The aim of this study was to prepare and characterize a hybrid layered material (organoclay) with a Na-montmorillonite and the triethylene glycol mono-n-decyl ether (C10E3) nonionic surfactant which forms a lamellar phase at room temperature. The synthesized organoclay was characterized by complementary techniques (Fourier transform infrared spectroscopy and X-ray diffraction). Experiments in conjunction with electron density analysis showed that a bilayer or membrane of C10E3 was intercalated within the interlayer space of a naturally exchanged Na-montmorillonite. The intercalation of a bilayer of C10E3 in a clay mineral offers new perspectives for the manufacturing of nanomaterials. While showing a hydrophobic surface and a large interlayer space value, the resulting organoclay preserves the compensating cations within the interlayer space allowing one to perform ion exchanges, making easier the intercalation of further organic molecules of important size with functional properties or for environmental purposes.