In the present work, the adhesion between substrates treated with identical polyelectrolyte multilayers (PEM) from polyallylamine hydrochloride (PAR) and poly(acrylic acid) (PAA) was studied using atomic force microscopy (AFM) and the Surface force apparatus (SFA). The AFM measurements, conducted under wet conditions for PEMs formed at pH 7.5, showed a higher adhesion (pull-off force) when PAH was adsorbed in the outermost layers. There was also a difference depending on the Molecular mass of the polymers, demonstrating a greater adhesion for the low molecular mass combination of polyelectrolytes. Furthermore, die time in contact showed to be of importance, with increasing pull-off forces with contact time at maximum load. The SFA measurements were conducted under dry conditions, at 100% RH, and under wet conditions for PEMs adsorbed at pH 7.5/3.5. The SFA adhesion measurements showed that under dry conditions, the adhesive forces between two high energetic mica substrates were lowered when they were covered by PEMs before the measurements. The thickness of the adsorbed layers was also measured using SFA. This showed that there was a significant swelling when the dry layers were exposed to 100% RH or to wet conditions. The swelling was higher, indicating a less rigid layer, when PAH was adsorbed in the outermost layer than when the PEM was capped with PAA.