This paper demonstrated a novel technique for catalytic etching of synthetic diamond crystallites using iron (Fe) powder without flowing gas. The effect of temperature on the etching behaviour on different crystal planes of diamond was investigated. The surface morphology and surface roughness of the processed diamond were examined by scanning electron microscope (SEM) and laser-probe surface profiling. In addition, the material composition of the Fe-treated diamond was characterized using micro-aman spectroscopy and the distribution of chemical elements and structural changes on Fe-loaded diamond surfaces were analyzed by energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD), respectively. Results showed that at the same temperature the {1 0 0} plane was etched faster than the {1 1 1} plane, and that the etching rate of both {1 0 0} and {1 1 1} plane increased with temperature. The etch pits on {1 0 0} plane were reversed pyramid with flat {1 1 1} walls, while the etch holes on {1 1 1} plane were characterized with flat bottom. It was also demonstrated that graphitization of diamond and subsequent carbon diffusion in molten iron were two main factors resulting in the removal of carbon from the diamond surface. (C) 2015 Elsevier B.V. All rights reserved.