For the first time, we have investigated the beneficial effects of non-cavitating coupling fluids and their moderate overpressures in enhancing mass-transfer and acoustic energy transfer in a double cell micro-sonoreactor. Silicon and engine oils of different viscosities were used as non-cavitating coupling fluids. A formulated monoethylene glycol (FMG), which is a regular cooling fluid, was also used as reference. It was found that silicon oil yielded a maximum acoustic energy transfer (3.05 W/cm2) from the double jacketed cell to the inner cell volume, at 1 bar of coupling fluid overpressure which was 2.5 times higher than the regular FMG cooling fluid. It was also found that the low viscosity engine oil had a higher acoustic energy value than that of the high viscosity engine oil. In addition, linear sweep voltammograms (LSV) were recorded for the quasi-reversible Fe2+/Fe3+ redox couple (equimolar, 5 × 10-3 M) on a Pt electrode in order to determine the mass-transport limited current density (jlim) and the dimensionless Sherwood number (Sh). From the LSV data, a statistical analysis was performed in order to determine the contribution of acoustic cavitation in the current density variation |Δj|average. It was found that silicon oil at 1 bar exhibited a maximum current density variation, |Δj|average of ~2 mA/cm2 whereas in the absence of overpressure, the high viscosity engine oil led to a maximum |Δj|average which decreased gradually with increasing coupling fluid overpressure. High viscosity engine oil gave a maximum Sh number even without any overpressure which decreased gradually with increasing overpressure. The Sh number for silicon oil increased with increasing overpressure and reached a maximum at 1 bar of overpressure. For any sonoelectrochemical processes, if the aim is to achieve high mass-transfer and acoustic energy transfer, then silicon oil at 1 bar of overpressure is a suitable candidate to be used as a coupling fluid.