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The preparation of microcellular foam in cylindrical gold targets is described. The goal cylinders were fabricated by electroplating gold onto a silicon bronze mandrel and leaching the mandrel with concentrated nitric acid. After several rinsing and cleaning steps, the cylinders were filled with a solution containing trimethylolpropanetriacrylate (TMPTA). Low density, microcellular polymeric foam was prepared by in situ photopolymerization of the TMPTA solution. Foam preparation was extremely sensitive to metal ion contaminants. In particular, copper ions left behind from the leaching process inhibit polymerization and must be removed in order to obtain uniform, non-shrinking foams. A study on the effects of potential contaminants and polymerization inhibitors on TMPTA photopolymerization is presented. In addition, a procedure for the effective leaching and cleaning of gold cylinders is described.