A series of thiol-ene (1.1:1 equiv) polymer microbeads (PMBs) were prepared via a high-shear suspension photopolymerization method to explore the physical properties of the networks as a function of composition. 1,3,5-triallyl-1,3,5-triazine-2,4,6(1H, 3H, 5H)-trione (TTT) and pentaerythritol tetrakis (3-mercaptopropionate) (PETMP) PMBs were selected for the synthesis of a heterogeneous photocatalyst. Particle size was characterized using DLS and OM, and thermal stability and T-g were assessed using TGA and DSC. PMBs produced from higher functionality monomers produce smaller particles, and T-g increased with monomer rigidity. TTT-PETMP PMBs were derivatized with C-60 to demonstrate the accessibility and reactivity of the residual thiols, successful inclusion of C-60 as the reactive ene moiety, and overall PMB utility as a scaffold material. Upon capping with C-60, the T-g of the composite particles increased significantly. Most importantly, the C-60-capped PMBs produced singlet oxygen in direct and indirect chemical assays, and the efficiency did not decrease after recycling. (C) 2016 Elsevier Ltd. All rights reserved.