Materials and methods for graphene synthesis

Method 1:
Chemicals and materials:

1. Natural graphite
2. Sodium nitrate
3. Sulfuric acid
4. Potassium permanganate
5. Hydrogen peroxide
6. Hydrochloric acid
7. Ammonium hydroxide
8. Ethanol
9. Deionized water

Synthesis of graphene oxide

 Pour 23 ml of H2SO4 into a beaker in an ice bath at 0 degrees
 Add 1.5g of graphite powder and stir for 5 mins. A dispersion is formed
 Add 0.5g of sodium nitrate and stir for 30 mins
 Remove the solution from ice bath
 Add 3g of potassium permanganate with stirring
 Leave the solution for 1 hr to react
 Gradually add 40ml of deionized water and stir for 30 mins
 Further add 100ml of deionized water slowly for further dilution
 Keep the solution at 70 degrees for 1 hour
 Add 30 ml of deionized water and H2O2
 Filter the solution
 Wash graphite oxide powder with 5% HCl solution
 Again wash GtO powder with deionized water
 Dry powder at 60 degrees
 Dissolve GtO powder into deionized water to obtain yellow brown dispersion
 Ultrasonicate this solution for 2 hrs
 Centrifuge the solution
 Dry at 60 degrees

Reduction by ammonium hydroxide

25 mL of ammonia was mixed into 25 mL of deionized water in beaker. Then the solution was
stirred for 30 min at 25 °C to get homogenized ammonia solution. 1.0 g of synthesized GO was
then added into ammonia water and stirred. This solution was kept directly into the microwave
frequency system for 60 min. The reduced graphene
sheets were settled at the bottom of the beaker and easily be separated after cool down the
solution at room temperature. The graphene sheets were obtained finally after washing with
deionized water and drying at 60 °C. Graphene sample product was labeled as GA.
Reduction using plant extract
1.0 g prepared GO was suspended into 90 mL of deionized water to obtain brown dispersion and
stirred until homogenize. Then 10 mL of plant extract was gradually added into the solution
while stirring. This dispersion was directly placed into the microwave generated system for
60 min by setting microwave oven at low power. Graphene product was settled at the bottom of
the solution and separated after cooling at room temperature. Finally, graphene sheets were
obtained after three times washing with deionized water. The product was dried at 60 °C and
labeled as GP.
Reduction using aloe vera
To 80 mL distilled water, 0.04 g of GO powder was added and the suspension was ultra-
sonicated for about 30 min. As purchased AV with different masses (3, 7.5 and 12 g) were added
to 10 mL deionized water and stirred for 10 min. AV solution was then added to the GO
suspension and was re uxed for 24 h at 95 _C. A er the reaction, the suspension was
centrifuged at ca. 3000 rpm. The black powder thus obtained was washed with distilled water
many times, then with ethanol and dried in air.

Method 2
Synthesis of graphene oxide

GO sheets were synthesized by a modified Hummers’ method.31 It started with graphite pretreatment.
To accomplish this, 12 g of graphite powder were added to an 80 °C solution of 50 mL of concentrated
H2SO4, 10 g of K2S2O8, and 10 g of P2O5. The mixture was reacted for 6 h, after which it was diluted
with 2 L of water, filtered, and washed using a 0.2 µm Nylon Millipore filter and dried in air overnight.
For the following oxidation step, 460 mL of H2SO4 were chilled to 0 °C using an ice bath. The oxidized
graphite was added to the acid and stirred. Then, 60 g of KMnO4 were added slowly with temperature
controlled below 10 °C. This mixture was allowed to react at 35 °C for 2 h, after which 920 mL of distilled
water were added slowly so as to keep the temperature below 50 °C. After further reaction for 2 h, 2.8 L
of water and 50 mL of 30% H2O2 were added, resulting in a brilliant yellow color along with bubbling.
The mixture was allowed to settle for at least a day before the supernatant was decanted. The
remaining mixture was then centrifuged and washed with a total of 5 L of 10% HCl solution followed by
5 L of water to remove the acid. The resulting solid was subjected to dialysis for a week to remove
remaining metal ions and acids. Finally, the product was vacuum-dried

Reduction by sugar
2 g glucose was added into 250 mL of homogeneous GO dispersion (0.5 mg/mL), followed by stirring for
30 min. Then 1 mL ammonia solution (25% w/w) was added to the resulting dispersion. After vigorously
shaking for a few minutes, the mixture was stirred for 60 min at 95 1C. The resulting black dispersion
was then filtered and washed with water for several times and the obtained GNS was redispersed in
water for further use.