Spatial and cure-time distribution of dynamic-mechanical properties of a dimethacrylate nano-composite

Objective: The purpose of this study was to evaluate a nano-filled dental composite, with varying cure irradiation-time, in terms of the spatial distribution of dynamic-mechanical properties determined at nanometre scale and the resultant distinction between filler, matrix and inter-phase regions. Materials and methods: Specimen groups (n = 5) of the composite Filtek Supreme XT were cured in 2 mm deep molds for 5, 10, 20 and 40 s, and stored for 24 h in distilled water at 37 °C. Properties were measured at 2 mm depth, on the lower specimen surfaces. Nano-dynamic-mechanical parameters (complex, storage and loss modulus, tan δ) were determined at an array of 65,000 locations in a 5 μm × 5 μm area. Micro-mechanical properties (hardness, modulus of elasticity, creep and elastic/plastic deformation) were also measured and additionally the real-time degree of cure, by ATR-FTIR, for 10 min after photo-initiation and after storage. Results: The spatial distribution of nano-dynamic-mechanical properties varied significantly enabling four distinguishable matrix, filler-cluster and inter-phase regions to be identified. Proceeding from matrix to filler-cluster locations, complex-moduli increased linearly and loss-factors decreased linearly, consistent with visco-elastic composite theory. Curing time strongly affected all measured properties at 2 mm depth. The organic matrix was shown to be inhomogeneous for all curing times. By increasing cure-time, the proportion of less well polymerized area decreased from 37.7 to 1.1%, resulting in a more homogeneous organic matrix. Significance: The experimentally observed graduated transition, in complex modulus and related dynamic-mechanical properties, across the matrix - inter-phases - filler-cluster regions is conducive to low internal stresses, in contrast to the abrupt modulus transitions anticipated or observed in many other particulate composite structures. The identification of these phase-regions provides a realistic basis for accurate nano- and micro-mechanical computational modelling. © 2008 Academy of Dental Materials.