Nanocomposites of poly(ethylene oxide) and molybdenum disulfide are prepared by the hydrolysis of lithiated molybdenum disulfide in an aqueous solution of PEO (mw 100 000) or poly[oxymethylene-oligo(oxyethylene)] (PEM, mw almost-equal-to 70 000). X-ray diffraction indicates an expansion of 8.3 angstrom in the interlayer spacing (c almost-equal-to 14.5 angstrom), consistent with the incorporation of a polymer double layer within the disulfide galleries. Reaction stoichiometries and elemental analyses indicate a composition of Li0.12(PEO)yMoS2 (y = 1.0-1.3) for the single-phase product. Analyses of extracted polymer demonstrate that high-molecular-weight polymer is present within the disulfide galleries. Scanning calorimetry of the nanocomposites indicates exothermic peaks at approximately 200 and 310-degrees-C, which are demonstrated to be associated with an order/disorder phase transition and polymer decomposition, respectively. A fully amorphous, unstacked phase is irreversibly generated by heating the nanocomposites at 200-degrees-C for several hours.