CN112679995A - Method for improving electrochemical corrosion resistance of conductive carbon black - Google Patents
Method for improving electrochemical corrosion resistance of conductive carbon black Download PDFInfo
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- CN112679995A CN112679995A CN202011441444.0A CN202011441444A CN112679995A CN 112679995 A CN112679995 A CN 112679995A CN 202011441444 A CN202011441444 A CN 202011441444A CN 112679995 A CN112679995 A CN 112679995A
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Abstract
The invention discloses a method for improving electrochemical corrosion resistance of conductive carbon black, which comprises the following two steps: step 1, mixing conductive carbon black with an alcohol solvent, and stirring for a period of time to uniformly disperse the conductive carbon black in the alcohol solvent; and 2, irradiating the conductive carbon black alcohol solution by using unfocused pulse laser, and stirring the solution in the irradiation process. Compared with the initial conductive carbon black, the conductive carbon black subjected to laser irradiation treatment has lower corrosion current under the condition of high potential and shows higher electrochemical corrosion resistance.
Description
Technical Field
The invention belongs to the field of proton exchange membrane fuel cell catalysts, and particularly relates to a method for improving electrochemical corrosion resistance of conductive carbon black.
Background
The proton exchange membrane fuel cell can directly convert the chemical energy of molecules such as methanol, hydrogen and the like into electric energy, and has the advantages of high energy conversion efficiency, environmental friendliness and the like. The electrocatalytic stability of the electrode catalyst directly affects the service life of the proton exchange membrane fuel cell, and the corrosion of the carbon carrier in the operation process of the cell is one of the main reasons for the attenuation of the catalytic activity of the catalyst. Currently, the most commonly used catalyst support is Vulcan XC-72R conductive carbon black. Under the harsh working environment of the proton exchange membrane fuel cell, the conductive carbon black is easy to generate electrochemical oxidation corrosion, the acting force between the conductive carbon black and the loaded Pt nano-particles is reduced, the agglomeration and the loss of Pt are aggravated, and the catalytic activity of the catalyst is rapidly attenuated. Therefore, optimizing the electrochemical corrosion resistance of the conductive carbon black has important significance for prolonging the service life of the proton exchange membrane fuel cell. At present, the most common method for improving the electrochemical corrosion resistance of conductive carbon black is high-temperature annealing (>1500 ℃), which has high energy consumption and high cost and needs to be carried out under the protection of inert gas, so that the method still has certain defects.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art, provides a method for improving the electrochemical corrosion resistance of conductive carbon black, and aims to solve the problems that the most common method for improving the electrochemical corrosion resistance of the conductive carbon black at present is high-temperature annealing (1500 ℃), the method has high energy consumption and high cost, and needs to be carried out under the protection of inert gas.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
a method for improving the electrochemical corrosion resistance of conductive carbon black is characterized by comprising the following two steps:
step 1, mixing conductive carbon black with an alcohol solvent, and stirring for a period of time to uniformly disperse the conductive carbon black in the alcohol solvent;
and 2, irradiating the conductive carbon black alcohol solution by using unfocused pulse laser, and stirring the solution in the irradiation process.
The alcohol solvent is one or more of methanol, ethanol and isopropanol.
The mass ratio of the conductive carbon black to the alcohol solvent is 1: 100-1: 700.
the wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 5-20 Hz, and the energy density is 200-800 mJ/cm2。
The time for irradiating the conductive carbon black alcohol solution by laser is 5-20 min.
The conductive carbon black is used as a carrier for proton exchange membrane fuel cell catalysts.
Has the advantages that:
the invention utilizes the alcoholic solution of the laser irradiation conductive carbon black to effectively improve the electrochemical corrosion resistance of the conductive carbon black, the method of the invention is simple, rapid, efficient and easy for batch production, the whole process flow is carried out under the room temperature condition, and inert gas protection is not needed, thereby avoiding the defects of large energy consumption and high cost of the traditional high-temperature annealing mode.
Drawings
FIG. 1 is a graph of corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black;
FIG. 2 is a graph of corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black;
FIG. 3 is a graph of corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black;
FIG. 4 is a graph of corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black;
FIG. 5 is a graph of corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black.
Detailed Description
The following detailed description of the embodiments of the present invention will be provided to facilitate better understanding of the technical solutions by the related art through the description of the embodiments with reference to the accompanying drawings
Example 1
Firstly, mixing 50 mg of conductive carbon black with 20mL of ethanol, and stirring for 10min to uniformly disperse the conductive carbon black in the ethanol;
subsequently, the ethanol solution of the conductive carbon black is irradiated by unfocused pulse laser, and the solution is still stirred during the irradiation process. The wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 10Hz, and the energy density is 400mJ/cm2The irradiation time was 15 min.
FIG. 1 shows the corrosion current versus time for an initial conductive carbon black and a laser irradiated conductive carbon black. At a potential of 1.2V (vs. nhe), no water decomposition reaction occurs, and the reaction that occurs at this time is mainly a carbon corrosion reaction, and therefore, the corrosion current at this potential can be used as a measure of the electrochemical corrosion resistance of the conductive carbon black. As can be seen from fig. 1, the laser irradiated conductive carbon black exhibited lower corrosion current than the initial conductive carbon black throughout the test; after 3600s, the corrosion current of the laser irradiation conductive carbon black is 0.147 mu A, which is obviously lower than that of the initial conductive carbon black (0.424 mu A). The test result shows that the conductive carbon black irradiated by the laser has higher electrochemical corrosion resistance. Electrochemical test conditions: the diameter of the working electrode is 5mm, the loading capacity of the conductive carbon black on the electrode is 50 mu g, the electrolyte is 0.5M sulfuric acid water solution saturated by nitrogen, the constant potential is 1.2V (vs. NHE), the time is 3600s, and the test temperature is 25 ℃.
Example 2
Firstly, mixing 35 mg of conductive carbon black with 20mL of ethanol, and stirring for 10min to uniformly disperse the conductive carbon black in the ethanol;
subsequently, the conductive carbon is irradiated with an unfocused pulsed laserBlack ethanol solution, the solution was still stirred during irradiation. The wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 10Hz, and the energy density is 300mJ/cm2The irradiation time was 10 min.
FIG. 2 shows the corrosion current versus time for the initial conductive carbon black and the laser irradiated conductive carbon black. As can be seen from FIG. 2, the laser irradiated conductive carbon black had a lower corrosion current than the initial conductive carbon black throughout the test; after 3600s, the corrosion current of the initial conductive carbon black is 0.424 muA, and the corrosion current of the laser irradiation conductive carbon black is 0.191 muA. The test result shows that the laser irradiation can effectively improve the electrochemical corrosion resistance of the conductive carbon black. Electrochemical test conditions: the diameter of the working electrode is 5mm, the loading capacity of the conductive carbon black on the electrode is 50 mu g, the electrolyte is 0.5M sulfuric acid water solution saturated by nitrogen, the constant potential is 1.2V (vs. NHE), the time is 3600s, and the test temperature is 25 ℃.
Example 3
Firstly, mixing 150 mg of conductive carbon black with 20mL of ethanol, and stirring for 10min to uniformly disperse the conductive carbon black in the ethanol;
subsequently, the ethanol solution of the conductive carbon black is irradiated by unfocused pulse laser, and the solution is still stirred during the irradiation process. The wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 20Hz, and the energy density is 800mJ/cm2The irradiation time was 20 min.
FIG. 3 shows the corrosion current versus time for the initial conductive carbon black and the laser irradiated conductive carbon black. As can be seen from FIG. 3, the laser irradiated conductive carbon black had a lower corrosion current than the initial conductive carbon black throughout the test; after 3600s, the corrosion current of the initial conductive carbon black is 0.424 μ A, and the corrosion current of the laser irradiation conductive carbon black is 0.113 μ A. The test result shows that the laser irradiation can effectively improve the electrochemical corrosion resistance of the conductive carbon black. Electrochemical test conditions: the diameter of the working electrode is 5mm, the loading capacity of the conductive carbon black on the electrode is 50 mu g, the electrolyte is 0.5M sulfuric acid water solution saturated by nitrogen, the constant potential is 1.2V (vs. NHE), the time is 3600s, and the test temperature is 25 ℃.
Example 4
Firstly, mixing 25 mg of conductive carbon black with 20mL of ethanol, and stirring for 10min to uniformly disperse the conductive carbon black in the ethanol;
subsequently, the ethanol solution of the conductive carbon black is irradiated by unfocused pulse laser, and the solution is still stirred during the irradiation process. The wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 5Hz, and the energy density is 200mJ/cm2The irradiation time was 5 min.
FIG. 4 shows the corrosion current versus time for the initial conductive carbon black and the laser irradiated conductive carbon black. As can be seen from FIG. 4, the laser irradiated conductive carbon black had a lower corrosion current than the initial conductive carbon black throughout the test; after 3600s, the corrosion current of the initial conductive carbon black is 0.424 muA, and the corrosion current of the laser irradiation conductive carbon black is 0.167 muA. The test result shows that the laser irradiation can effectively improve the electrochemical corrosion resistance of the conductive carbon black. Electrochemical test conditions: the diameter of the working electrode is 5mm, the loading capacity of the conductive carbon black on the electrode is 50 mu g, the electrolyte is 0.5M sulfuric acid water solution saturated by nitrogen, the constant potential is 1.2V (vs. NHE), the time is 3600s, and the test temperature is 25 ℃.
Example 5
Firstly, mixing 80 mg of conductive carbon black with 20mL of ethanol, and stirring for 10min to uniformly disperse the conductive carbon black in the ethanol;
subsequently, the ethanol solution of the conductive carbon black is irradiated by unfocused pulse laser, and the solution is still stirred during the irradiation process. The wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 20Hz, and the energy density is 600mJ/cm2The irradiation time was 15 min.
FIG. 5 shows the corrosion current versus time for the initial conductive carbon black and the laser irradiated conductive carbon black. As can be seen from FIG. 5, the laser irradiated conductive carbon black had a lower corrosion current than the initial conductive carbon black throughout the test; after 3600s, the corrosion current of the initial conductive carbon black is 0.424 muA, and the corrosion current of the laser irradiation conductive carbon black is 0.204 muA. The test result shows that the laser irradiation can effectively improve the electrochemical corrosion resistance of the conductive carbon black. Electrochemical test conditions: the diameter of the working electrode is 5mm, the loading capacity of the conductive carbon black on the electrode is 50 mu g, the electrolyte is 0.5M sulfuric acid water solution saturated by nitrogen, the constant potential is 1.2V (vs. NHE), the time is 3600s, and the test temperature is 25 ℃.
From the above embodiments, it can be seen that the electrochemical corrosion resistance of the conductive carbon black can be improved by irradiating the alcohol solution of the conductive carbon black with the unfocused pulsed laser.
The invention is described above with reference to the accompanying drawings, it is obvious that the specific implementation of the invention is not limited by the above-mentioned manner, and it is within the scope of the invention to adopt various insubstantial modifications of the inventive concept and solution, or to apply the inventive concept and solution directly to other applications without modification.
Claims (6)
1. A method for improving the electrochemical corrosion resistance of conductive carbon black is characterized by comprising the following two steps:
step 1, mixing conductive carbon black with an alcohol solvent, and stirring for a period of time to uniformly disperse the conductive carbon black in the alcohol solvent;
and 2, irradiating the conductive carbon black alcohol solution by using unfocused pulse laser, and stirring the solution in the irradiation process.
2. The method of claim 1, wherein the conductive carbon black has improved electrochemical corrosion resistance, and the method comprises the steps of: the alcohol solvent is one or more of methanol, ethanol and isopropanol.
3. The method of claim 1, wherein the conductive carbon black has improved electrochemical corrosion resistance, and the method comprises the steps of: the mass ratio of the conductive carbon black to the alcohol solvent is 1: 100-1: 700.
4. a lift according to claim 1The method for resisting electrochemical corrosion of conductive carbon black is characterized by comprising the following steps: the wavelength of the pulse laser is 1064nm, the diameter of a light spot is 7mm, the pulse width is 7ns, the frequency is 5-20 Hz, and the energy density is 200-800 mJ/cm2。
5. The method of claim 1, wherein the conductive carbon black has improved electrochemical corrosion resistance, and the method comprises the steps of: the time for irradiating the conductive carbon black alcohol solution by laser is 5-20 min.
6. The method of improving the electrochemical corrosion resistance of conductive carbon black of any one of claims 1 to 5, wherein: the conductive carbon black is used as a carrier for proton exchange membrane fuel cell catalysts.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114644332A (en) * | 2022-03-01 | 2022-06-21 | 郑州大学 | Method for purifying spheroidal carbon in conductive carbon black |
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| CN114644332A (en) * | 2022-03-01 | 2022-06-21 | 郑州大学 | Method for purifying spheroidal carbon in conductive carbon black |
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