Abstract The growth behavior of anodic porous alumina formed via anodizing in a new electrolyte, squaric acid (3,4-dihydroxy-3-cyclobutene-1,2-dione), is reported for the first time. A high-purity aluminum foil was anodized in a 0.1 M squaric acid solution at 293 K and a constant applied potential of 100-150 V. Anodic oxides grew on the aluminum foil at applied potentials of 100-120 V, but a burned oxide film was formed at higher voltage. Anodic porous alumina with a cell size of approximately 200–400 nm and sub-100-nm-scale pore diameter was successfully fabricated by anodizing in squaric acid. The cell size of the anodic oxide increased with anodizing time because of the uneven growth of the porous layer. The anodic porous alumina obtained by squaric acid anodizing consists of amorphous Al 2 O 3 containing 5-6 at% carbon from the electrolyte.