We have investigated the microstructure and electrical properties of HfTaON high-k films deposited on n-type Si (100) substrate using a dual ion beam sputtering deposition technique (DIBSD). It is worth noting that HfO2 begin to precipitate from four-compound HfTaON and crystallize as a monoclinic phase after annealing at 1100 degrees C. From FTIR spectra, one strong absorption peak at 512 cm(-1), which is characteristic of the HfO2 monoclinic structure is also observed. The interfacial SiOx can be formed during the annealing procedure rather than sputtering process, and the increase of atomic percentage of Si-O bands and transition from SiOx (x < 2) to SiO2 are observed with the increase of annealing temperature. High efficiency HfTaON film prepared by novel DIBSD has a higher dielectric constant of 24 and lower leakage current of 2.28 x 10(-8) A at V-g = (V-fb - 1), as compared with that of SiO2 center dot center dot HfSiON center dot center dot HfTaO films with same thickness. (C) 2011 Elsevier B.V. All rights reserved.