A hetero-bifunctional gelator composed of two different polymerizable groups, acryl and diacetylene, and used to gelate an acrylic monomer has been prepared. The photopolymerization of the organogel formed in hexyl methacrylate produces a free-standing film, in which fluorescent polydiacetylene nanofibers are embedded in a poly(hexyl methacrylate) matrix (see figure).