As a nano-material possessing moderate conductivity, magnetic and dielectric property, novel hexanoic acid doped polyaniline (PAni/HA) micro/nanocomposites containing TiO 2 and Fe 3 O 4 were prepared by template free method under various polymerization conditions. FT/IR spectra of PAni/HA/TiO C. PAni/HA polymerized at low temperature exhibited higher conductivity (1:0 Â 10 À3 S/cm) compared with PAni/HA polymerized at higher temperature (7:0 Â 10 À4 S/cm). The conductivities of the PAni/HA/TiO 2 and PAni/HA/TiO 2 /Fe 3 O 4 were relatively low (3:3{4:2 Â 10 À4 S/cm) after addition of TiO 2 and Fe 3 O 4 . PAni/HA/TiO 2 /Fe 3 O 4 micro/nanocomposites synthesized at 0 C exhibited higher magnetization (Ms = 7.7 emu/g) compare with micro/nanocomposites that synthesized at 25 C (Ms = 4.7 emu/g). TGA characterizations of the micro/nanocomposites were also being discussed in this paper.