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It is attractive to prepare and control the structure of noble metal nanoparticle /polymer composites. The room temperature electron reduction via glow discharge as electron source is a simple, easy, cheap and energy efficient way to reduce metal ions. It is excellent for size control with fast nucleation and slow crystal growth. The room temperature operation makes it very useful for the preparation of noble metal and polymer assembly. Gold nanoparticle/PVP sheet like composites can be easily fabricated by this electron reduction by adding poly(vinylpyrrolidone) (PVP) into the solution with HAuCl4. The reduction time can influence the size of Au nanoparticles. Also the size of Au nanoparticles and the structure of assembly can be controlled by mixing other metal ions in aqueous solutions. This study is leading to many applications like SERS and sensor.