Composite resin reinforced with fluorescent europium-doped hydroxyapatite nanowires for in-situ characterization.

Objective: The object is to find an easy but efficient way to illustrate the in-situ dispersion of nano-scaled one-dimensional fillers in composite resins, and to correlate their dispersion status with the properties of composite resins.

Methods: Fluorescent europium-doped hydroxyapatite nanowires (HANW:Eu) were synthesized via the hydrothermal method. The HANW:Eu was mixed into Bis-GMA/TEGDMA (60/40, w/w) at different contents (1-5wt.%), and different processing methods (kneading, grinding, stirring) were tested to achieve good dispersion of HANW:Eu with the aid of fluorescent imaging system. Then, the mixtures of HANW:Eu and barium glass powder (BaGP) were kneaded into resin at a fixed content (70wt.%) while at different mixing ratios. In addition to the 3D fluorescent imaging, characterizations were carried out on mechanical properties, fractured surface, wear resistance and polymerization shrinkage, to correlate the composite properties of with the dispersion status of the incorporated HANW:Eu.

Results: By doping calcium with 5mol.% of europium, the obtained HANW:Eu displayed strong fluorescence, which made the illustration of its in-situ dispersion status within composites being possible. And this helped to judge that kneading was more efficient to homogeneously disperse HANW:Eu than grinding and stirring. However, it was illustrated vividly that HANW:Eu aggregated severely when it was co-incorporated with BaGP into composites at the total content of 70wt.%, which had not been previously revealed by other microscope observations. In comparison with composites containing 70wt.% of BaGP, improvements in the mechanical properties of resulting composites were identified for the cases containing 3wt.% of HANW and 67wt.% of BaGP, however, their wear volume loss and the polymerization shrinkage did not decrease as expected due to the HANW aggregations.

Significance: The fluorescent filler prepared in this study provides a feasible strategy to illustrate the in-situ dispersion status of inorganic fillers, which provides guidance for the processing of composite resins.