How To Make Graphene Oxide

Introduction
Graphene has become one of the most important materials of the 21st century and there
exists a huge variety of methods for making it. Quite a few of these are well out of the
reach of the average small lab, independent researcher, inventor and experimenter.
However many of them are quite approachable and have been demonstrated in my videos
on youtube
https://www.youtube.com/user/RobertMurraySmith
Mostly, people have been interested in producing graphene and a lot of the methods get
you straight there. However, initially, the best way of making large amounts of graphene
was through a wet chemical method that first made graphene oxide and from that you
went back to graphene. As better and better methods were developed for getting straight
to graphene developed the wet chemical methods fell behind as they were dangerous,
expensive and needed practice to get right.
But, graphene oxide as a material in itself is well worth looking and and shouldnt be
abandoned in the rush for graphene.
One of the best ways of producing large amounts of graphene oxide via a wet chemical
method is by the so-called Tour method, which is an adaptation of the Hummers
method.
The Method in this guide is from the paper Improved Synthesis of Graphene Oxide that
appeared in ACSNano in July 2010. In the month that it appeared it was one of the most
downloaded of all scientific papers.
The method is really very simple, but if you are going to try it you will need a heated
stirrer as you have to stir the mix at 50 degrees centigrade for 12 hours and nobody wants
to do that by hand!
The video is at
https://www.youtube.com/watch?v=c17ePPuEaAk&index=30&list=PLbQqm4rNo6243e
69xp-ZPUkYDb38oS4xU
and is called How To Make Graphene Oxide - The Tour Method

So What Do you Need?

For something like this you need to get the good stuff. Although you can use hardware
store items the results are never going to be as good as if you buy a few items of high
grade materials. For the graphite you will need flake graphite powder you can try

ground up pencils but you are likely to be disappointed the powder size can vary from 5
microns to 150 microns. The particle size will affect the end product and what it is good
to use for. For exaple the small sizes will inkjet print but the will be less conductive than
the larger particle every thing is a trade off.
Materials
3 grams of Graphite
18 grams of Potassium Permanganate
360 mL of 96% Sulphuric Acid
40mL of 75% Phosphoric Acid
400mL of De-Ionised Water
3mL of 30-35% Hydrogen Peroxide
Equipment
A Heater Stirrer
2 Beakers 1 x 1L and 1x500mL
A Large Glass Container (a 2L Jug)
A glass Stirring Rod
A pipette able to measure 3mL
Safety Equipment
Gloves
Glasses
For Washing
200mL Water
200mL Ethanol
200mL 30% Hydrochloric Acid
Procedure
Making the Graphene Oxide is extraordinarily easy. The real problem arises because this
uses strong acids and the temperature should not be allowed to go over 55 degrees
centigrade.
1) Mix the 3g of graphite and 18 grams of potassium permanganate (a 1:6 ratio by
weight) together in the 1 Liter beaker ensuring an even mix.
2) Add 360mL of 96% sulphuric acid to the 500mL beaker, then add 40mL of 75%
phosphoric acid (a 6:1 ratio) the mixture will get a little warm wear gloves and
glasses
3) Stir the graphite and permanganate mix with one hand and add the acid mix to
with the other stirring all the while.

4) Stir until mixed

5) Place on the heater stirrer and stir at 50 degrees centigrade for 12 hours
6) Allow to cool to room temperature
7) Make ice from around 400mL of de-ionised water
8) Add the ice to the large glass container
9) Pour the graphite acid mix over the ice into the large glass container
10) Add 3mL of 30% hydrogen peroxide to mixture and stir
Congratulations you now have a jar full of graphene oxide. The next thing you need to
do is clean it.
To Clean It
You can follow the procedure in the video
https://www.youtube.com/watch?v=HICuva__6Q4&index=23&list=PLbQqm4rNo6243e
69xp-ZPUkYDb38oS4xU
Which is called Washing and Finishing Graphene Oxide After Making It and gives all the
details on how to finish the graphene oxide off.

Finish
Anyway, hope this helped and thank you for reading,
Rob.