A kind of amine-based reinforced graphene film, nitrogen-doped graphene film and preparation method thereof
A nitrogen-doped graphene and graphene film technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems of limiting large-scale and continuous preparation of graphene films, difficult to disperse and coordinate solidification, and impossible solidification and molding. , to achieve the effect of easy operation, simple operation and widening range
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Embodiment 1
[0035] The preparation method of graphene oxide solution:
[0036] Add 10g of graphite, 150ml of 98% sulfuric acid, and 30ml of nitric acid into a 500ml Erlenmeyer flask and stir at room temperature for 24 hours, slowly pour it into 1L of water to collect the solid, wash it 3 times, and dry it at 80°C for 4 hours. Repeat the pre-oxidation process twice. The dried pre-oxidized graphite was put into a box furnace and thermally expanded at 900°C for 20s to obtain thermally expanded graphite oxide. In a 500ml wide-mouth Erlenmeyer flask, mix 5g of heat-expandable graphite oxide with 300ml of sulfuric acid, 5g of K 2 S 2 o 8 , 7g of phosphorus pentoxide mixed and heated at 80°C for 4 hours, diluted with 2L of water, filtered and washed, dried in air for 3 days to obtain pre-oxidized thermally expandable graphite. Mix dry pre-oxidized heat-expandable graphite with 200ml of sulfuric acid at a low temperature of 0-5°C, add 20g of potassium permanganate, add slowly, stir at 35°C fo...
Embodiment 2
[0039] The preparation method of graphene oxide solution is as embodiment 1.
[0040] Extrude a 30mg / mL graphene oxide solution at a extrusion speed of 10mL / h in a device with a flat inline die, with a die height of 100μm and an aspect ratio > 5, in ethylenediamine at 60°C and sodium citrate mixed solution (the mass fraction of ethylenediamine is 20%, the mass fraction of sodium citrate is 20%), stay in 8h, solidify and form a film by reducing self-assembly, and obtain amine-based reinforced graphite after drying at 85°C for 4h olefin film; wherein, the percentage is the mass percentage of each component relative to the mixed liquid. The thickness, tensile strength, elongation at break and electrical conductivity of the obtained amine-based reinforced graphene film are shown in Table 1.
Embodiment 3
[0042] The preparation method of graphene oxide solution is as embodiment 1.
[0043] Extrude 10mg / mL graphene oxide solution at a rate of 100mL / h through a device with a flat inline die. The die height is 500 μm and the aspect ratio is >5. The mixed solution of ethylene tetramine and sodium bisulfite (the mass fraction of ammonia water is 30%, the mass fraction of triethylene tetramine is 5%, the mass fraction of sodium bisulfite is 40%) stays in 24h, self-assembles by reduction Solidify into a film, and dry at 75°C for 12 hours to obtain an amine-reinforced graphene film; wherein, the percentages are the mass percentages of each component relative to the mixed solution. The thickness, tensile strength, elongation at break and electrical conductivity of the obtained amine-based reinforced graphene film are shown in Table 1.
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