In this paper we describe a new surface-enhanced Raman scattering (SERS)-active silver substrate that was
roughened using a combination of electrochemical triangular-wave oxidation/reduction cycles (ORCs) and
argon plasma treatment to obtain a stronger SERS effect. The mechanically polished Ag substrate was first
treated with radio-frequency-excited Ar plasma. The treated Ag substrate was then roughened through ORC
treatment in an aqueous solution containing 0.1 M KCl. Finally, this roughened Ag substrate was retreated
with radio-frequency-excited Ar plasma. Rhodamine 6G (R6G) was used as a Raman probe to evaluate the
SERS enhancement of the various Ag substrates. Encouragingly, the SERS intensity of R6G was increased
up to 8-fold, with the SERS spectrum of R6G exhibiting better resolution, when using the fully treated Ag
substrate, relative to the use of an electrochemically ORC-treated Ag substrate that had not been subjected to
plasma treatment. The improved SERS effects were related to the coalescence of grains and hills as well as
the formation of dells and pits during the electrochemical ORCs and Ar plasma roughening processes.