Preparation method and application of a 4h-sic integrated self-supporting photoanode
A photoanode, self-supporting technology, applied in the direction of anodic oxidation, electrode, electrode shape/type, etc., can solve the problems of carrier transport loss that is difficult to ignore, hindering the catalytic efficiency of photolysis of water, and few self-supporting photoanodes, etc. Achieve low photolysis water onset potential, high water splitting photocurrent density, and improve photocatalytic efficiency
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Embodiment 1
[0041] The preparation method of the 4H-SiC integrated self-supporting photoanode in this embodiment is as follows:
[0042] First, use acetone, absolute ethanol and deionized water to ultrasonically clean the 4H-SiC single chip (commercial 4H-SiC single chip purchased from Taiyuan Yixing Co., Ltd.) for 20 min respectively, and then use a DC power analyzer (model KEYSIGHT, N6705B ) as the electrochemical etching power supply, the cleaned 4H-SiC single wafer as the anode, and the graphite sheet as the cathode. 2 h 5 OH, HF and H 2 o 2Anodic oxidation etching of 4H-SiC single wafer was carried out in uniformly mixed etching solution (volume ratio 6:6:1); all experimental reagents used were of analytical grade.
[0043] The anodic etching process is carried out in two steps:
[0044] The first step is to remove the capping layer etching, first apply a pulse voltage with a period of 0.8s, a residence time of 0.4s, and a voltage of 19V (T 0.8s =19V 0.4s +0V 0.4s ) to etch th...
Embodiment 2
[0051] The only difference between Embodiment 2 and Embodiment 1 is that the etching time lasts for 4 minutes when the second step of continuous periodic etching is performed, and the others are the same as Embodiment 1, which will not be repeated here.
[0052] Use a scanning electron microscope (FESEM, S-4800, Hitachi, Japan) to characterize the structure of the 4H-SiC integrated self-supporting photoanode made in Example 2, and its surface SEM image is as follows Figure 6 As shown, it can be seen that it has a uniform nanopore structure with a pore diameter of about 50-70nm; its cross-sectional SEM image is shown in Figure 7 As shown, it can be seen that the depth of the etched layer of the nanohole array is about 13.3 μm.
[0053] Under the simulated sunlight irradiation of xenon lamp, Chenhua CHI-660D electrochemical workstation was used to characterize its photoelectrocatalytic performance, and the linear voltammetry scanning curve prepared at a scanning speed of 25mV / ...
Embodiment 3
[0055] The only difference between embodiment 3 and embodiment 1 is that the etching time lasts for 7 minutes when the second step of continuous periodic etching is performed, and the others are the same as embodiment 1, which will not be repeated here.
[0056] Use a scanning electron microscope (FESEM, S-4800, Hitachi, Japan) to characterize the structure of the 4H-SiC integrated self-supporting photoanode made in embodiment 3, and its surface SEM image is as follows Figure 9 As shown, it can be seen that it has a uniform nanopore structure with a pore diameter of about 50-70nm; its cross-sectional SEM image is shown in Figure 10 As shown, it can be seen that the depth of the etched layer of the nanohole array is about 15.5 μm.
[0057] The photoelectrocatalytic performance was characterized by Chenhua CHI-660D electrochemical workstation under the simulated sunlight irradiation of xenon lamp. The linear voltammetry scanning curve obtained at a scanning speed of 25mV / s is...
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