A simple catalytic synthesis of polycarbosilane (PCS) from polydimethylsilane (PDMS) was developed by using anodized aluminum oxide (AAO). Three types of AAO catalysts were used: spiral, stirrer, and cylinder. The AAO catalysts can be reused and do not need a filtering process, which can simplify the complex synthetic processes of PCS and save time and cost. The catalytic property of AAO comes from the high specific surface area of its nanopores and its many Lewis acid sites. By including the total synthetic process of spinable PCS, electrospun PCs was also produced. (C) 2008 Elsevier B.V. All rights reserved.