N-doped graphene preparation method and application of N-doped graphene
A technology of nitrogen-doped graphene and graphene solution, applied in the direction of graphene, nano-carbon, etc., can solve the problems of not being able to be applied on a large scale and being expensive, and achieve the effects of low cost, good stability and simple preparation process
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[0032] A preparation method of nitrogen-doped graphene, comprising the following steps:
[0033] 1) Dissolution of graphene oxide solid
[0034] Add graphene oxide solids into water and ultrasonically disperse for 30-240 minutes to form a uniformly dispersed graphene oxide solution with a concentration of 0.1-2.0 g / L;
[0035] 2) Reduction of hydrazine hydrate to obtain reduced graphene oxide solution
[0036] Put an ammonia solution with a mass fraction of 25% to 28% into the graphene oxide solution in step 1), and adjust the pH value of the graphene oxide solution to 9 to 11, and then add the graphene oxide solution with the graphene oxide solution A hydrazine hydrate solution with a volume ratio of 1:20 to 1:150 and a concentration of 1 mol / L is stirred for 30 to 60 minutes to obtain a mixed solution, and then the mixed solution is heated to 95°C and reacted for 1 hour to obtain a reduced state graphene oxide solution, and then directly cool the reduced state graphene oxi...
Embodiment 1
[0044] After adjusting the pH value of the graphene oxide solution to 10.02 with ammonia water, add a 1mol / L hydrazine hydrate solution with a volume ratio of 1:100, and then add a volume ratio of 1:25 with a mass fraction of 50% cyanide after the reduction reaction is completed. The amine aqueous solution is controlled by rotary evaporation with water temperature of 50° C., rotation rate of 100 rpm, and vacuum of 50 mbar to remove water to obtain a cyanamide-reduced graphene oxide composite material. The roasting conditions were then controlled to be a roasting temperature of 900° C., roasting for 60 min, and an argon flow rate of 50 mL / min. The product was cleaned with double distilled water and 50% ethanol solution respectively to obtain black powder nitrogen-doped graphene. In the 0.1mol / L, pH=7 phosphate buffer, the oxygen reduction electron transfer number was 3.75.
Embodiment 2
[0046] After adjusting the pH value of the graphene oxide solution to 10.02 with ammonia water, add a 1mol / L hydrazine hydrate solution with a volume ratio of 1:100, and then add a volume ratio of 1:25 with a mass fraction of 50% cyanide after the reduction reaction is completed. The amine aqueous solution is controlled by rotary evaporation with water temperature of 50° C., rotation rate of 100 rpm, and vacuum of 50 mbar to remove water to obtain a cyanamide-reduced graphene oxide composite material. The roasting conditions were then controlled to be a roasting temperature of 1000° C., roasting for 60 min, and an argon flow rate of 100 mL / min. The product was cleaned with double distilled water and 50% ethanol solution respectively to obtain black powder nitrogen-doped graphene. In the 0.1mol / L, pH=7 phosphate buffer, the oxygen reduction electron transfer number was 3.91.
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