Macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and preparation method
A graphene aerogel and composite material technology, which is applied in the field of macroscopic three-dimensional Fe3O4 graphene aerogel ultra-light composite material and preparation, and achieves the effects of mild reaction conditions, simple preparation and easy mass production
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Embodiment 1
[0033] Step 1, pretreatment graphite powder
[0034] At room temperature and under magnetic stirring conditions, add 35 g of graphite powder to 520 mL of a mixed acid solution (1:3) of concentrated nitric acid and concentrated sulfuric acid and stir for 24 hours. Add high-purity water to dilute to 1.5L, and then filter and wash to neutrality (pH = 7) with a glass sand core filter device with a filter membrane pore size of 0.45 μm to obtain a filter cake, and dry the obtained filter cake at 60°C for 2 After a few days, it was ground and processed in batches at 1100°C for 30s to obtain pretreated graphite powder.
[0035] Step 2, preparing graphene oxide solution
[0036] Using the pretreated graphite powder obtained in step 1 as raw material, the graphite oxide solution was prepared by the traditional Hummer method, and then the graphene oxide solution was obtained by ultrasonic stripping, with a concentration of about 4.0 mg / mL.
[0037] Step 3, preparing ferric hydroxide co...
Embodiment 2
[0048] Step one to step three are the same as embodiment 1.
[0049] Step 4, preparation of macroscopic three-dimensional Fe 3 o 4 Graphene airgel ultra-light composite material:
[0050] Fe(OH) 3 The mass ratio with graphene oxide is 1: 1,
[0051] ① Take 15 mL of the graphene oxide solution prepared in step 2 and dilute it with 15 mL of high-purity water, then adjust its pH to 9 with ammonia water under magnetic stirring, and then sonicate for 1 hour to prepare a diluted graphene oxide solution;
[0052] ② At room temperature, the 1.8mLFe(OH) prepared in step 3 3 Add the colloid dropwise to the diluted graphene oxide solution prepared in ①, and stir for 1 hour to make a reaction solution;
[0053] ③ Transfer the reaction solution prepared in ② into a 50mL hydrothermal kettle, and let it stand at 180°C for 24h; then cool the hydrothermal kettle to room temperature to obtain Fe 2 o 3 Graphene hydrogel;
[0054] ④ Fe to be obtained 2 o 3 The graphene hydrogel was move...
Embodiment 3
[0058] Step one to step three are the same as embodiment 1.
[0059] Step 4, preparation of macroscopic three-dimensional Fe 3 o 4 Graphene airgel ultra-light composite material:
[0060] Fe(OH) 3 The mass ratio with graphene oxide is 1.5: 1,
[0061] ① Take 15 mL of the graphene oxide solution prepared in step 2 and dilute it with 15 mL of high-purity water, then adjust its pH to 9 with ammonia water under magnetic stirring, and then sonicate for 1 hour to prepare a diluted graphene oxide solution;
[0062] ② At room temperature, the 2.7mLFe(OH) prepared in step 3 3 Add the colloid dropwise to the diluted graphene oxide solution prepared in ①, and stir for 1h;
[0063] ③ Transfer the reaction solution prepared in ② into a 50mL hydrothermal kettle, and let it stand at 180°C for 24h; then cool the hydrothermal kettle to room temperature to obtain Fe 2 o 3 Graphene hydrogel;
[0064] ④ Fe to be obtained 2 o 3 The graphene hydrogel was moved to ammonia water with a con...
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