In this paper we report the development of self-standing tubular geometry of aligned carbon nanotubes with very high surface area (∼90 m²/g). The synthesis involves spray pyrolysis of ferrocene-benzene solution in nitrogen atmosphere. The effects of temperature, ferrocene concentration, flow rate of nitrogen gas and the pumping rate of the liquid precursor were studied. The products were analyzed with transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Raman spectroscopy. The optimum condition for formation of macro-tubular geometry was found to be 950 °C, 50 mg/ml ferrocene in benzene, 1.5 ml/min pumping rate of liquid precursor and 5 lpm of nitrogen gas flow rate. The length and the diameter of the macrotube were 5 cm and 1 cm respectively with a thickness of 120 μm. The authors intend to use this tube in separation technology.