to obtain the carbon material with a hierarchical pore structure, and the specific surface area, micropore specific gravity and conductivity of the material are improved while the flexibility is maintained, so that excellent electrochemical performance is shown.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1(a) is the apparent morphology of a porous carbon material based on carbonized melamine foam and Co-ZIF-L, (b) is the apparent morphology after bending 180 degrees, and (c-e) is the apparent morphology of the material before and after compression.
FIG. 2 is SEM images of carbonized melamine foam and porous carbon materials based on carbonized melamine foam and Co-ZIF-L in example 1 of the present invention, wherein (a) is an SEM image of carbonized melamine foam, and (b) and (c) are SEM images of porous carbon materials based on carbonized melamine foam and Co-ZIF-L, respectively.
FIG. 3 is a cyclic voltammetry curve and (b) a constant current charge and discharge curve of a porous carbon material based on melamine foam and Co-ZIF-L directly used as a flexible electrode.
FIG. 4 is a cyclic voltammogram of porous carbon materials based on melamine foam and Co-ZIF-L at different degrees of bending.
Fig. 5 shows a carbonized melamine foam having poor mechanical properties prepared in comparative example 2.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The melamine foam used in example 1 of the present invention was purchased from Sichuan new ultra-polymerized material Co., Ltd, and the performance indexes thereof are shown in Table 1 below:
example 1:
cutting melamine foam (8 × 5 × 2.5cm, maximum tensile strength of 0.03451 + -0.0007 MPa, Sichuan super-polymer new material Co., Ltd.) into rectangular blocks of 4.5 × 2.5 × 0.2cm, carbonizing at 800 deg.C in hydrogen and argon atmosphere, heating at 5 deg.C/min, and keeping the temperature for 1 h. And then, soaking the carbonized foam in a cobalt nitrate hexahydrate aqueous solution, wherein the concentration of the cobalt nitrate hexahydrate aqueous solution is 15mg/mL, and standing for 12 hours. And then, adding 33.7 mg/mL of dimethyl imidazole into the solution, standing for 12h, taking out, washing with water, and drying at 70 ℃ to obtain a ZIF-L loaded composite sample on the carbonized sponge. And (3) placing the composite sample into a 3mol/L (sample and potassium hydroxide are 1:3) solution, standing for 3h, taking out, drying, carrying out secondary carbonization at 800 ℃ in an argon atmosphere, heating at a speed of 5 ℃/min, keeping the temperature for 3h, cooling to room temperature, taking out, standing for 10h in 37% hydrochloric acid, washing with distilled water to be neutral, and drying at 70 ℃ to obtain a final sample.
FIG. 1a shows that the prepared porous carbon maintains the appearance of the original carbonized melamine foam, is in a lamellar shape and utilizes the transmission of electrons. The prepared sample has high mechanical properties and will not break after bending 180 degrees, see fig. 1b, and after compression the sample will not collapse and will recover its original state after removal of the external force, see fig. 1 c-e. Tensile tests show that the composite material has good tensile property, the maximum tensile strength is 0.07824 +/-0.008729 MPa, and the mechanical property is unchanged after the composite material is restored to the original state.
SEM appearance observation is carried out on the prepared porous carbon material, and the figure is shown in figure 2. Wherein (a) is carbonized melamine foam and (b) (c) is SEM morphology of porous carbon based on melamine foam and Co-ZIF-L. It can be seen that the carbonized melamine foam has a smooth surface, while the porous carbon based on melamine foam and Co-ZIF-L has a layer of porous carbon coated on the original carbonized melamine foam. The porous carbon wrapped at the periphery mainly comes from the activation and carbonization of Co-ZIF-L loaded on the surface of carbonized melamine foam, and residual Co ions are removed by soaking hydrochloric acid, so that the porosity is further improved. Porous carbon based on melamine foam and Co-ZIF-L with a BET specific surface area of 1136m2A pure carbonized melamine foam having a specific surface area of 4m2/g。
Example 2
The sample of example 1 was used as a self-supporting flexible electrode material to test its electrochemical performance. The test method is as follows: the test system is a three-electrode system comprising 6M KOH solution as electrolyte and 2.5X 2.5cm2The platinum sheet of (2) was used as the counter electrode and the carbon material of example 1 was used as the working electrode.
The tested cyclic voltammetry curve and constant current charging and discharging curve are shown in figure 3. At current densities of 1, 2, 3, 5, 10 and 20A/g, the specific volumes are respectively 238, 213, 194, 158, 112 and 71F/g.
Example 3
The samples from example 1 were subjected to cycle performance testing. Under the test condition that the current density is 3A/g, after 10000 cycles, the specific volume is 182F/g, and the retention rate is 94%.
Example 4
The samples of example 1 were tested at different bending angles and their cyclic voltammograms are shown in FIG. 4. Under the test condition of the sweep speed of 50mv/s, the specific volumes of the samples were 103, 102 and 93F/g when the samples were not bent, bent 90 degrees and bent 180 degrees, respectively, and thus it was found that the specific volume was slightly reduced to 90% of the original value when the samples were bent 180 degrees, thereby exhibiting excellent flexibility and electrochemical properties.
Comparative example 1
And performing electrochemical test on the directly carbonized melamine foam as a self-supporting flexible electrode. The preparation method of the directly carbonized melamine foam comprises the following steps: the melamine foam is directly carbonized, the carbonization condition is hydrogen and argon atmosphere, the temperature rise rate is 5 ℃/min, the carbonization temperature is 700-. At current densities of 1, 2, 3, 5, 10 and 20A/g, the specific volumes are respectively 92, 72, 63, 56, 41 and 30F/g. Therefore, the porous carbon based on the carbonized melamine foam and the Co-ZIF-L has higher electrochemical characteristics compared with the pure carbonized melamine foam. The main reason is that the nitrogen-doped carbon is loaded on the surface of carbonized foam through Co-ZIF-L, is treated by alkali liquor, is activated and carbonized to form nitrogen-doped carbon with a hierarchical pore structure, and is wrapped on the surface of original carbonized melamine foam to increase the specific surface area of the material. The presence of hierarchical pores also facilitates mass transport. In the carbonization process, the cobalt ions contained in the Co-ZIF-L can improve the graphitization degree of the material and further improve the conductivity of the material, and the residual cobalt ions after carbonization can be removed by washing with hydrochloric acid and further improve the porosity of the material. Thus, porous carbon based on carbonized melamine foam and Co-ZIF-L has a higher specific volume than pure carbonized melamine foam.
In addition, the Co-ZIF-L load and the subsequent activation and carbonization treatment do not affect the apparent morphology and mechanical properties of the original material, the obtained carbon material still has good tensile property, compressive property and flexibility, and the structure is not damaged under external forces of compression, bending and the like, and meanwhile, the high electrochemical property is still maintained.
Comparative example 2:
cutting melamine foam (8 × 5 × 2.5cm, purchased from Tanshinal house, Ledian, Jinhua, Zhejiang province, model: LD-1539F) into rectangular blocks of 4.5 × 2.5 × 0.2cm, carbonizing at 800 deg.C in hydrogen and argon atmosphere, heating at 5 deg.C/min, and keeping the temperature for 1 h. The carbonized melamine foam has poor mechanical properties, can be kneaded and broken by hands, has no flexibility and cannot be subjected to subsequent research. See fig. 5.
The invention provides a preparation method of porous carbon based on melamine foam and a metal organic framework material, and the porous carbon is used as an all-solid-state electrode for a super capacitor. The melamine foam is a cheap and environment-friendly porous material, and can maintain the original three-dimensional porous structure and excellent mechanical properties after carbonization. However, the directly carbonized melamine foam has poor electrochemical performance due to the low specific surface area and the lack of micropores. According to the method, carbonized melamine foam is loaded and activated/carbonized through a metal organic framework material (Co-ZIF-L) with a sheet structure to obtain a carbon material with a hierarchical pore structure, the specific surface area, micropore specific gravity and conductivity of the material are improved while the original flexibility is maintained, and therefore excellent electrochemical performance is shown.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a melamine foam flexible self-supporting electrode is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
immersing melamine foam into a cobalt salt solution;
adding dimethyl imidazole, standing and drying;
washing with alkali liquor, drying, and washing and drying after activation to obtain the porous carbon flexible self-supporting electrode material.
2. The method for preparing a melamine foam flexible self-supporting electrode as set forth in claim 1, wherein: the melamine foam is treated at constant temperature for 1-2h under the carbonization condition of hydrogen and argon atmosphere, the temperature rise rate is 5 ℃/min, the carbonization temperature is 700-900 ℃.
3. The method for preparing a melamine foam flexible self-supporting electrode as set forth in claim 1, wherein: and immersing the melamine foam into a cobalt salt solution, wherein the cobalt salt solution is a cobalt nitrate hexahydrate solution, the concentration of the cobalt nitrate hexahydrate solution is 10-30mg/mL, the solvent is water, and the standing time is 6-12 h.
4. A method for preparing a melamine foam flexible self-supporting electrode as set forth in claim 3, wherein: and washing with alkali liquor, wherein the alkali liquor comprises one or more of potassium hydroxide and sodium hydroxide, the solute concentration is 2-4mol/L, and the ratio of the sample to the solute is 1:3 (mass ratio) and the standing time is 3-5 h.
5. A method for preparing a melamine foam flexible self-supporting electrode as set forth in claim 3, wherein: the secondary carbonization is carried out under the carbonization conditions of argon, the temperature rising rate is 5 ℃/min, the carbonization temperature is 900 ℃ and the constant temperature is 3 hours.
6. A method for preparing a melamine foam flexible self-supporting electrode as claimed in any one of claims 1 to 5, wherein: and (3) drying after standing, wherein the standing time is 6-12h, the drying temperature is 60-80 ℃, and the drying temperature is 60-80 ℃ and the drying time is 12-24 h.
7. The method for preparing a melamine foam flexible self-supporting electrode as set forth in claim 1, wherein: and (3) after activation, washing and drying, namely standing in hydrochloric acid for 10h, washing with distilled water to be neutral, and drying at the drying temperature of 60-80 ℃ for 12-24 h.
8. The melamine foam flexible self-supporting electrode prepared by the method of any one of claims 1 to 7, which is characterized in that: the BET specific surface area can reach 1136m2/g。
9. The melamine foam flexible self-supporting electrode of claim 8, wherein: the specific volume reaches 238F/g, and after 10000 cycles, the specific volume retention rate is 94 percent.
10. The melamine foam flexible self-supporting electrode of claim 8, wherein: bending 180 degrees, and the specific volume retention rate is 90 percent.
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