Preparation method of nitrogen-doped carbon shell coated molybdenum carbide core microsphere material with core-shell structure
A technique of wrapping molybdenum carbide and core-shell structure, which is applied in the preparation/purification of carbon, tungsten/molybdenum carbides, carbides, etc., can solve the problems of hydrogen evolution activity to be improved, complex synthesis steps, etc. Synthesize simple, novel structure effects
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Embodiment 1
[0020] After adding 3 g of guanosine and 0.8 mL of sulfuric acid into 50 mL of aqueous solution, they were fully dissolved in a water bath at 80 °C until the solution was transparent, and 3 g of ammonium heptamolybdate was weighed into the solution, stirred for 5 min, and then transferred to In the lining of the hydrothermal kettle; put the hydrothermal kettle into the oven and heat it at 180 °C for 2 h, let it cool down to room temperature naturally, then wash and filter with water, dry at 60 °C for 24 h, and then obtain the precursor; The obtained precursor was ground into powder, and heated at a heating rate of 10 °C / min in 10% H 2 / N 2 Under the atmosphere, the temperature was raised from 30 °C to 350 °C, and the temperature was kept for 1 h, and the temperature was continued to rise to 750 °C, and the temperature was kept for 2 h. Cool naturally to room temperature and grind to obtain molybdenum carbide microsphere material with core-shell structure. Named Mo 2 C@NC-T ...
Embodiment 2
[0022] After adding 3 g of guanosine and 0.8 mL of sulfuric acid into 50 mL of aqueous solution, fully dissolve it in a water bath at 80 °C until the solution is transparent, weigh 3 g of ammonium heptamolybdate into the solution, stir for 5 min, and transfer the solution to water In the lining of the hot kettle; put the hydrothermal kettle into the oven and heat it at 180 °C for 6 h, wait for it to cool down to room temperature naturally, then wash and filter with water, and dry at 60 °C for 24 h to obtain the precursor; the obtained precursor The body was ground into powder, and heated at a rate of 10 °C / min in 10% H 2 / N 2 Under atmosphere, heat up from 30 ℃ to 350 ℃, stay for 1 h, continue to heat up to 750 ℃, stay for 2 h, cool down to room temperature naturally, and grind to get molybdenum carbide microsphere material with core-shell structure. Named Mo 2 C@NC-T 6 .
Embodiment 3
[0024] After adding 3 g of guanosine and 0.8 mL of sulfuric acid into 50 mL of aqueous solution, they were fully dissolved in a water bath at 80 °C until the solution was transparent, and 3 g of ammonium heptamolybdate was weighed into the solution, stirred for 5 min, and then transferred to In the lining of the hydrothermal kettle; put the hydrothermal kettle into the oven and heat it at 180 °C for 12 h, wait for it to cool down to room temperature naturally, then wash and filter with water, and dry at 60 °C for 12 h to obtain the precursor; The obtained precursor was ground into powder, and heated at a rate of 10 °C / min in 10% H 2 / N 2 Under atmosphere, heat up from 30 ℃ to 350 ℃, stay for 1 h, continue to heat up to 750 ℃, stay for 2 h, cool down to room temperature naturally, and grind to get molybdenum carbide microsphere material with core-shell structure. Named Mo 2 C@NC-T 12 .
[0025] figure 1 It is the STEM Mapping diagram of the molybdenum carbide material obta...
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