School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, 30332, USA.
Chemphyschem. 2012 Nov 12;13(16):3700-6. doi: 10.1002/cphc.201200450. Epub 2012 Aug 28.
Microwaves (MWs) are applied to initialize deoxygenation of graphene oxide (GO) in the solid state and at low temperatures (∼165 °C). The Fourier-transform infrared (FTIR) spectra of MW-reduced graphene oxide (rGO) show a significantly reduced concentration of oxygen-containing functional groups, such as carboxyl, hydroxyl and carbonyl. X-ray photoelectron spectra confirm that microwaves can promote deoxygenation of GO at relatively low temperatures. Raman spectra and TGA measurements indicate that the defect level of GO significantly decreases during the isothermal solid-state MW-reduction process at low temperatures, corresponding to an efficient recovery of the fine graphene lattice structure. Based on both deoxygenation and defect-level reduction, the resurgence of interconnected graphene-like domains contributes to a low sheet resistance (∼7.9×10(4) Ω per square) of the MW-reduced GO on SiO(2) -coated Si substrates with an optical transparency of 92.7 % at ∼547 nm after MW reduction, indicating the ultrahigh efficiency of MW in GO reduction. Moreover, the low-temperature solid-state MW reduction is also applied in preparing flexible transparent conductive coatings on polydimethylsiloxane (PDMS) substrates. UV/Vis measurements indicate that the transparency of the thus-prepared MW-reduced GO coatings on PDMS substrates ranges from 34 to 96 %. Correspondingly, the sheet resistance of the coating ranges from 10(5) to 10(9) Ω per square, indicating that MW reduction of GO is promising for the convenient low-temperature preparation of transparent conductors on flexible polymeric substrates.
微波(MWs)被应用于在固态和低温(约 165°C)下引发氧化石墨烯(GO)的脱氧。MW 还原氧化石墨烯(rGO)的傅里叶变换红外(FTIR)光谱显示含氧官能团(如羧基、羟基和羰基)的浓度显著降低。X 射线光电子能谱证实微波可以在相对较低的温度下促进 GO 的脱氧。拉曼光谱和 TGA 测量表明,在低温下的等温固态 MW 还原过程中,GO 的缺陷水平显著降低,对应于精细石墨烯晶格结构的有效恢复。基于脱氧和缺陷水平的降低,相互连接的类石墨烯畴的复兴有助于 MW 还原 GO 在 SiO2 涂层 Si 衬底上的低片电阻(约 7.9×10(4)Ω/平方),在 MW 还原后在约 547nm 处具有 92.7%的光学透明度,表明 MW 在 GO 还原中的超高效率。此外,低温固态 MW 还原也应用于在聚二甲基硅氧烷(PDMS)衬底上制备柔性透明导电涂层。UV/Vis 测量表明,如此制备的 MW 还原 GO 涂层在 PDMS 衬底上的透明度范围从 34%到 96%。相应地,涂层的片电阻范围从 10(5)到 10(9)Ω/平方,表明 MW 还原 GO 有望在柔性聚合物衬底上低温制备透明导体。