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Aluminum sol, dry gel, and film were prepared by sol-gel and a dipping-withdrawing method. The effect of polyethylene glycol (PEG) on the behavior of aluminum sol, gel, and film was investigated by DLS, rotary viscometer, XRD, IR, EPMA, and light microscope, respectively. The solid gels drying at room temperature was identified as amorphous phase, and the addition of PEG nearly has no effect on the structure of aluminum dry gel. It is indicated that the sol viscosity decreases with the PEG content increasing, while the micelle size in sol decreases first then increases. The uniformity and attached particles of the film are improved to a certain extent after PEG addition. According to the analytic results, we demonstrate that the improvement is caused by low viscosity and small micelle size of sol resulting from the PEG addition.