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The influence of the addition of ethylene glycol (EG) on the pore self-ordering process in anodic aluminium oxide (AAO) membranes prepared by hard anodization (HA) was investigated. It was illustrated that EG has a substantial effect on the pore arrangement of AAO, and it was found that a smaller pore size can be obtained with an EG concentration reaching 20 wt% in aqueous electrolyte. The number of estimated defects of AAO increases significantly with an increase in EG concentration to 50 wt%. Excellent ordering of pores was realized when the samples were anodized in the 30 wt%-EG-containing aqueous electrolyte.