I have synthesized graphene by our home built ethanol cvd setup earlier, but now I am not able to get large area graphene on copper, because there is a huge white contamination of 100 nm order. Thank you
SiO2 contamination is possible, however post-reaction XPS measurements will most likely indicate mainly Si-C bonds, as SiO2 is carbothermally reduced in the conditions for Gr growth (aprox 950 C, >1h, 1 Torr?)
Indeed. I have yet to understand or read anything on that phenomenon. We limited the contamination by successively using several quartz tubes, that way their lifespan increases.
However, some papers talk about the reactivity of graphene edges which might be why you see those particles there (although I think in literature not thoroughly studied yet), look in the attached file, and in the following references:
Zhang, X. Y.; Wang, L.; Xin, J.; Yakobson, B. I.; Ding, F. J Am Chem Soc 2014, 136, (8), 3040-3047.
Wang, X. R.; Dai, H. J. Nat Chem 2010, 2, (8), 661-665.
but they do not experience this SiO2 contamination.
We suffered with our home built CVD by an increasing in time SiO2 contamination on graphene, we are almost sure it's caused by aging of the tube quartz mounted in our system, partially due to copper oxides penetration in quartz structure. We carefully avoided the use of vacuum grease inside the CVD chamber.
SiO2 contamination on our samples, appear, at SEM observation, as white sphere with a diameter about 10-100 nm. It seems deposited preferentially on copper boundary grain and in competition with graphene growth.
We partially resolver the problem changing frequently the tube with a new one, before it deteriorates. You can also do a post treatment on graphene with HF to remove the SiO2.
Hi Xiao, There was two type of contamination one from dirty quartz tube and another from silica vacuum grease. Size of white contaminated particle was 20 nm and 200 nm which came from quartz tube and silica grease respectively. If O ring for sealing the vacuum at a longer distance from furnace so there was no any contamination due to silica vacuum grease. We have replaced my quartz tube with a longer quartz tube which solve my both problem. Thanks.