Activated carbon spheres (ACS) were prepared at different heating rates by carbonization of the resole-type phenolic beads (PB) at 950oC in N2 atmosphere followed by activation of the resultant char at different temperatures for 5 h in CO2 atmosphere. Influence of heating rate on porosity and temperature on carbon structure and porosity of ACS were investigated. Effect of heating rate and temperature on porosity of ACS was also studied from adsorption isotherms of nitrogen at 77 K using BET method. The results revealed that ACS have exhibited a BET surface area and pore volume greater than 2260 m2/g and 1.63 cm3/g respectively. The structural characteristics variation of ACS with different temperature was studied using Raman spectroscopy. The results exhibited that amount of disorganized carbon affects both the pore structure and adsorption properties of ACS. ACS were also evaluated for structural information using Fourier Transform Infrared (FTIR) Spectroscopy. ACS were evaluated for chemical composition using CHNS analysis. The ACS prepared different temperatures became more carbonaceous material compared to carbonized material. ACS have possessed well-developed pores structure which were verified by Scanning Electron Microscopy (SEM). SEM micrographs also exhibited that ACS have possessed well-developed micro- and meso-pores structure and the pore size of ACS increased with increasing activation temperature.