I need a complete procedure for making single layer graphene using CVD and copper foil (25 um thickness).
Particularly concentration of solution used for cleaning like acetic acid or HCl etc
I have used the following procedure:
1) Chemical cleaning: aceton -> isopropanol -> ethanol - DI water. 10 min. for every solution in the ultrasonic bath
2) Annealing in Hydrogen atmosphere: 30 min at 1000 degree C
You ccould see details in the attached paper.
Article Durability and degradation mechanism of graphene coatings de...
Oleksiy did u treat copper with any acid for removing oxide, i need that concentration o f acid to remove oxide layer
No, I didn't use any acid. The oxyde layer was removed during annaling in the Hydrogen atmosphere.
Standard lab grade acetic acid I have used for 5 min to remove the oxide layer. if it not works, keep Cu substrates in FeCl3 solution for 1 min to remove the top layer of Cu.
Best Wishes.
If you use 100 micron Cu foil then you can recrystallize top surface and used chemical hand polishing method to get very large area monolayer Gr.
1. Annealing 1050 / 1060 C
Annealing time = around 5 hr (Ramping up time = 30 min to 1 hr, Steady temp time = 5 hrs)
Gas condition Ar:H2 :: 5:1
2. Chemical polishing:
- Take Cu etchant with different dilutation. At least 4-5 dilutation of Cu etchant with water
- High concentration Cu etchant will smooth up the Cu substrate, but it will oxidized the Cu substrate also
- Rub with diluted Cu etchant to remove the majority of oxide
- Rub with more diluted etchant to romve more oxide
- Reapet these procesess untill all of the Oxide removes and Substrate looks clean and shiny
- Rub with water at the end to remove CuCl3 from the substrate
After these you will get something like this attached image..
Good luck..
You can use 0.1 M diluted HCL solution to clean the Cu substrate, It will help you to remove the native oxide from the substrate, good luck!
It depends which particular CU foil you are using... there are some Cu foils from Alfa Aesar which have some coatings which must need to remove.... The best is use Acetic acid to clean Cu foil, just immerse Cu foil piece in it for 2-5 minutes and remove and rinse with water and blow dry with N2, the one with HCl and FeCl3/HCl etch the surface a bit which is not that good for growth. I hope this will help.
Best
Irfan
You can find a very complete investigation of that matter in the supplementary information associated to my article 10.1039/C8NR09841G. Many methods are available, some inefficient, for instance acetic acid is indeed inefficient if you have a coating (as mentioned by Irfan) with certain types of commercial foils. I also have tried several techniques mentioned to work in the literature, but to no avail in my case. Obtaining a cleaning technique efficient in all cases is not trivial. It really depends on what graphene quality you want to get in the end. So it is really to be tested in your specific case. Regards.
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