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The sol–gel method was employed to prepare an inorganic–organic hybrid, silica/poly(HEMA). The chemical structure of this material was analyzed by means of FTIR and solid 29Si-NMR. Using TEM and low voltage FESEM imaging at high magnifications (e.g., 300 KX), the hybrid was found to comprise nano-particles whose sizes fall largely over the range 20–30 nm.