A method to obtain three-dimensional sub-micrometric periodic structures is presented. The experimental set-up consists in a pulsed UV laser beam source (lambda = 355 nm) coming into an interferometer in order to generate four beams converging inside a chamber. According to the directions, to the relative intensities and to the polarizations of these four beams, a 3D interference pattern can be obtained inside the overlapping volume of these four beams; the characteristics of the four laser beams have been optimized in order to obtain a maximal contrast of intensity. In order to visualize the interference pattern, its contrast and its stability at each laser pulse, a video camera coupled to an oil immersion microscope objective has been installed above the interferometer. By suppressing the central beam, it is also possible to generate a bidimensional interference pattern which defines an hexagonal structure in the (1 1 1) plane with a period of 377 nm. This optical set-up has been used to obtain 3D sub-micrometric periodic structures in negative photoresists. Experiments consist in a one- or multi-pulse irradiation of the photoresist followed by a development procedure which leads to a sub-micrometric face-centred cubic structure cut in a(1 1 1)plane with a cell parameter of 650 nm. The optimization of the experimental conditions is presented for two kinds of photoresists; the role of the substrate according to its reflectivity at the laser wavelength and its influence on the interference pattern is also discussed. (c) 2007 Elsevier B. V. All rights reserved.