A high temperature and high pressure microstructure control method for electrocatalytic hydrogen production materials
A high temperature and high pressure, hydrogen material technology, applied in chemical instruments and methods, hydrogen, molybdenum sulfide and other directions, can solve the problem that the catalytic mechanism is not yet clear, and achieve the effect of simple process, high efficiency and short experiment time
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Embodiment 1
[0027] Use commercially purchased MoS with a particle size of about 3 μm 2 As the starting material, the powder is pressed into a cylinder with a diameter of 4 mm and a height of 2 mm. Put the sample into the synthetic block of the six-sided top press, use the six-sided top hydraulic press at a room temperature of 25 ° C, and the pressure is 1GPa, 3GPa, and 5GPa respectively, keep the pressure for 15 minutes, and then release it to normal pressure. The prepared samples were ground into powders in an agate mortar. X-ray diffraction and Raman results of samples prepared under different pressure conditions are shown in figure 1 and figure 2 . X-ray diffraction and Raman results show that MoS in the range of 5GPa 2 Still keep P6 3 / mmc structure, with the increase of pressure, the orientation of (001) crystal plane is slightly enhanced. It shows that in this pressure range, the long-range order of the structure is not destroyed, and only the fine-tuning effect is available ...
Embodiment 2
[0029] Using the sample prepared in Example 1, its microstructure was tested by transmission electron microscopy, and its electrocatalytic properties were tested by electrochemical workstation. See the experimental results image 3 , Figure 4 . After pressurization, MoS 2 Stacking faults appear in the steel, and the stacking fault content increases as the pressure increases, and the higher the pressure, the more obvious the distortion and overlap of the stacking faults. The test of catalytic properties shows that under acidic conditions, as the pressure increases, the properties of electrocatalytic hydrogen production first increase and then decrease, and the optimal value of properties appears at 3GPa. Therefore, the stacking faults introduced by high pressure can effectively improve the MoS 2 However, when the pressure is too high, the stacking faults will be distorted or overlapped, and its properties will decrease instead. The reason is that the microstructure stacki...
Embodiment 3
[0031] Use commercially purchased MoS with a particle size of about 3 μm 2 As the starting material, the powder is pressed into a cylinder with a diameter of 4 mm and a height of 2 mm. Put the sample into the synthetic block of the six-sided top press, use the six-sided top hydraulic press to maintain the pressure for 15 minutes under the conditions of 3GPa, 200°C, 400°C, and 600°C, and then unload it to normal pressure. The prepared samples were ground into powders in an agate mortar. X-ray diffraction and Raman results of samples prepared under different temperature conditions are shown in Image 6 and Figure 7 . X-ray diffraction results show that, relative to the starting materials, the temperature causes MoS 2 An obvious preferred orientation is formed in the (001) direction, and it can be found that at 200 °C, MoS 2 The relatively poor crystallinity indicates that its internal microstructure has more defects, and its crystallinity is relatively enhanced when the te...
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