A novel, simple method was developed to prepare conjugated polymer array in a large scale by using a spinodal dewetting technique. Mica, silicon, and glass were selected as substrates. The results show that with a suitable concentration of poly(9,9-dihexylfluorene) (PF) in volatile organic solvent the polymer forms different sizes of array on the substrates. Atomic force microscopy measured the three-dimensional structure of the arrays, and the relative FFT and PSD analyses reveal the detail information of the dewetting process and the array formation mechanism. The size of spots in the arrays is controlled by the evaporation speed of solvent and concentration of the PF solutions. The photoluminescence of PF arrays were also measured. (c) 2005 Wiley Periodicals, Inc.