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Honeycomb patterned hybrid films were prepared from sulfonated polystyrene (SPS) and tetrabutyl titanate (TBT) by a combination of the “breath figure” technique with a gelation process. The influences of solvents, concentration and the mass ratio of SPS/TBT in the hybrid sols on the morphology of the honeycomb films were investigated. The results from SEM, FTIR, DSC, TG and XRD showed that well-ordered films were formed when benzene was used as solvent, the mass ratios of SPS/TBT in the range of 10/1∼1/2 and the concentration of SPS maintained in the range of 20-80 mg/mL.