AbstractA layer-by-layer (LbL) self-assembly technique using polyallylamine hydrochloride (PAH) and polyacrylic acid (PAA) was employed to build up polyelectrolyte multi-layers on pretreated thermomechanical pulp fibres. These pretreated fibres previously had been oxidized by means of a 4-acetamido TEMPO-mediated process in order to create carboxylic functions. These allow the subsequent formation of amide bonds between PAH and fibres. X-ray photo-electronic spectroscopy (XPS) analyses confirmed the formation of amide bonds between the carboxylic function on the fibres and the primary amine function of the PAH. Besides, the surface charge intensity of the coated fibres was determined by measuring the zeta potential after each treatment step.