CN109763139B - α-Co(OH)2/PPy/GO nanosheet and OER electrocatalytic modified electrode based on same - Google Patents
α-Co(OH)2/PPy/GO nanosheet and OER electrocatalytic modified electrode based on same Download PDFInfo
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Abstract
The present invention relates to alpha-Co (OH)2a/PPy/GO nano-sheet and an OER electro-catalysis modified electrode based on the same. The electrode comprises a glassy carbon electrode serving as a substrate electrode and a polypyrrole/graphene oxide (PPy/GO) nanosheet modified by alpha-cobalt hydroxide attached to the glassy carbon electrode. Due to the existence of the alpha-cobalt hydroxide, the reaction rate of water decomposition is enhanced, and only a lower overpotential is needed, so that the nano material modified electrode shows higher electrochemical activity and good stability in the aspect of water decomposition.
Description
Technical Field
The invention belongs to the field of electrochemical catalysis, and particularly relates to an electrocatalytic modified electrode and a preparation method and application thereof.
Background
Combustion products based on high specific energy content of hydrogen and carbon neutrality have long been considered as alternative fuels to replace fossil fuels, meeting global energy consumption. Two semi-reaction environment-friendly hydrogen production modes taking renewable energy as power have been widely explored.
The hydrogen production by electrolyzing water is characterized by abundant raw materials, simple method and extremely wide application of hydrogen. Oxygen Evolution Reactions (OERs) with multi-step, four electron processes are limited by their slow kinetics compared to Hydrogen Evolution Reactions (HER). Increasing OER activity by adding a catalyst becomes critical for water electrolysis. Conventional Ir/Ru-based catalysts play an important role in OER. However, the disadvantages of rare content, high price and poor stability greatly limit the large-scale application of the compound. Therefore, the development of a chemically modified electrode capable of electrocatalytic water decomposition, especially capable of improving OER activity, has important significance for the research of electrocatalytic decomposition of water.
Disclosure of Invention
One purpose of the invention is to provide alpha-Co (OH) with low price and high catalytic performance2a/PPy/GO nanosheet.
It is another object of the present invention to provide a method for producing the sameBy alpha-Co (OH)2An OER electro-catalysis modified electrode prepared from the/PPy/GO nano sheet is used for electro-catalysis water splitting.
In order to achieve the purpose, the invention adopts the following technical scheme:
α-Co(OH)2the preparation method of the/PPy/GO nano sheet comprises the following steps:
1) under the condition of ultrasonic radiation, pyrrole (Py) is chemically polymerized on a GO nano-sheet in situ to obtain a polypyrrole/graphene oxide (PPy/GO) nano-sheet;
2) dispersing PPy/GO nano-sheets in water, and adding CoCl into the system2·6H2O and ammonia water are evenly stirred and reacted, the obtained product is washed by distilled water and ethanol in sequence, centrifuged and dried in vacuum to obtain alpha-Co (OH)2a/PPy/GO nanosheet.
Preferably, the above-mentioned α -Co (OH)2a/PPy/GO nano sheet, according to the mass ratio, CoCl2·6H2O:PPy/GO＝30:1。
Preferably, the above-mentioned α -Co (OH)2a/PPy/GO nano sheet, wherein in the step 2), the reaction conditions are as follows: reacting for 10-14h at the pH of 8-10 at normal temperature.
Preferably, the above-mentioned α -Co (OH)2In the step 1), pyrrole (Py) is chemically polymerized in situ on a GO nano-sheet prepared by a Hummers method under the condition of ultrasonic radiation to obtain the PPy/GO nano-sheet.
Based on alpha-Co (OH)2The OER electro-catalysis modified electrode of/PPy/GO nano-sheet takes a glassy carbon electrode as a substrate electrode, and the alpha-Co (OH)2alpha-Co (OH) prepared by attaching/PPy/GO nano-sheets on glassy carbon electrode2a/PPy/GO modified glassy carbon electrode.
Based on alpha-Co (OH)2The preparation method of the OER electrocatalytic modified electrode of the/PPy/GO nano-sheet comprises the following steps:
1) mixing the above-mentioned alpha-Co (OH)2the/PPy/GO nano-sheet is ultrasonically dispersed in absolute ethyl alcohol to obtain a uniformly dispersed composite modifier;
2) dropping the uniformly dispersed composite modifier on the surface of a clean glassy carbon electrode, and drying at room temperatureDrying to obtain alpha-Co (OH)2a/PPy/GO modified glassy carbon electrode.
The above-mentioned one based on alpha-Co (OH)2The application of the OER electrocatalytic modified electrode of the/PPy/GO nano-sheet in electrocatalytic decomposition of water for oxygen evolution. The method comprises the following steps: mixing the above-mentioned alpha-Co (OH)2A/PPy/GO modified glassy carbon electrode is used as a working electrode, an Hg/HgO electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode to form a three-electrode system, and electrocatalysis on water is realized in a 1M potassium hydroxide aqueous solution.
Compared with the prior art, the invention has the following remarkable advantages:
1. due to the existence of the alpha-cobalt hydroxide, the modified electrode prepared by the invention can accelerate the speed of water decomposition into oxygen and hydrogen in the presence of the divalent cobalt compound on the surface of the nanosheet, realizes the application of water-electricity catalysis, enhances the reaction efficiency of water-electricity catalytic decomposition, and enables the nanomaterial modified electrode to show higher activity and good linearity in the aspect of water-electricity catalysis.
2. The modified electrode prepared by the method has the advantages of stronger electrochemical performance, better stability, better linearity and the like.
3. The modified electrode prepared by the invention realizes the hydrogen production and oxygen production by electrocatalytic decomposition of water, and provides a new idea and method for the actual application of electrocatalytic decomposition of water.
4. In the invention, the cobalt is low in price and large in storage capacity, and meanwhile, the polypyrrole/graphene oxide (PPy/GO) is used as a substrate to synthesize the cobalt compound-organic conductive compound, so that the conductive capability of the cobalt compound in electrochemical catalysis is promoted, and the catalytic performance of the cobalt compound is further improved.
5. The modified electrode prepared by the invention has the advantages of low price, stability, simple operation and high reaction speed.
Drawings
FIG. 1 shows a-Co (OH)2Electron microscopy images of/PPy/GO nanosheets;
wherein, (a) alpha-Co (OH)2Scanning Electron Microscope (SEM) pictures of/PPy/GO nanosheets; (b) alpha-Co (OH)2Transmission Electron Microscope (TEM) picture of/PPy/GO nanosheet.
Figure 2 is an XRD pattern of different modified electrodes.
FIG. 3 is a comparison graph of linear sweep voltammetry for electrocatalytic decomposition of water by different modified electrodes.
FIG. 4 is a Tafel slope diagram of electrocatalytic water decomposition of various modified electrodes.
FIG. 5 is a cyclic voltammogram of modified electrodes at different sweep rates.
FIG. 6 is a linear relationship between the sweep rate and the current density when the modified electrode is used for electrolyzing water.
FIG. 7 is a modified electrode timing current diagram.
FIG. 8 is a Nyquist plot of the modified electrode at different overvoltages.
Detailed Description
The present invention will be described in further detail with reference to preferred embodiments and drawings, it being understood that the preferred embodiments described herein are merely illustrative and explanatory of the invention and are not restrictive thereof.
Example 1 alpha-Co (OH)2/PPy/GO nanoplates
The preparation method comprises the following steps:
1) preparation of GO nanosheets: 67.5mL of concentrated sulfuric acid was added to a three-necked flask, and 2.0g of high purity graphite and 1.6g of NaNO were added3Stirring uniformly, keeping the temperature of the system less than 5 ℃, and adding 9g KMnO into the mixed solution within one hour4Then placing the mixture in a water bath at 36 ℃ for reaction for 0.5 h. After standing at room temperature for 14 days, the mixture is diluted with 560mL of water at 60 ℃, and H is added dropwise2O2And (3) centrifuging the solution while the solution is hot (rmp is 10000), washing the solution to be neutral, and drying the solution in vacuum at 50 ℃ to obtain the GO nano sheet.
2) PPy/GO nanosheet: adding 0.2g of GO nano-sheets into 100mL of deionized water, performing ultrasonic dispersion, adding 0.2g of pyrrole (Py), performing ultrasonic dispersion, and adding 1.2g of FeCl3·6H2And O, continuing to perform ultrasonic treatment for 0.5h, performing centrifugal washing and vacuum drying to obtain the PPy/GO nano sheet.
3)α-Co(OH)2Preparation of/PPy/GO nano-sheet: 50mg PPy/GO was dispersed in 50mL water and 1.5g Co (OH) was added to the system2·6H2O and 1mL ammonia water are stirred evenly and then are weakly stirred at room temperatureStirring continuously for 12h under alkaline condition (pH 9), after reaction, washing the obtained product with distilled water and ethanol in sequence, centrifuging, and drying in vacuum to obtain alpha-Co (OH)2a/PPy/GO nanosheet.
(II) detection
1、α-Co(OH)2An electron microscope image of the/PPy/GO nanosheet is shown in FIG. 1, wherein (a) is a Scanning Electron Microscope (SEM) image; (b) for Transmission Electron Microscopy (TEM) pictures, it can be seen from FIG. 1 that alpha-Co (OH) prepared according to the invention2The surface of the nano-sheet presents a flaky texture.
2. FIG. 2 is X-ray diffraction diagram of each composition, a is GO X-ray diffraction diagram, b is PPy/GO X-ray diffraction diagram, c is Co (OH)2X-ray diffraction pattern, d is alpha-Co (OH)2X-ray diffraction pattern of/PPy/GO, wherein ● is Co (OH)2The diffraction peak of (A-Co), (OH) is well synthesized by the invention as can be seen from the comparison of figure 22/PPy/GO。
Example 2 based on alpha-Co (OH)2OER (organic electroluminescent) electrocatalytic modified electrode of/PPy/GO nanosheet
The preparation method comprises the following steps:
1) 2mg of the dried alpha-Co (OH) prepared in example 1 were taken2Adding 1mL of ethanol into the/PPy/GO nano-sheet, and performing ultrasonic dispersion for 20min to obtain a black suspension with the concentration of 2mg/mL, namely the composite modifier for later use.
2) And (3) processing of the electrode: polishing the glassy carbon electrode on a polishing cloth by using 0.3 mu M of aluminum oxide suspension, then ultrasonically cleaning by using deionized water, polishing the polishing cloth into a mirror surface by using 0.05 mu M of aluminum oxide suspension, finally ultrasonically cleaning by using ethanol and deionized water, and drying by using high-purity nitrogen for later use.
3) Preparing a modified electrode: transferring 5 mu L of the composite modifier prepared in the step 1) by using a microsyringe, dripping the composite modifier on the surface of the glassy carbon electrode which is polished clean, and naturally drying at room temperature to obtain alpha-Co (OH)2a/PPy/GO modified glassy carbon electrode for later use.
(II) electrochemical Performance testing
1. Linear sweep voltammetric contrast for electrocatalytic oxygen evolution reaction of different modified electrodes
The method comprises the following steps: in a 1M KOH electrolytic cell, a GO modified glassy carbon electrode, a PPy/GO modified glassy carbon electrode and Co (OH) are respectively used2Modified electrode, alpha-Co (OH)2(ii) GO modified electrode and alpha-Co (OH)2the/PPy/GO modified electrode is used as a working electrode, the Hg/HgO electrode is used as a reference electrode, and the platinum wire electrode is used as an auxiliary electrode; the test was carried out on a CHI660e electrochemical workstation, with accompanying computer software for experimental data acquisition and processing; and carrying out linear scanning voltammetry test in a potential range of 1.2V-1.8V (vs. RHE), and recording a stable linear scanning voltammogram.
As shown in fig. 3, a linear sweep voltammetry contrast graph for electrocatalytic water oxygen evolution by different modified electrodes is shown, wherein a curve is a GO electrode, a curve is a PPy/GO modified glassy carbon electrode, and neither modified electrode has obvious current mutation. curve c is Co (OH)2Modified glassy carbon electrode, d curve is alpha-Co (OH)2The e curve of the/GO modified glassy carbon electrode is alpha-Co (OH)2the/PPy/GO modified electrode. The current density of curves c-e gradually increases and the overpotential gradually decreases. Explanation of pure Co (OH)2Materials and alpha-Co (OH)2The electrical conductivity of/GO is poor although it has oxygen evolution properties, while a larger current density and a very low overpotential are observed on the e-curve, comparing with alpha-Co (OH)2the/PPy/GO modified electrode has better electrocatalytic activity when electrolyzing water and evolving oxygen. Meanwhile, the comparison of Tafel curve (as shown in figure 4) obtained by linear sweep voltammogram can also show alpha-Co (OH)2the/PPy/GO has a very low Tafel slope. Thus showing the good catalytic activity of the catalyst in the oxygen evolution reaction.
2. Study of dynamics of modified electrode surface
With alpha-Co (OH)2the/PPy/GO modified electrode is a working electrode, the Hg/HgO electrode is a reference electrode, and the platinum electrode is an auxiliary electrode; the experiment was carried out on a CHI660e electrochemical workstation, including acquisition and processing of experimental data; in a 1M KOH solution, cyclic voltammetry scanning is carried out within a potential range of 1.12-1.28V (vs. RHE), and the scanning speed range is 2-20 mV/s.
FIG. 5 shows a-Co (OH)2the/PPy/GO modified electrode generates an oxygen evolution reaction cyclic voltammogram under the conditions of different scanning speeds. FromIt can be seen that as the sweep rate increases, the current density of the cyclic voltammogram also increases linearly, i.e., the water oxidation peak current increases with increasing sweep rate. By studying the influence of the scan rate on the oxidation peak current, the kinetics of the electrode reaction can be inferred.
Fig. 6 is a linear relationship of current density and scanning speed. As shown in FIG. 6, the scan rate is in the range of 2-20 mV/s, the oxidation peak current of water has a good linear relationship with the scan rate, and the slope obtained therefrom is the double layer capacitance (C)dl) Is 15.1mF.cm-2. It can be seen that the oxidation process of water is performed in a surface-controlled manner under the experimental conditions.
3. Stability measurement of catalyst
With alpha-Co (OH)2the/PPy/GO modified electrode is a working electrode, the Hg/HgO electrode is a reference electrode, and the platinum electrode is an auxiliary electrode; the experiment was carried out on a CHI660e electrochemical workstation, including acquisition and processing of experimental data; the chronoamperometric test was performed for a long time in a 1M KOH solution at a potential of 1.58V (vs. RHE). FIG. 7 shows that after 20h of testing, the current density of the catalyst decreased by only 9.4%, indicating a-Co (OH)2the/PPy/GO nano material has good stability under strong alkaline conditions.
4. Electrochemical impedance testing
With alpha-Co (OH)2the/PPy/GO material modified glassy carbon electrode is used as a working electrode, the Hg/HgO electrode is used as a reference electrode, the platinum electrode is used as an auxiliary electrode, and the base solution is 1M KOH solution; experiment impedance tests at different overpotentials, including acquisition and processing of experimental data, were performed on the CHI660e electrochemical workstation. As a result, as shown in FIG. 8, from the curves a to e, the electron transfer resistance (first semicircle in the Rct curve) gradually decreases with increasing overpotential, i.e., the conductivity increases, and α -Co (OH) is again illustrated kinetically2Good conductivity of/PPy/GO in electrolytic water evolution of oxygen.
The foregoing is merely a preferred embodiment of this invention, which is intended to be illustrative, not limiting; those skilled in the art will appreciate that many variations, modifications, and even equivalent variations are possible within the spirit and scope of the invention as defined in the appended claims.
Claims (3)
1. Based on alpha-Co (OH)2The application of the OER electrocatalytic modified electrode of/PPy/GO nano-sheet in electrocatalytic decomposition of water is characterized in that the OER electrocatalytic modified electrode is based on alpha-Co (OH)2The OER electrocatalytic modified electrode of/PPy/GO nano-sheet is prepared by taking a glassy carbon electrode as a substrate electrode and adding alpha-Co (OH)2alpha-Co (OH) prepared by attaching/PPy/GO nano-sheets on glassy carbon electrode2a/PPy/GO modified glassy carbon electrode;
the alpha-Co (OH)2The preparation method of the/PPy/GO nano sheet comprises the following steps:
1) under the condition of ultrasonic radiation, pyrrole is chemically polymerized on a GO nano-sheet in situ to obtain a PPy/GO nano-sheet;
2) dispersing PPy/GO nano-sheets in water, and adding CoCl into the system2·6H2O and ammonia water are evenly stirred and reacted, the obtained product is washed by distilled water and ethanol in sequence, centrifuged and dried in vacuum to obtain alpha-Co (OH)2a/PPy/GO nanosheet;
according to the mass ratio, CoCl2·6H2O: PPy/GO=30 : 1；
In the step 2), the reaction conditions are as follows: reacting for 10-14h at normal temperature and pH = 8-10.
2. Use according to claim 1, characterized in that said composition is based on α -Co (OH)2The preparation method of the OER electrocatalytic modified electrode of the/PPy/GO nano-sheet comprises the following steps:
1) alpha-Co (OH) according to claim 12the/PPy/GO nano-sheet is ultrasonically dispersed in absolute ethyl alcohol to obtain a uniformly dispersed composite modifier;
2) dropping and coating the uniformly dispersed composite modifier on the surface of a clean glassy carbon electrode, and drying at room temperature to obtain alpha-Co (OH)2a/PPy/GO modified glassy carbon electrode.
3. According toUse according to claim 1, characterized in that the method is as follows: alpha-Co (OH) according to claim 12A/PPy/GO modified glassy carbon electrode is used as a working electrode, an Hg/HgO electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode to form a three-electrode system, and electrocatalysis on water is realized in a 1M potassium hydroxide aqueous solution.
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