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Nano-second temporal particle behavior in high-power impulse magnetron sputtering discharge in a cylindrical cathode

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Graphene films were exposed to low-pressure capacitively coupled (E-mode) and inductively coupled (H-mode) argon radio frequency plasmas to investigate damage formation by very-low-energy ion irradiation. In the H-mode, plasma parameters were assessed by a Langmuir probe and plasma sampling mass spectrometry to determine the conditions of fixed ion fluence but with different average ion energies. The populations of argon metastable and resonant argon atoms were also measured by optical absorption spectroscopy to determine their contribution to the total energy flux during plasma treatment. In the H-mode, in which plasma-graphene interactions are dominated by ion irradiation effects, Raman spectroscopy reveals a significant rise in the D/G ratio and full width at half maximum of the G peak as well as the onset of graphene amorphization, even at very low ion energies (between 7 and 13 eV). In the E-mode characterized by comparable ion energy but much lower ion density, significant damage is also observed, a feature ascribed to the additional energy flux linked to the de-excitation of metastable argon species on the graphene surface.

Raman spectroscopy provides rich optical signals that can be used, after data analysis, to assess if a graphene layer is pristine, doped, damaged, functionalized, or stressed. The area being probed by a conventional Raman spectrometer is, however, limited to the size of the laser beam (∼1 µm); hence, detailed mapping of inhomogeneities in a graphene sample requires slow and sequential acquisition of a Raman spectrum at each pixel. Studies of physical and chemical processes on polycrystalline and heterogeneous graphene films require more advanced hyperspectral Raman capable of fast imaging at a high spatial resolution over hundreds of microns. Here, we compare the capacity of two different Raman imaging schemes (scanning and global) to probe graphene films modified by a low-pressure plasma treatment and present an analysis method providing assessments of the surface properties at local defects, grain boundaries, and other heterogeneities. By comparing statistically initial and plasma-treated regions of graphene, we highlight the presence of inhomogeneities after plasma treatment linked to the initial state of the graphene surface. These results provided statistical results on the correlation between the graphene initial state and the corresponding graphene–plasma interaction. This work further demonstrates the potential use of global hyperspectral Raman imaging with advanced Raman spectra analysis to study graphene physics and chemistry on a scale of hundreds of microns.