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Summary: Conducting polyaniline (PANI) and montmorillonite (MMT) nanocomposites were prepared from aniline sulfate and MMT by a mechanochemical synthesis route. X‐Ray diffraction analysis confirmed that, by controlling the aniline sulfate content, mechanochemical synthesis led to two types of different formations. After polymerization, the mechanochemical route synthesized much more PANI between the clay layers compared to a solution method. The electrical conductivities of the synthesized PANI‐MMT nanocomposites in pressed pellets ranged in the order of between 10−4 and 10−3 S · cm−1.X‐ray powder diffraction patterns of the intercalation products prepared by grinding montmorillonite with various amounts of Ani‐SO4 in a mortar.imageX‐ray powder diffraction patterns of the intercalation products prepared by grinding montmorillonite with various amounts of Ani‐SO4 in a mortar.

Summary: Non‐ionic pyrrole was directly intercalated into unmodified montmorillonite (MMT) and organically modified MMT galleries by adsorption, and subsequently polymerized within the interlamellar spaces by a mechanochemical route under solvent‐free conditions. XRD analysis revealed the successful intercalation of pyrrole into unmodified MMT and organically modified MMT clay galleries by mechanochemical grinding. After in situ polymerization, the XRD and FT‐IR analyses confirmed the insertion of polypyrrole chains between both MMT galleries.X‐ray powder diffraction patterns of (A) pyrrole‐intercalated MMT and (B) pyrrole‐intercalated C18‐MMT.imageX‐ray powder diffraction patterns of (A) pyrrole‐intercalated MMT and (B) pyrrole‐intercalated C18‐MMT.

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Nanocomposites consisting of conducting polyaniline and clay minerals were successfully synthesized from mechanochemically intercalated anilinium fluoride; the nanocomposites prepared by the mechanochemical intercalation method contained much more polyaniline in the clay layers than those prepared by a conventional solution method.