Nanosized zinc oxide (ZnO) particles were prepared in an amphiphilic N,N-dimethylacrylamide (DMAA) gel composed of a three-dimensional network with an effective pore size of the order of nanometers. The procedures consist of two major steps: (1) preparation of a precursor and (2) hydrolysis of the precursor to form nanoparticles. First, the plate-type dry gel was swollen in ethanol containing zinc acetate (ZnAc) in order to diffuse ZnAc molecules into the gel. Then, the ethanolic solution containing the gel was heated to ∼80°C to prepare the precursor. In the hydrolysis of the precursor, lithium hydroxide was added as the catalyst to the precursor solution containing the gel, and the solution was placed in an ultrasonic bath. Although the DMAA gel containing ZnO particles was completely transparent, it exhibited a yellow-green luminescence when irradiated with UV light. The ZnO nanoparticles stably dispersed in the gel network without growing, aggregating, or flowing out for over several months at a relatively high temperature of 50°C. The particle size depended on the effective pore size of the gel network, which could be controlled by the synthesis composition of the gel, that is, by the concentrations of DMAA as the primary monomer and N,N′-methylenebisacrylamide (MBAA) as the cross-linker used for synthesizing the gel. This implies that the particle size can be controlled at the nanosized level by the synthesis composition of the gel.