Pd-Si-structured novel mesoporous nanocomposite catalytic materials, having quite high Pd/Si ratios, were synthesized by an acidic direct hydrothermal synthesis route. The nanocomposite catalytic materials were then characterized by XRD, XPS, EDS, nitrogen adsorption, and SEM techniques. Unlike MCM-41, the XRD patterns indicated a rather wide d((100)) band at a 2 theta value of about 1.9. The materials, with very high Pd/Si wt ratios between 1.43 and 2.66, were synthesized and had BJH surface area values between 600 and 200 m(2)/g. The pore size distributions of these materials were also quite narrow, indicating pores between 2 and 7 nm.