I am planning to anneal monolayer graphene on SiO2 grown by CVD process, 400oC in Ar gas atmosphere for complete removal of PMMA, In this process I can either use Ar gas or vacuum.(If both used simultaneously vacuum will be released and vacuum pump exhausts oil out) Any suggestions how to implement this?
Lot of discussion in RG regarding your question.
https://www.researchgate.net/post/Removal_of_PMMA_residue_from_graphene_surface-any_thoughts?_sg=WDb871BPC%2B9T4nXuHa5wSoK4zJm99ZhMIzc%2Bx5B37gWuFwQ%2BicruNdlhaZO0IDpR_N5iR7Gb%2BsYLXMIgse5a3ELlTvq2OSEoTKy2GDRlOLqnKhgttmrg2kbVmzonL%2BTrc_o402kzT%2BlUStRji98VVHAp5iLtbbA1jkDmSCK4h9%2BYqrzIEplk8aiRbKBVVlL8dp&_tpcectx=search
https://www.researchgate.net/post/Dissolving_of_PMMA_layer?_sg=hRAww5vWlLqFf%2FPC%2Bx5chl4Guo6KEBeRbvW9b872gqcsxbLQr%2BbzVuq8MY713CEV_%2FXGsdybyTK5LVlrTiZvPyYKco0MWwqrWv%2BQQmaQ%2B8dsZ2l8YnRWUU1RVZHcWcNjJ_JlvsW9TbKxFAVHuEzfqPCvyKbt%2FBl3XiUvmHX%2FKcsaFXokZaPeMPW8D8HzUKXBM4&_tpcectx=search
https://www.researchgate.net/post/How_can_I_remove_PMMA_Polymethyl_methacrylate_residue_from_graphene_surface?_sg=jFU0D97YiSajX1rKC2sdx4lyr4FR47sJ5WZhUx6V7rhT2HPftoiMip20zcoce8Xl_uXIB8LY87yQBuixHU1teQDDaxE2z%2FVf73B594OrP1ib5FjYGHwmTlVuvexW7dZpS_3UyUnL8%2FaK9fjiU56cTdH8yh1Ou8B3kBFhbSF35n3wxcTqEN7B%2FcD6LIUTCmfB%2Bg&_tpcectx=search
https://www.researchgate.net/post/Im_trying_to_remove_PMMA_layer_on_top_of_graphene_on_a_SiO2_substrate_using_acetone_how_can_I_reduce_washing_away_the_sample_when_removing_the_PMMA?_sg=mogke86xed36PezVOzGo86eCbikrgitNGFx2vvR7%2BquE0qrz29gzr5VjeNAhwNV%2B_ZvcxcRrk23wknBR0PYVOA33PXH45t8MJd%2FEa%2FG6vkV21JjFce61pKc2aEhOEmWza_h29Og9TEXln0rN4XsaEq2sCZOy495khTFOXXuMtXFiiHXGujjew2zOgNMFRKkViY&_tpcectx=search
https://www.researchgate.net/post/How_can_I_obtain_PMMA_free_Polymer_free_surface_after_transferring_single_or_a_few_layers_of_graphene_on_a_target_substrate?_sg=KReaTbCiGz%2BHNmIKEcT0nGkIRcoKxm10hpp2F12lApX2O9AJF%2F3NckP5mao2YrZp_gvE45WnHl%2BXy0YeY3Nq5xCHG8k0Oy%2FgX1ODYbq3rqFgR0GmRPUglNDEFxkziaktG_xF4h%2FjUKY%2BZYwMsZOZS2LsoWlMUWN0%2BODNqAINCC3YbzbuMf%2BYAMD8IUFVQ8FspH&_tpcectx=search
Before annealing step.. you can partially or completely remove PMMA with acetone.. see this paper from Ruoff group: doi: 10.1063/1.3643444 and many more papers on this topic.
Rather than using vacuum or pure Ar environment for annealing, use Ar/H2... H2 helps in defect healing and improves conductivity.
Use a dry vacuum pump instead of oil one. Small pumps are available for ~Rs.10,000/-. Some bigger anneal systems use small 'fill and evacuate' cycles for anneal in an atmosphere.
Lot of discussion in RG regarding your question.
https://www.researchgate.net/post/Removal_of_PMMA_residue_from_graphene_surface-any_thoughts?_sg=WDb871BPC%2B9T4nXuHa5wSoK4zJm99ZhMIzc%2Bx5B37gWuFwQ%2BicruNdlhaZO0IDpR_N5iR7Gb%2BsYLXMIgse5a3ELlTvq2OSEoTKy2GDRlOLqnKhgttmrg2kbVmzonL%2BTrc_o402kzT%2BlUStRji98VVHAp5iLtbbA1jkDmSCK4h9%2BYqrzIEplk8aiRbKBVVlL8dp&_tpcectx=search
https://www.researchgate.net/post/Dissolving_of_PMMA_layer?_sg=hRAww5vWlLqFf%2FPC%2Bx5chl4Guo6KEBeRbvW9b872gqcsxbLQr%2BbzVuq8MY713CEV_%2FXGsdybyTK5LVlrTiZvPyYKco0MWwqrWv%2BQQmaQ%2B8dsZ2l8YnRWUU1RVZHcWcNjJ_JlvsW9TbKxFAVHuEzfqPCvyKbt%2FBl3XiUvmHX%2FKcsaFXokZaPeMPW8D8HzUKXBM4&_tpcectx=search
https://www.researchgate.net/post/How_can_I_remove_PMMA_Polymethyl_methacrylate_residue_from_graphene_surface?_sg=jFU0D97YiSajX1rKC2sdx4lyr4FR47sJ5WZhUx6V7rhT2HPftoiMip20zcoce8Xl_uXIB8LY87yQBuixHU1teQDDaxE2z%2FVf73B594OrP1ib5FjYGHwmTlVuvexW7dZpS_3UyUnL8%2FaK9fjiU56cTdH8yh1Ou8B3kBFhbSF35n3wxcTqEN7B%2FcD6LIUTCmfB%2Bg&_tpcectx=search
https://www.researchgate.net/post/Im_trying_to_remove_PMMA_layer_on_top_of_graphene_on_a_SiO2_substrate_using_acetone_how_can_I_reduce_washing_away_the_sample_when_removing_the_PMMA?_sg=mogke86xed36PezVOzGo86eCbikrgitNGFx2vvR7%2BquE0qrz29gzr5VjeNAhwNV%2B_ZvcxcRrk23wknBR0PYVOA33PXH45t8MJd%2FEa%2FG6vkV21JjFce61pKc2aEhOEmWza_h29Og9TEXln0rN4XsaEq2sCZOy495khTFOXXuMtXFiiHXGujjew2zOgNMFRKkViY&_tpcectx=search
https://www.researchgate.net/post/How_can_I_obtain_PMMA_free_Polymer_free_surface_after_transferring_single_or_a_few_layers_of_graphene_on_a_target_substrate?_sg=KReaTbCiGz%2BHNmIKEcT0nGkIRcoKxm10hpp2F12lApX2O9AJF%2F3NckP5mao2YrZp_gvE45WnHl%2BXy0YeY3Nq5xCHG8k0Oy%2FgX1ODYbq3rqFgR0GmRPUglNDEFxkziaktG_xF4h%2FjUKY%2BZYwMsZOZS2LsoWlMUWN0%2BODNqAINCC3YbzbuMf%2BYAMD8IUFVQ8FspH&_tpcectx=search
After transferring graphene to substrate, use acetic acid for removal of PMMA. It is very effective. It will avoid extensive annealing. Then, annealing in vacuum of Ar/.H2 will solve the left residues. But there is no complete removal, you may find very clean area also the area with residues depending on the uniformity of PMMA thickness. It is also influenced by the folds, wrinkles on graphene after transfer. But still I found acetic acid more effective than any other chemical.
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