Freestanding crystalline diamond/graphite nanoflake hybrid films have been deposited in H(2)/CH(4) gas mixtures using a high pressure (1 3 x 10(4) Pa) direct current plasma discharge Sacrificial layers of close-packed silica microspheres were used as a matrix to produce dual gas chemistries on the plasma-facing and reverse sides of the microspheres A continuous polycrystalline diamond film was formed on the front surface whilst graphite was deposited in the form of nanoflakes as a thinner hemispherical layer on the reverse side of the silica spheres respectively Chemical etching of the silica matrix yielded crystalline diamond/well-aligned graphite nanoflakes hybrid films (C) 2010 Elsevier B V All rights reserved