A kind of method of vanadium-based mxene in-situ derivative sulfide
A vanadium sulfide and sulfide technology, which is applied in the field of vanadium-based MXene in-situ derivation of sulfide, can solve the problems of large amount of waste liquid, insufficient conductivity, long test period, etc., to achieve improved material strength, high material utilization rate, The effect of simple and convenient operation
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Embodiment 1
[0034] The method for in-situ derivative sulfide of vanadium-based MXene is characterized in that: it specifically comprises the following steps:
[0035] S1: 1 g of vanadium-based MAX was etched with 1 g of sodium fluoride and 30 mL of concentrated hydrochloric acid at 85-95 °C for 72 h, centrifuged and washed with deionized water until the pH was 6, and freeze-dried to obtain 1 g of vanadium-based MXene.
[0036] S2: Take the vanadium-based MXene obtained in S1, put 0.3g into a mortar, grind it with 0.7g of sublimation sulfur and mix it thoroughly, and pour the mixture into a porcelain boat. During the grinding process, in order to prevent the generation of vanadium oxides , the ambient temperature should be less than 40 ℃;
[0037] S3: Put the porcelain boat in S2 into a tube furnace for calcination in an argon atmosphere to prepare vanadium sulfide-MXene materials. The tube furnace calcination conditions are: the argon flow rate is controlled at 20sccm, and the temperature...
Embodiment 2
[0041] S1: 1 g of vanadium-based MAX was etched with 1 g of sodium fluoride and 30 mL of concentrated hydrochloric acid at 85-95 °C for 72 hours, centrifuged and washed with deionized water until the pH was 6, and freeze-dried to obtain 1 g of vanadium-based MXene;
[0042] S2: Take the vanadium-based MXene obtained in S1, put 0.1 g of it into a mortar, grind it with 0.4 g of sublimated sulfur, and mix it thoroughly, and pour the mixture into a porcelain boat. During the grinding process, in order to prevent the generation of vanadium oxides , the ambient temperature should be less than 40 ℃;
[0043] S3: Put a lid on the porcelain boat containing the mixture of MXene and sulfur powder in S2 to ensure that the sulfur can fully contact MXene, and then put it into a tube furnace for calcination in an argon atmosphere to prepare the vanadium sulfide-MXene material. The calcination conditions of the furnace were as follows: the flow rate of argon was controlled at 15 sccm, the tem...
Embodiment 3
[0047] S1: 1 g of vanadium-based MAX was etched with 1 g of sodium fluoride and 30 mL of concentrated hydrochloric acid at 85-95 °C for 72 h, centrifuged and washed with deionized water until the pH was 6, and freeze-dried to obtain 1 g of vanadium-based MXene;
[0048] S2: Take the vanadium-based MXene obtained in S1, put 0.1 g of it into a mortar, grind it with 0.4 g of sublimated sulfur and mix it thoroughly, and pour the mixture into a porcelain boat. During the grinding process, in order to prevent the generation of vanadium oxides , the ambient temperature should be less than 40 ℃;
[0049] S3: Cover the porcelain boat with the mixture of MXene and sulfur powder in S2, and then cover it with a layer of porcelain boat, and then put it into a tube furnace for calcination in an argon atmosphere to prepare the vanadium sulfide-MXene material. The tube furnace roasting conditions are: The flow rate of argon gas was controlled at 15sccm, the temperature was raised to 500°C at ...
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