Determination of polymerization shrinkage kinetics in visible-light-cured materials: methods development.

An instrument for the reproducible measurement of polymerization shrinkage kinetics is described, constructed around a disc-shaped specimen sandwiched between two glass plates. Test specimens of light-sensitive dental restorative materials were irradiated through the lower, rigid plate. The upper, non-rigid plate was readily deflected by an increase of the adhesive stress from the polymerizing and shrinking sample. Deflection was measured by an LVDT transducer and computer-recorded. Dimensional changes were confined to the specimen disc-thickness dimension, such that the fractional linear shrinkage approximated the volumetric shrinkage. Shrinkage data are reported for representative materials: unfilled and resin composites, base-lining materials, and an impression material. Equilibrium shrinkage magnitudes ranged from 0.65%, for the impression material, to 7.9% for the unfilled resin. The kinetic behavior was approximately characterized by an overall time constant, ranging from 12.5 to 280 s, associated with an exponential growth curve, although the initial shrinkage was near-linear in time, for many materials, due to non-steady-state concentrations of polymer free-radicals. The test-specimen geometry facilitates rapid and essentially uniform cure and hence the determination of minimum possible time-constants at each ambient temperature and incident light-intensity. Study of hybrid glass-ionomer materials, without spurious dehydration effects, was also achieved.