Composite membranes of niobium(V) oxide and cellulose acetate (Cel/Nb2O5) were prepared with the following Nb2O5 loadings (in wt%) : 1.1, 6.1, 9.8, 15.6, and 20.9. The thermal stability of the membranes slightly decreased in relation to the pure membrane on incorporation of the metal oxide into the matrix. Scanning electron microscopy and niobium mapping with an X-ray EDS microprobe showed that the metal oxide particles are homogeneously dispersed in the matrix. The electronic absorption bands indicated that the oxide particle size varies from that of the monomer to those of oligomer species on increased Nb2O5 loading in the matrix. The dispersed oxide possesses mainly Lewis acid character, a clear indication that on increasing the oxide loading in the matrix, the coordination number of the metal is not saturated by formation of the Nb-O-Nb bond.