We have prepared thin Zr-B films at low temperatures as a new material applicable to an extremely thin barrier against Cu diffusion in Si-ULSI metallization. The obtained Zr-B films mainly consist of the ZrB2 phase with a nanocrystalline texture on SiO2 and a fiber texture on Cu. The resistivity of the Zr-B films depends on the substrate of SiO2 or Cu. The constituent ratio of B/Zr is almost 2, though the contaminants of oxygen, nitrogen, and carbon are incorporated in the film. The nanocrystalline structure of the Zr-B film on SiO2 is stable due to annealing at temperatures up to 500 degrees C for 30 min. We applied the 3-nm thick Zr-B film to a diffusion barrier between Cu and SiO2, and the stable barrier properties were confirmed. We can demonstrate that the thin Zr-B filmis a promising candidate for thin film application to a metallization material in Si-ULSIs. (C) 2009 Elsevier B.V. All rights reserved.