A new nanocomposite was synthesized by reacting the layered double hydroxide Al0.33Mg0.67(OH)(2)(C12H25SO4)(0.33).0.64H(2)O with poly(ethylene oxide). The composite was characterized with X-ray powder diffraction, thermal analysis (simultaneous thermogravimetric analysis/differential scanning calorimetry), Fourier transform infrared spectroscopy, photoelectron spectroscopy, and electron diffraction. The. nanocomposite has the layered structure of the double hydroxide simultaneously intercalated with dodecyl sulfate anions and poly(ethylene oxide) molecules. The characterization indicates a nanocomposite with a well-ordered structure.