In this study, the effects of the sulfur-selenium substitution inside sprayed ZnS compounds are discussed. First, the spray pyrolysis method has been used to grow the ZnS layers on glass substrates at relatively low temperatures. After an appropriate cooling phase, the substrate-layer set was introduced inside a sealed tube. Consecutively, selenium supply was introduced and vaporized under vacuum conditions inside the sealed tube containing the formerly ZnS prepared layers. The annealing time was varied from I to 48 h. Precisely, the tube arrangement was heated to about 350 degrees C in order to vaporize the selenium. On heating supply withdrawal, the selenium reacts with the existing layer. To prevent revaporization and minimize undesirable zinc oxides formation during crystal growth, a small amount of nitrogen was introduced into the tube. AFM technique and Vickers microhardness protocol subjected to the Boubaker polynomials expansion Scheme (BPES), have been carried out in order to evaluate the obtained ZnS1-xSex|(0 <= X<0.5) layers. performance and properties. (C) 2009 Elsevier B.V. All rights reserved.