This review describes our recent works on the preparation of Ni-alloy films deposited by electroless deposition as a diffusion barrier layer for ultra large-scale integration (ULSI) interconnects by using an all-wet process. In this process, we create a novel wet fabrication process including a self-assembled monolayer (SAM) as an attachment technique between diffusion barrier layer and a substrate. Our proposal process was applied to the substrates Of SiO2/Si and both organic (methyl silsesquioxane) and inorganic (hydrogen silsesquioxane) low-k dielectrics. The key technique of this proposed process is using SAM as a catalyst trapping layer. The Ni-alloy films such as NiB were deposited on catalyzed SiO2 or low-k substrates. The electrolessly deposited NiB films were found to exhibit sufficient thermal stability and an acceptable barrier property for preventing Cu diffusion into the SiO2 and low-k dielectrics. (c) 2007 Elsevier Ltd. All rights reserved.