Polyaniline/carboxylated multi-walled carbon nanotube (PAni/c-MWNT) nanocomposites have been synthesized by micellar aided emulsion polymerization with various c-MWNTs compositions, viz., 0.5, 1, 5, and 10 wt %. The microcrystalline parameters such as the nanocrystal size (< N >), lattice strain (g), interplanar distance (d(hkl)), width of the crystallite size distribution, surface weighted crystal size (D,), and volume of the ordered regions were calculated from the X-ray data by using two mathematical models, namely the Exponential distribution and Reinhold distribution methods. The effects of heat ageing on the microcrystalline parameters of the PAni/c-MWNT nanocomposites were also studied and the results are correlated. The thermal stability and electrical resistivity of the PAni/c-MWNT nanocomposites were examined with thermogravimetric analysis (TGA) and a conventional two-probe method. The TGA data indicate that the thermal stability of the nanocomposites improved after the incorporation of c-MWNTs. The influence of temperature on the resistivity of the nanocomposites was also measured. (C) 2008 Wiley Periodicals, Inc.