Preparation method of a self-supporting transition metal dichalcogenide/carbon composite film
A transition metal and disulfide technology, applied in the field of electrochemical catalysis, can solve the problems of water pollution, energy shortage, air pollution, etc., and achieve the effects of good application prospects, excellent electrocatalytic performance, and simple and convenient process.
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Embodiment 1
[0036] Preparation of the precursor: Add 0.2g polyacrylonitrile (PAN) to 2.05g DMSO, and stir in a water bath at 60°C for 1h until the solution is uniformly mixed; after that, add 0.25g (NH 4 ) 2 MoS 4 , continue stirring in a water bath until the solution is evenly mixed.
[0037] Spin coating process: take a certain size (about 20×10mm 2 ) graphite paper (two thicknesses, 60 μm and 400 μm, respectively), and then drop a certain amount of precursor solution. When rotating the film, the rotation rate was set at 500rpm in the low-speed start-up stage, and the time was set at 10s; the high-speed rotation rate was adjusted to 6000rpm, and the time was set at 60s, so that the precursor solution was evenly spread on the graphite paper substrate to form a film, and finally placed at room temperature for It dries naturally.
[0038] CVD process: the experiment uses a tube-type resistance furnace for heating and heat preservation, and the device is as figure 1shown. Gases (argon...
Embodiment 2
[0043] Precursor preparation: Add 0.2g polyacrylonitrile (PAN) to 2.05g N,N-dimethylformamidoamine (DMF), and stir in a water bath at 60°C for 1 hour until the solution is evenly mixed; after that, add Add 0.25g (NH 4 ) 2 WS 4 , continue stirring in a water bath until the solution is evenly mixed.
[0044] Spin coating process: take a certain size (about 20×10mm 2 ) graphite paper (about 60 μm in thickness) was fixed on a glass slide, and then a certain amount of precursor solution was added dropwise. When rotating the film, the rotation rate is set at 500rpm in the low-speed start-up stage, and the time is set to 10s; the high-speed rotation rate is adjusted to 6000rpm, and the time is set to 60s, so that the precursor solution is evenly spread on the graphite paper substrate to form a film, and finally placed at room temperature to make it Let dry naturally.
[0045] CVD process: the experiment uses a tube-type resistance furnace for heating and heat preservation, and t...
Embodiment 3
[0050] The preparation of precursor and spin-coating process are identical with embodiment 2
[0051] CVD process: The experiment uses a tube resistance furnace to heat and keep warm. Gases (argon, hydrogen and hydrogen sulfide gas) are introduced into the quartz tube 2 from the outside of the tubular resistance furnace 1 (ie, the left side in the figure), and the spin-coated sample 3 is placed in the constant temperature zone of the furnace.
[0052] After sealing the quartz tube, blow nitrogen gas (300mL / min, 20min) to exhaust the air in the tube. Keep feeding nitrogen at a rate of 300mL / min, while feeding hydrogen at a rate of 60mL / min. From room temperature, the temperature was raised to 200°C over 20 minutes, and kept at 200°C for 1 hour.
[0053] Raise the temperature to 500°C at 10°C / min, keep the temperature for 1 hour, turn off the hydrogen after the heat preservation is over, and continue to raise the temperature.
[0054] After 35 minutes, the temperature was rai...
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