A surface rejuvenation process was developed for generation variable thickness of metal deposits on polymer microspheres via electroless plating. Thus, Ni(II), Cu(II) and Ag(I) complexes formed on triethylenetetramine (TETA) functional crosslinked poly( glycidyl methacrylate) (PGMA) microspheres were reduced to zero-valent metals. The resulting metals (1.1-1.5 mmol g(-1)) were employed as seed points for electroless metal plating (self-seeding) without using Pd or tin pre-activating species. Treatment of the metalized surfaces with hydrazine or hydrazinium formate was demonstrated to reactivate (rejuvenate) the surface and allows further metal deposition from electroless plating solutions. Followed repeating of the surface rejuvenation-metalization steps resulted in step wise increasing of the metal deposits (90-290 mg per g in each cycle), as inferred from metal analyses, ESEM and XPS analysis. Experiments showed that, after 6 times of cycling the metal deposits exceed 1 g per g of the microspheres on average. The process seemed to be promising for tuning up of the metal thickness by stepwise electroless plating. (C) 2013 Elsevier B.V. All rights reserved.