The work reported in this paper relates to preparation and characterization of carbon nanomaterials by CVD method on different substrates by decomposition of certain hydrocarbons at 550-800℃ using a horizontal quartz tube reactor. Monometallic and bimetallic catalyst system of iron and nickel were used for the preparation of different carbon nanomaterials. The influence of various parameters such as substrate/catalyst preparation parameters, the nature of substrate, catalyst concentration, reaction time and temperature on the growth, yield and alignment of carbon nanotubes has been studied. The characterization of carbon nanomaterials has been carried out using SEM, TEM and TGA. The carbon nanomaterials developed were vertically aligned on a large area of flat quartz substrate.