A method for preparing boron-doped three-dimensional graphene with supercritical carbon dioxide
A technology of carbon dioxide and graphene, which is applied in the production of bulk chemicals, electrical components, battery electrodes, etc., can solve the problems of affecting performance, structural damage, and inability to obtain graphene in one step, so as to overcome the complexity of the process and the method is simple Effect
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Embodiment 1
[0035] (1) Prepare graphene oxide solution: dissolve graphene oxide powder in tetrahydrofuran and ultrasonically disperse for 2 hours until completely dispersed; the concentration of graphene oxide is 3 mg / mL.
[0036] (2) Transfer 1ml of graphene oxide tetrahydrofuran solution to the autoclave, and add a certain amount of tetrahydrofuran borane reducing agent, the concentration of reducing agent is 0.4mol / L.
[0037] (3) Into the autoclave, the volume fraction is 99.9% high-purity CO 2 , adjust the temperature and pressure so that CO 2 Reach the supercritical state, keep constant temperature and pressure for a certain period of time, and slowly release the pressure; take out the powder, wash with acetone, and then centrifuge and dry to obtain boron-doped three-dimensional graphene. The reaction conditions are: temperature 80°C, pressure 150ATM, reaction time: 15h .
[0038] Structural and Morphological Characterization:
[0039] The obtained boron-doped three-dimensional gra...
Embodiment 2
[0043] (1) Prepare graphene oxide solution: dissolve graphene oxide powder in tetrahydrofuran and ultrasonically disperse for 2 hours until completely dispersed; the concentration of graphene oxide is 5 mg / mL.
[0044] (2) Transfer 1ml of graphene oxide tetrahydrofuran solution to the autoclave, and add a certain amount of tetrahydrofuran borane reducing agent, the concentration of reducing agent is 0.4mol / L.
[0045] (3) Pass into the high-pressure reactor with a volume ratio of 99.9% high-purity CO 2 , adjust the temperature and pressure so that CO 2 After reaching the supercritical state, the pressure will be released slowly after constant temperature and pressure for a certain period of time. The powder was taken out, washed with acetone, washed with water, and then centrifuged and dried to obtain boron-doped three-dimensional graphene. The reaction conditions were: temperature 80°C, pressure 150ATM, and reaction time: 15h.
[0046] The morphology of the three-dimensiona...
Embodiment 3
[0050] (1) Prepare graphene oxide solution: dissolve graphene oxide powder in tetrahydrofuran and ultrasonically disperse for 2 hours until completely dispersed; the concentration of graphene oxide is 10 mg / mL.
[0051] (2) Transfer 1ml of graphene oxide tetrahydrofuran solution to the autoclave, and add a certain amount of tetrahydrofuran borane reducing agent, the concentration of reducing agent is 0.8mol / L.
[0052] (3) Pass into the high-pressure reactor with a volume ratio of 99.9% high-purity CO 2 , adjust the temperature and pressure so that CO 2 After reaching the supercritical state, the pressure will be released slowly after constant temperature and pressure for a certain period of time. The powder was taken out, washed with acetone, washed with water, and then centrifuged and dried to obtain boron-doped three-dimensional graphene. The reaction conditions were: temperature 80°C, pressure 150ATM, and reaction time: 15h.
[0053] The morphology of the three-dimension...
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