ABSTRACT:The polycarbynes are polymeric precursors that can be used in the synthesis of both diamond films and powders. They are soluble in common organic solvents; therefore, they can be coated on any surface in various thicknesses and then converted to diamond via sintering. Polycarbynes can be synthesized in a simple undivided electrochemical cell so their synthesis are both cheap and easy. Here, we report the electrochemical synthesis of poly(methylcarbyne). The poly(methylcarbyne) was characterized using UV/visible spectroscopy, Gel Permeation Chromatography and ATR FTIR, 1 H NMR, 13 C NMR spectroscopies. The polymer was converted to diamond via sintering and characterized by Optical microscopy and Raman and X-ray spectroscopies.