W.M. Palin

Investigating filler morphology and mechanical properties of new low-shrinkage resin composite types

Three types of low-shrinkage composites are today commercially available: Ormocers, cationic ring-opening curing systems and highly filled methacrylate-based materials, which cure via free-radical polymerization mechanisms. The aim of this study was to characterize the inorganic fraction of materials belonging to each type and to compare their mechanical properties. Two Ormocers (Admira and an experimental Ormocer V35694), one ring-opening composite (Filtek Silorane) and five methacrylate-based composites [Filtek Supreme XT, Tetric EvoCeram, Grandio, Synergy D6 (Coltène-Whaledent, Langenau, Germany) and an experimental material, V34930] were tested. Inorganic fillers were quantified by thermogravimetric analysis and morphologically characterized by scanning electron microscopy. Dynamic modulus was determined by an impulse excitation technique, static elastic moduli and flexural strength by a three-point bending method. The results were analyzed using ANOVA tests (P < 0.05) and linear correlations. Grandio, V34930 and V35694 exhibited significantly higher filler mass fractions. Both dynamic and static moduli of Grandio and V34930 were significantly higher than the other materials (P < 0.05), although no significant difference in flexural strength was observed between material type (P > 0.05). From the present findings, it was suggested that V35694 and Filtek Silorane exhibit comparable properties to conventional methacrylate-based composites, although clinically the cavity type and location must guide material choice. Under high occlusal load, the use of Grandio and V34930 might be favoured. For small cavities, alternative technologies could be preferred as the need for mechanical resistance is lower and the potential for stress generation is greater.

Dynamic monitoring of refractive index change through photoactive resins

OBJECTIVES The change in optical characteristics through the bulk of curing photopolymers is not fully understood. Photopolymerization processes are accompanied by photoinitiator absorption, density changes and volumetric shrinkage, which alter optical properties and affects curing efficiency through depth. METHODS This investigation demonstrates the use of a novel low coherence interferometry technique for simultaneous measurement of optical (refractive index) and physical (shrinkage) properties throughout curing of photoactive monomers containing various concentrations of bisphenol-A-diglycidyl ether dimethacrylate and triethylene glycol dimethacrylate. RESULTS Reliability of the interferometry technique was compared with an Abbé refractometer and showed a significant linear regression relationship (p<0.001; adjusted R(2)>0.99) for both uncured and cured resins. The extent and rate of refractive index change and magnitude of shrinkage strain was dependent upon monomer formulation. SIGNIFICANCE The development of this interferometry technique provides a powerful non-invasive tool that will be useful for improving light transmission through photoactive resins and filled resin composites by precise control of optical properties through material bulk.

Time-resolved simultaneous measurement of group index and physical thickness during photopolymerization of resin-based dental composite

Light-activated resin-based dental composites are increasingly replacing dental amalgam. However, these materials are limited by inefficient setting reactions as a function of depth that constrain the maximum extent of cure. Insufficient curing can contribute to an overall reduction in biocompatibility of the material. We demonstrate dynamic refractive index measurements of a commercial dental composite throughout cure using spectral domain low coherence interferometry. Our results show a linear relationship between the change in refractive index and polymerization-induced reduction in physical thickness during light-activated curing. This relationship between the optical and physical density demonstrates the potential of this technique as a unique noninvasive tool for measurement of the conversion degree of curing dental composite materials.

Dynamic monitoring of curing photoactive resins: A methods comparison

OBJECTIVE The aim of this investigation was to determine reaction enthalpy, ion viscosity and curing light transmission changes of unfilled methacrylate-based systems in order to compare methods that monitor photoactive resin polymerization. METHODS Photoinitiator (0.2%, w/v, camphoroquinone), accelerator (0.3%, w/v, amine) and inhibitor (ranging from 0 to 1%, w/v, butylated hydroxytoluene, BHT) were incorporated in an experimental BisGMA/TEGDMA co-monomer mixture (50/50, w/v). The concentration of BHT was varied from 0.00, 0.01, 0.05, 0.10, 0.50 to 1.00% (w/v). Light transmission (LT), reaction enthalpy (UV-differential scanning calorimetry, DSC), and ion viscosity (dielectrical analysis, DEA) were determined during irradiation of the resins (40s; halogen light curing-unit). Statistical analysis was performed using two-way ANOVA followed by post hoc tests (alpha=0.05). Curve fitting and regression calculation were done. RESULTS There was no significant change in the time to reach the maximum rate of polymerization (reaction time) in the individual systems up to a BHT concentration of 0.05% (P>0.05). Starting at a concentration of 0.10% BHT an increase in time of reaction could be found from 4.0s (LT), 4.07s (DEA) and 4.9s (DSC) to a maximum of 7.4s (DSC), 9.43s (DEA) and 9.67s (LT). Linear increase (y=5.588 x x) in time to the maximum speed of reaction could be found with a correlation of R(2)=0.992. CONCLUSIONS The speed of polymerization reaction is strongly influenced by BHT concentration. The linear relationship should allow for the prediction of the speed of reaction during blending of a methacrylate-based resin. The three test systems allow for monitoring the complex polymerization kinetics of unfilled methacrylate-based systems.

Dynamic Cure Measurement of Dental Polymer Composites Using Optical Coherence Tomography

Dental amalgam is being increasingly replaced by Light-activated resin-based dental composites. However, these materials are limited by inefficient setting reactions as a function of depth, constraining the maximum extent of cure and reducing biocompatibility. In this paper we demonstrate a novel metrological tool for dynamic monitoring of refractive index and thickness change through curing resins using spectral-domain optical coherence tomography. We present real-time measurements from pre- to post-cure of a series of un-filled bisphenol-A diglycidyl ether dimethacrylate (bisGMA) and triethylene glycol dimethacrylate (TEGDMA) resins with different inhibitor concentrations. Our results demonstrate that refractive index measurements are sensitive to the extent of cure of such resins and that the inhibitor concentration strongly affects the cure dynamics and final extent of cure.

Investigating the limits of resin-based luting composite photopolymerization through various thicknesses of indirect restorative materials

OBJECTIVE To determine the limitations of using light-curable resin-based luting composites (RBLCs) to bond indirect ceramic/resin-composite restorations by measuring light transmittance through indirect restorative materials and the resulting degree of conversion (DC) of the luting-composites placed underneath. METHODS Various thicknesses (0-4mm) and shades of LAVA Zirconia and LAVA Ultimate were prepared and used as light curing filters. A commercial, light curable RBLC, RelyX Veneer (control) was compared with four experimental RBLCs of the following composition: TEGDMA/BisGMA (50/50 or 30/70wt%, respectively); camphorquinone/amine (0.2/0.8wt%) or Lucirin-TPO (0.42wt%); microfillers (55wt%) and nanofillers (10wt%). RBLCs covered with the LAVA filter were light-cured for 40s, either with the dual-peak BluephaseG2 or an experimental device emitting either in the blue or violet visible band. The samples were analyzed by Raman spectroscopy to determine DC. Light transmittance through the filters was measured using a common spectroscopy technique. RESULTS All the factors studied significantly influenced DC (p<0.05). RBLCs with increased TEGDMA content exhibited higher DC. Only small differences were observed comparing DC without filters and filters ≤1mm (p>0.05). For thicknesses ≥2mm, significant reductions in DC were observed (p<0.05). Transmittance values revealed higher filter absorption at 400nm than 470nm. A minimal threshold of irradiance measured through the filters that maintained optimal DC following 40s irradiation was identified for each RBLC formulation, and ranged between 250-500mW/cm2. SIGNIFICANCE This work confirmed that optimal photopolymerization of RBLCs through indirect restorative materials (≤4mm) and irradiation time of 40s is possible, but only in some specific conditions. The determination of such conditions is likely to be key to clinical success, and all the factors need to be optimized accordingly.