A novel technique has been devised for the synthesis of microporous α-Cr 2 O 3 (eskolaite). The technique was based on the formation of amorphous-Cr 2 O 3 onto microporous activated carbon through adsorption–reduction of dichromate ions (Cr2O72-) at the activated carbon/aqueous solution interface. Then, the Cr 2 O 3 -loaded carbon was thermally processed under oxidizing conditions to remove the carbon and recover the chromium oxide as α-Cr 2 O 3 . Both the Cr 2 O 3 -loaded carbon and the synthetic product were characterized by XRD, SEM, surface area and pore volume measurements. The synthetic eskolaite assayed 97.3% Cr 2 O 3 and its specific surface area was 15.48m 2 /g and pore size of 16.1Å.