Appl Phys A (2008) 93: 105–110 DOI 10.1007/s00339-008-4645-5 Synthesis of 3-dimensional periodic nanostructures in an interference field of UV laser light M. Salaün · M. Audier · M. Duneau · F. Delyon Received: 12 October 2007 / Accepted: 4 March 2008 / Published online: 29 May 2008 © Springer-Verlag 2008 Abstract In 2000, Campbell et al. (Nature 404:53, 2000) have shown that three-dimensional periodic nanostructures can be obtained from UV laser interference irradiation of photoresist for 6 nanosecond single pulse. We have devel- oped a similar experiment for photolytic gas phase decom- position and for photopatternable organic–inorganic hybrid resins. Different steps in results, presently reported, were first to determine the characteristics of both the 3D interference pattern and interferometer to be associated to a CVD re- actor and second to verify the mechanical stability of the set up confirmed with the structuration of a siloxane based methacrylic resins by UV polymerization and finally to grow periodic nanostructures by photolytic gas phase decomposi- tion of chromyl chloride. The experimental results obtained so far indicate that, depending on the electromagnetic en- ergy density, a vapor phase decomposition of chromyl chlo- ride leads to periodic arrays of either Cr–O amorphous or Cr 2 O 3 particles on glass and (001)TiO 2 substrates at room temperature. PACS 42.70.Qs · 81.07.St · 81.16.Mk · 81.16.Nd M. Salaün ( ) · M. Audier LMGP, INPG, UMR 5628, 3, Parvis Louis Néel, BP 257, 38016 Grenoble Cedex 1, France e-mail: mathieu.salaun@inpg.fr M. Duneau · F. Delyon CPHT, Ecole Polytechnique, UMR 7644, 91128 Palaiseau Cedex, France 1 Introduction Since Yablonovitch’s pioneering work on photonic crys- tals [1] there has been considerable interest in investigat- ing fabrications of two- and three-dimensional (2D and 3D) periodic arrays on the scale of visible light wavelengths. Currently most of the methods for making such photonic crystal structures are based upon conventional lithography and ionic abrasion techniques [2]. For 3D structures, re- ported new techniques [3] have included interference litho- graphy and electro-deposition [4, 5], two-photon-absorption photo-polymerisation of resins [6], micro-assembly of semi- conductor three-dimensional photonic crystals [7], self- assembly of colloids [8], and holographic lithography [9, 10]. Scaling these techniques to low cost mass produc- tion of 3D photonic crystals made from a large variety of materials remains however a challenge. In this work, the possibility to perform the growth of a sub-micronic periodic structuration by the chemical decom- position of gaseous species was studied using a technique derived by Campbell et al. [9] on the 3D holographic litho- graphy. Let us recall that in this technique a photosensitive film of either photoresist or organic–inorganic hybrid com- pound [11] is exposed to a light interference pattern within the duration of a single laser pulse and then developed in a solvent in order to obtain a photonic crystal. After a pre- sentation on the generation of a 3D interference pattern and on the characterization of its stability, results on the pho- tolysis of chromyl chloride in this 3D interference field are reported. 2 Interference of four beams Let us recall that, in the previous work [12], a 3D network is obtained as follows: a primary polarized UV laser beam