This work reports on the synthesis and characterization of nanostructured composites based on proton‐exchanged montmorillonite (MMT‐H ⁺ ) and conducting polymers, namely, polyaniline (PANI), polypyrrole (PPy), and poly(aniline‐co‐pyrrole) (P(ANI‐co‐Py)), prepared via in situ oxidative polymerization using ammonium persulfate (APS) as the oxidant. Structural investigations by X‐ray diffraction (XRD), X‐ray fluorescence (XRF) spectrometry, Fourier‐transform infrared (FT‐IR) spectroscopy, and scanning electron microscopy (SEM) confirmed the successful intercalation of the polymers within the MMT‐H ⁺ interlayers. The copolymer P(ANI‐co‐Py) exhibited an intermediate basal spacing ( d (001) = 24.86 Å), larger than that of PANI (22.87 Å) and PPy (22.46 Å). SEM analysis revealed pronounced morphological differences: PANI generated porous and granular structures, PPy formed dense globular aggregates, whereas the copolymer displayed heterogeneous porosity, leading to increased surface area and enhanced interfacial interactions. Optoelectronic and electrochemical analyses (UV–Vis and cyclic voltammetry [CV]) highlighted clear synergistic effects in the P(ANI‐co‐Py)/MMT‐H ⁺ nanocomposite. The electrochemical tunability originates from the combined redox activity of aniline (ANI) and pyrrole (Py) units, resulting in merged and broadened redox responses intermediate between those of the corresponding homopolymers, while UV–Vis spectra exhibit broadened absorption bands indicative of extended conjugation. Thermal characterization using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) demonstrated superior thermal stability of the copolymer nanocomposite, marked by an extended degradation range (200–600°C), a 40% increase in residual mass at 800°C, and a delayed degradation onset compared to the homopolymer systems. These improvements were attributed to nanoconfinement and cross‐linking effects. These results identify P(ANI‐co‐Py)/MMT‐H ⁺ as a thermally stable and electrochemically tunable nanocomposite with optimized morphology, suitable for high‐temperature electronic applications and advanced functional coatings.

The development of efficient and low-cost adsorbents for dye-contaminated wastewater remains an important challenge in environmental remediation. In this study, an interlayer-expanded polypyrrole/maghnite–Cu²⁺ nanocomposite (PPy/Mag–Cu²⁺) was successfully synthesized through purification of raw maghnite, sodium activation, Cu²⁺ ion exchange, and in situ oxidative polymerization of pyrrole. The obtained hybrid was characterized by X-ray fluorescence, X-ray diffraction, Fourier-transform infrared spectroscopy, UV–Vis spectroscopy, scanning electron microscopy, and cyclic voltammetry. The results confirmed the successful incorporation of Cu²⁺ and polypyrrole while preserving the layered aluminosilicate framework. XRD analysis revealed a progressive increase in basal spacing from 17.49 Å for raw maghnite to 25.95 Å for the final nanocomposite, indicating effective intercalation and formation of an expanded hybrid structure. The adsorption performance of PPy/Mag–Cu²⁺ was evaluated for methylene blue removal under batch conditions. Adsorption was strongly influenced by contact time, pH, and initial dye concentration, with equilibrium reached after approximately 80 min and optimum removal at pH 9. Equilibrium data were best fitted by the Langmuir model, with a maximum monolayer adsorption capacity of 43.66 mg g⁻¹, while kinetic data followed the pseudo-second-order model. These findings demonstrate that PPy/Mag–Cu²⁺ is a promising and cost-effective hybrid adsorbent for cationic dye removal from aqueous media.

This work reports the synthesis and comprehensive characterization of HCl-doped poly(3-bromoaniline)/MoO₃, polypyrrole/MoO₃, and poly(3-bromoaniline-co-pyrrole)/MoO₃ nanocomposites prepared via chemical oxidative in situ polymerization to enhance thermal stability and morphological properties. Structural investigations by FTIR and UV–Vis spectroscopy confirmed successful doping and chemical interactions between the polymers and MoO₃. X-ray diffraction (XRD) analysis verified the preservation of the orthorhombic α-MoO₃ crystalline phase across all composites, with peak broadening indicative of polymer-induced lattice strain and reduced crystallite size due to acid treatment and polymer embedding. Morphological examination using scanning electron microscopy (SEM) revealed exfoliated MoO₃ nanobelts uniformly dispersed within hierarchically porous polymer matrices, promoting increased surface area and ion accessibility. Thermal analyses via thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) demonstrated enhanced thermal stability and distinct degradation behaviors relative to pristine polymers, attributed to robust polymer–inorganic interfacial interactions that enhance composite stability. These findings suggest that the hybrid nanocomposites, combining enhanced thermal robustness and tunable morphology, are promising for energy storage devices, electrochemical sensors, and thermally stable conductive coatings.