CN107754786B - By using KMnO4Method for improving electrocatalytic oxidation on direct oxidized graphite paper - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 58
- 239000010439 graphite Substances 0.000 title claims abstract description 58
- 230000003647 oxidation Effects 0.000 title claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 229910016978 MnOx Inorganic materials 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- 239000013543 active substance Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 3
- 230000009467 reduction Effects 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000011149 active material Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- B01J35/33—
Abstract
By using KMnO4The method for improving the electrocatalytic performance on the direct oxidation graphite paper comprises the following steps: (1) cutting graphite paper into rectangles, cleaning the rectangles with acetone and deionized water, placing the rectangles in an oven for drying to obtain dried graphite paper, and placing the dried graphite paper in a polytetrafluoroethylene bottle; (2) configuring KMnO4A solution; (3) taking KMnO4Adding the solution into the polytetrafluoroethylene bottle with the graphite paper in the step (1), then putting the bottle into a stainless steel hydrothermal kettle, sealing and reacting; (4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the reacted graphite paper is washed by deionized water and dried to obtain MnOxa/GP electrode. The method of the invention directly utilizes KMnO4Direct oxidation of graphite paper, which is both a reducing agent and a base material for supporting active substances, reduction product MnOxThe manganese dioxide and the graphite paper can be firmly combined by growing on the graphite paper sheet, so that the electrocatalytic performance is improved, and the active substances are not easy to fall off, so that the electrocatalytic performance is stable.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a method for preparing a metal electrode by using KMnO4Directly oxidizing graphite paper to obtain active matter MnOxThe material can be firmly combined with the graphite paper substrate, thereby obtaining high-activity MnOxa/GP electrode, a method for enhancing electrocatalysis.
Background
The manganese element is rich in source, the electrocatalytic performance of the manganese oxide attached to the surface of the current collector is discussed, and the research on the electrocatalytic performance of the manganese oxide has important practical significance. The main reason for the restriction of the electrocatalytic properties of manganese oxides is their poor electrical conductivity. The conductive capability of the carbon nano material is improved by compounding the carbon nano material with the carbon nano material, and the electrocatalytic performance of the carbon nano material is hopefully enhanced.
The hydrothermal synthesis process is carried out in a reaction kettle, the solution is used as a medium, a high-temperature and high-pressure environment is created by heating the reaction kettle, substances which are insoluble or insoluble in the normal condition can be dissolved, and the substances are subjected to the processes of dissolving, recrystallizing or curing, so that the nano-structured material is finally formed. The active material is electrodeposited on the active substrate, so that the OER electrocatalytic activity can be extremely high, but after the cycle test, the active material is easily exfoliated, and the electrocatalytic performance is reduced. Therefore, the enhancement of the adhesion of the active substance on the surface plays a key role in improving the performance of the active substance. The active material and the substrate are subjected to chemical reaction, so that a strong coupling relation exists between the active material and the conductive substrate, and the active electrode with firm adhesion is a means for effectively improving the electrocatalytic performance of the material OER.
In this method, we used KMnO as a hydrothermal method4The solution is used as an oxidant and is chemically reacted with the substrate graphite paper to obtain an active substance MnOxThe material can be firmly combined with the graphite paper substrate, thereby obtaining high-activity MnOxa/GP electrode, a method for enhancing electrocatalysis.
At present, KMnO is not utilized at home and abroad4The direct oxidation of the graphite paper promotes the manganese dioxide and the graphite paper to be firmly combined, and improves the relevant reports of the electrocatalysis performance.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
One of the technical problems to be solved by the invention is to utilize a simple process to firmly combine the electrocatalyst with the substrate; the second technical problem to be solved by the invention is to obtain an effective electrocatalyst deposition layer by using a hydrothermal method; the invention aims to solve the technical problem of improving the electrocatalysis performance of the electrode by using a simple process. In order to achieve the purpose, the invention adopts the following technical scheme:
by using KMnO4The method for improving the electrocatalytic performance on the direct oxidation graphite paper comprises the following steps:
(1) cutting graphite paper into a rectangle, cleaning the rectangle by acetone and deionized water, placing the rectangle in a drying oven at 60 ℃ for drying for at least 6 hours to obtain dried graphite paper, and placing the dried graphite paper in a polytetrafluoroethylene bottle;
(2) configuring KMnO4A solution;
(3) 20mL of KMnO was taken4Adding the solution into the polytetrafluoroethylene bottle with the graphite paper in the step (1), then putting the bottle into a stainless steel hydrothermal kettle, sealing and reacting;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the graphite paper after the reaction is washed for 4-5 times by deionized water and dried in a drying oven at 60 ℃ to obtain MnOxa/GP electrode.
Preferably, the area of the graphite paper is not less than 1cm2。
Preferably, KMnO in step (2)4The concentration of the solution is 0.01-2mol L-1。
Preferably, the temperature of the reaction in step (3) is 100-180 ℃; the reaction time is 4-16 h.
Preferably, the drying time in step (4) is 0.1 to 12 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method of the invention directly utilizes KMnO4Direct oxidation of graphite paper, which is both a reducing agent and a base material for supporting active substances, reduction product MnOxThe manganese dioxide can be firmly combined with the graphite paper by growing on the graphite paper sheet, so that the electrocatalytic performance is improved. The active substance is not easy to fall off, so that the electrocatalysis performance is stable.
(2) The method has the advantages of simple process, mild conditions and low cost.
Drawings
FIG. 1 is an electron micrograph of unreacted graphite paper;
FIG. 2 shows MnO prepared in example 1xElectron microscopy of the/GP electrode;
FIG. 3 is a comparative MnO deposition on graphite paperxThe LSV curve of (a);
FIG. 4 shows MnO obtained in example 1xLSV curve of/GP electrode;
FIG. 5 shows MnO obtained in example 2xLSV curve of/GP electrode;
FIG. 6 shows MnO obtained in example 3xLSV curve of/GP electrode.
Detailed Description
Specific embodiments of the present invention are described in detail below with reference to specific examples, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Example 1：
By using KMnO4A method for enhancing electrocatalytic oxidation on directly oxidized graphite paper, comprising the steps of:
(1) cutting graphite paper into 1 × 2.3cm at room temperature2Cleaning a rectangle with a specification by acetone and deionized water, and placing the rectangle in a 60 ℃ oven for at least 6 hours;
(2) placing the dried graphite paper into a 25mL polytetrafluoroethylene inner container;
(3) weighing appropriate amount of KMnO4Stirring and dissolving in deionized water, dissolving in 100mL volumetric flask to obtain a solution with a concentration of 0.05mol L-1The solution of (1);
(4) 20mL of prepared KMnO was measured4The solution is added into stainless steel water with graphite paper and the kettle is sealed and reacted for 6h at 140 ℃. After the reaction is finished, the reaction kettle is naturally cooled to room temperature, the graphite paper after the reaction is washed for 4 to 5 times by deionized water and dried for 6 hours in a 60 ℃ drying oven to obtain MnOxa/GP electrode.
Example 2：
By using KMnO4A method for enhancing electrocatalytic oxidation on directly oxidized graphite paper, comprising the steps of:
(1) cutting graphite paper into 1 × 2.3cm at room temperature2Cleaning a rectangle with a specification by acetone and deionized water, and placing the rectangle in a 60 ℃ oven for at least 6 hours;
(2) placing the dried graphite paper into a 25mL polytetrafluoroethylene inner container;
(3) weighing appropriate amount of KMnO4Stirring and dissolving in deionized water, dissolving in 100mL volumetric flask to obtain a solution with a concentration of 0.05mol L-1The solution of (1). 20mL of prepared KMnO was measured4Adding the solution into a stainless steel hot kettle with graphite paper placed therein, sealing, and reacting at 120 ℃ for 6 h;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the graphite paper after the reaction is washed for 4 to 5 times by deionized water and dried for 6 hours in a 60 ℃ drying oven to obtain MnOxa/GP electrode.
Example 3：
By using KMnO4A method for enhancing electrocatalytic oxidation on directly oxidized graphite paper, comprising the steps of:
(1) cutting graphite paper into 1 × 2.3cm at room temperature2Cleaning a rectangle with a specification by acetone and deionized water, and placing the rectangle in a 60 ℃ oven for at least 6 hours;
(2) placing the dried graphite paper into a 25mL polytetrafluoroethylene inner container;
(3) weighing appropriate amount of KMnO4Stirring and dissolving in deionized water, dissolving in 100mL volumetric flask to obtain a solution with a concentration of 0.05mol L-1The solution of (1);
(4) 20mL of prepared KMnO was measured4Adding the solution into stainless steel water with graphite paper, sealing the kettle, and reacting at 200 deg.C for 6 h. After the reaction is finished, the reaction kettle is naturally cooled to room temperature, the graphite paper after the reaction is washed for 4 to 5 times by deionized water and dried for 6 hours in a 60 ℃ drying oven to obtain MnOxa/GP electrode. MnO prepared in examples 1-3 was treated with CHI 660D electrochemical workstationxBy the/GP electrodeAll electrochemical performance tests were performed.
At a constant temperature of 30 ℃, a three-electrode system is adopted, and an AgCl/Ag electrode (internal charge is 3.5 mol. L)-1Saturated KCl solution) as a reference electrode, a platinum sheet electrode as an auxiliary electrode, a graphite paper electrode as a working electrode, and an appropriate electrolyte selected according to the properties of the working electrode, wherein the electrolyte selected in the example is an alkaline KOH solution (1 mol. L)-1). Before the test is started, high-purity oxygen is continuously introduced into the electrolytic cell for 30min to ensure that the electrolyte is saturated with oxygen.
In addition, it is necessary to complement the method of the invention in the examples to obtain a measure of the performance of the electrode (specific value of high specific capacitance), preferably in comparison with the electrode obtained by the conventional method (control).
TABLE 1 determination of the Performance of the electrodes obtained by the method of the invention
Note: the control was MnOx deposited on graphite paper, otherwise the same as the process of the invention.
As is clear from Table 1, MnO obtained by the method of the present inventionxThe electrocatalytic performance of the/GP electrode is better.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (4)
1. By using KMnO4The method for improving the electrocatalysis performance on the direct oxidation graphite paper is characterized by comprising the following steps:
(1) cutting graphite paper into a rectangle, cleaning the rectangle by acetone and deionized water, placing the rectangle in a drying oven at 60 ℃ for drying for at least 6 hours to obtain dried graphite paper, and placing the dried graphite paper in a polytetrafluoroethylene bottle;
(2) configuring KMnO4A solution;
(3) 20mL of KMnO was taken4Adding the solution into the polytetrafluoroethylene bottle with the graphite paper in the step (1), then putting the bottle into a stainless steel hydrothermal kettle, sealing and reacting;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the graphite paper after the reaction is washed for 4-5 times by deionized water and dried in a drying oven at 60 ℃ to obtain MnOxa/GP electrode;
wherein the reaction temperature in the step (3) is 120-200 ℃; the reaction time is at least 6 h;
among them, KMnO4 directly oxidizes graphite paper, which is both a reducing agent and a base material supporting an active substance, and the reduction product MnOx is grown on the graphite paper.
2. Utilizing KMnO as in claim 14The method for improving the electrocatalysis performance on the direct oxidation graphite paper is characterized in that the area of the graphite paper is not less than 1cm2。
3. Utilizing KMnO as in claim 14The method for improving the electrocatalytic performance on the direct oxidation graphite paper is characterized in that KMnO in the step (2)4The concentration of the solution is 0.01-2mol L-1。
4. Utilizing KMnO as in claim 14The method for improving the electrocatalytic performance on the graphite paper by direct oxidation is characterized in that the drying time in the step (4) is 0.1-12 h.
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| CN112981453A (en) * | 2021-02-05 | 2021-06-18 | 常熟理工学院 | Method for preparing water oxidation electrode by using waste stainless steel as base material |
| CN115472443B (en) * | 2022-08-18 | 2023-12-15 | 浙江理工大学 | Method for loading graphene quantum dots on graphite paper by hydrothermal method and application of method in aspect of preparing planar miniature supercapacitor |
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