Self‐assembled hollow nanosphere composites of polyaniline and Au nanoparticles (PANI‐p‐TSA/Au) were chemically synthesized from solutions containing p‐toluenesulfonic acid (p‐TSA) with the addition of gold chloride trihydrate as the oxidant. The composite materials were characterized by SEM, TEM, and a range of spectroscopic methods. Spectroscopic characterizations confirmed that the polymeric product is a form of doped PANI, while electron diffraction and X‐ray diffraction showed that elemental Au was present in the PANI‐p‐TSA/Au nanocomposites. The room temperature electrical conductivity of the PANI‐p‐TSA/Au nanocomposites was two orders of magnitude greater than a PANI‐p‐TSA obtained in the presence of ammonium persulfate as the oxidant under the same conditions.
