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Hydrogen silsesquioxane (HSQ) is a high-resolution negative-tone inorganic resist for electron beam lithography. Investigations on the smoothness of the surfaces of thin films (less than 100 nm thick) have been conducted for nanolithography applications. It is demonstrated that films at thicknesses down to 25 nm have very low rms roughness and are defect free. Using 50 kV electron beam lithography, we demonstrate the achievement of isolated 6-nm-wide lines and 27 nm period gratings in 30 nm HSQ films on silicon substrates. These results are superior to those achieved with poly(methylmethacrylate) resist and demonstrates the versatility of HSQ for nanolithography. © 2003 American Vacuum Society.