A process has been developed to produce regular arrays of hollow metal microstructures on substrates of choice. Optical lithography was used to define high aspect ratio structures in photoresist. The resist structures were selectively metallized by electroless (EL) deposition such that metal was deposited only on the sidewalls of the resist and on the surface of the substrate. Dissolution of the polymeric photoresist resulted in regular arrays of hollow metal cylinders and cones with geometries and structure spacings determined by the original resist structures. Characterization of metallized microstructures using surface analytical techniques and SEM is presented. Arrays of microstructures with 500–1000 Å thick EL Ni walls and aspect ratios (height/tip diameter) of 8:1 are shown.