ABSTRACT:A novel liquid/solid two-phase reaction has been discovered that enables destruction of a series of low-molecular-weight chloro-/bromo-hydrocarbons to carbonbased materials. The solid phase is anhydrous potassium hydroxide and the liquid phase is a benzene or tetrahydrofuran solution of halide and contains a certain amount of tetrabutyl ammonium bromide (TBAB) as phase transfer catalyst. The structure of the carbon-based materials have been characterized by elemental analysis, Fourier transform infrared (FT-IR), FT-Raman, and X-ray photoelectron spectroscopies, and their morphologies have been examined by wide-angle X-ray diffraction and transmission electron microscopy. The results indicate that the products are amorphous nanoparticles and contain mainly elemental carbon. They consist of sp, sp 2 , and sp 3 carbon atoms simultaneously and can be regarded as carbyne analogues. This work provides a convenient method for synthesizing new carbon-based materials in relatively high yields.