Degree of conversion, depth of cure, and color stability of experimental dental composite formulated with camphorquinone and phenanthrenequinone photoinitiators.

PURPOSE: This study evaluated the applicability of 9,10-phenanthrenequinone (PQ) in experimental dental composites. MATERIALS: Camphorquinone (CQ), PQ, ethyl 4-N,N-dimethylaminobenzoate (EDMAB) and diphenyliodonium salt (DPI) were employed. A mixture of 2,2-bis(4-[2-hydroxy-3-methacryloxypropoxy]phenyl)-propane/triethylene glycol dimethacrylate (60:40%) and silanated glass filler at 60% were used. A two-peak-based light-emitting diode (LED) was used. METHODS: The photoinitiator absorption and the light emission spectra were determined by a Ultraviolet-visible spectroscopy and a spectroradiometer, respectively. Relative photon absorption (RPabs) was calculated. Fourier-transformed infrared spectroscopy analysis was used to determine the degree of conversion (DC). The optical properties were determined with a spectrophotometer. Depth of cure was assessed from adapted International Organization for Standardization (ISO) 4049. Results were analyzed with descriptive analysis, analysis of variance, and Tukey's test (α = 5%). RESULTS: PQ showed higher RPabs than CQ. Regarding the DC, CQ + EDMAB (control), CQ + EDMAB + DPI, PQ + DPI, and PQ + EDMAB + DPI produced statistically similar results. Groups formulated with CQ presented higher depth of cure. Only the group formulated with CQ + EDMAB presented satisfactory color stability (ΔE < 3.3). CONCLUSION: PQ presented higher RPabs than CQ and it was able to produce DC similar to CQ + EDMAB, when used with DPI. However, groups formulated with PQ produced lower depth of cure, greater yellowing, and less color stability than the traditional combination CQ and amine. CLINICAL SIGNIFICANCE: Although research with novel photoinitiator systems should be encouraged, the traditional camphorquinone and amine pair remains as a reliable combination for the formulation of dental composites.

Comparative evaluation of dental resin composites based on micron- and submicron-sized monomodal glass filler particles.

OBJECTIVES: A model resin composite containing a novel monomodal inorganic filler system based on submicron-sized Ba-Si-Al glass particles (NanoFine NF180; Schott) was formulated and compared with an experimental composite containing micron-sized particles (UltraFine UF1.0; Schott). METHODS: The filler particles were characterized using X-ray microanalysis and granulometry, while the composites were characterized in terms of filler-resin morphology, radiopacity, degree of CC conversion, hardness, flexural strength/modulus, work-of-fracture, surface roughness and gloss (before and after simulated toothbrushing abrasion), and bulk compressive creep. The composites were formulated from the same photoactivated dimethacrylate co-monomer, incorporating mass fractions of 75% micron- and 78% submicron-sized particles. Quantitative data were analyzed at a significance level of p<0.05. RESULTS: Both filler systems exhibited a narrow grain size range (175±30 and 1000±200 nm), with differences restricted to the size and specific area of the particles. The composites were similar in radiopacity, flexural strength, work-of-fracture, and creep. The submicron composite was harder but had lower flexural modulus and CC conversion. No significant differences in roughness were observed before brushing, although the submicron composite had higher gloss. Brushing increased roughness and decreased gloss on both materials, but the submicron composite retained higher gloss after brushing. SIGNIFICANCE: The monomodal submicron glass filler system demonstrated potential for use in restorative dental composites, particularly due to improved esthetic properties.

Color stability, conversion, water sorption and solubility of dental composites formulated with different photoinitiator systems.

OBJECTIVES: The aim of this study was to formulate materials with high color stability and reduced degradation by using photoinitiator systems derived from phosphine oxides alternative to the traditional camphorquinone (CQ)/amine system. METHODS: Materials were formulated with the monomers BisGMA and TEGDMA as organic matrix. The photoinitiators tested were CQ+amine (EDMAB), phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide (BAPO), BAPO+EDMAB, diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide (TPO) and TPO+EDMAB. A 60% mass of silanated glass filler particles was added. Degree of CC conversion was evaluated by Fourier-transformed infrared spectroscopy 10min after photopolymerization. The color properties were evaluated by a digital spectrophotometer, applying the CIELab parameters, either before photoactivation, immediately after photoactivation, 24h after dry storage, and one month after water immersion. Water sorption and solubility were assessed by mass gain or loss after storage in water for 30 days. Data were analyzed using ANOVA and Tukey's test (5%). RESULTS: Degree of conversion did not differ statistically among all the tested formulations. Regarding color, only groups with TPO presented satisfactory color stability after one month of water storage (ΔE<3.3). Water sorption and water stability did not differ among the groups. CONCLUSIONS: Degree of conversion, water sorption and water solubility did not differ among all the tested groups. The TPO-based groups were the only materials with satisfactory color stability after one month of water storage. CLINICAL SIGNIFICANCE: The use of a photoinitiator system containing TPO might improve the color stability of resin composites compared with the traditional CQ/amine system while attaining similar physico-chemical properties for the composite.

Effect of nanofillers' size on surface properties after toothbrush abrasion.

PURPOSE: To investigate the effect of filler-particle size of experimental and commercial resin composites, undergoing toothbrush abrasion, on three surface properties: surface roughness (SR), surface gloss (G) and color stability (CS). METHODS: Four model (Ivoclar/Vivadent) and one commercial resin composite (Tokuyama) with varying filler-size from 100-1000 nm were examined. Six discs (10 mm x 2 mm) from each product were prepared and mechanically polished. The samples were then submitted to 20,000 brushing strokes in a toothbrush abrasion machine. SR parameters (Ra, Rt and RSm), G, and CS were measured before and after toothbrush abrasion. Changes in SR and G were analyzed by 2-way ANOVA, with Bonferroni post hoc test. CS values were submitted to one-way ANOVA and Bonferroni post hoc test (alpha=0.05). RESULTS: Initial G values ranged between 73-87 gloss units (GU) and were reduced after toothbrush abrasion to a range of 8-64 GU. Toothbrush abrasion resulted in significant modifications in SR and G amongst the materials tested, attributed to filler sizes. There was statistically significant difference in color (delta E* ranged from 0.38-0.88). Filler size did not affect color stability. Toothbrush abrasion resulted in rougher and matte surfaces for all materials tested. Although the individual differences in surface roughness among filler sizes were not always significant, the correlation showed a trend that larger filler sizes resulted in higher surface roughness after abrasion for the SR parameters Ra and Rt (r = 0.95; r = 0.93, respectively). RSm showed an increase after toothbrush abrasion for all resin composites, however no significant correlation was detected (r = 0.21).There was a significant correlation between G and Ra ratios (r = - 0.95).

Effect of co-initiator ratio on the polymer properties of experimental resin composites formulated with camphorquinone and phenyl-propanedione.

OBJECTIVES: To evaluate the effect of amine ratio (ethyl 4-dimethylaminobenzoate, EDMAB) on the maximum rate of polymerization (R(p)(max)), degree of conversion (DC), Knoop hardness (KH), water sorption (Wsp), water solubility (Wsl) and color changes (DeltaE) over time of resin composites formulated with the photoinitiators camphorquinone (CQ), phenylpropanedione (PPD) and CQ-PPD in combination. MATERIALS AND METHODS: Experimental resin composites were made with photoinitiator:amine ratios of 2:1, 1:1, 1:1.5 and 1:2 by weight. R(p)(max) was evaluated with differential scanning calorimetry (DSC), DC with DSC and Fourier transformed infrared (FTIR) spectroscopy, KH with Knoop indentation, Wsp and Wsl adapted from ISO 4049; and color with a chromameter. The results were analyzed with two-way ANOVA/Tukey's multiple comparison test (p<0.05). RESULTS: The higher the amine ratio in the composite, the higher was DC, R(p)(max), and KH, and the lower was Wsl, regardless of the photoinitiator type. The use of PPD alone resulted in poorer properties than CQ and CQ-PPD. Many factors seem to affect the color changes and the b-axis data revealed that the higher the amine ratio, the higher was the +b value (yellowing) for CQ and CQ-PPD formulations. CONCLUSIONS: Higher amine ratios led to improved polymer properties, but also produced more yellowing in resin composites with CQ and CQ-PPD. The use of PPD alone was not advantageous for producing good final properties when compared to CQ and CQ-PPD.

Cross-link density evaluation through softening tests: effect of ethanol concentration.

OBJECTIVES: The aim of this study was to investigate whether the ethanol concentration used would influence the outcomes obtained through softening tests when comparing light-activation modes. METHODS: Disc specimens (n=20) of Filtek Z250 and Filtek Z100 (3M ESPE) were light activated by standard (S) and pulse-delay (PD) modes. Initial Knoop hardness (KHN) measurements were performed 24h after dry storage at 37 degrees C. Half of the specimens (n=10) of each resin-composite were stored in absolute ethanol (100%) and the other half in 75% ethanol solution, for 24h at room temperature, and KHN was determined anew. Initial hardness data were submitted to Student's t-test (p=0.05). Percentages of hardness decrease were analyzed by two-way ANOVA followed by pairwise Tukey's test (p=0.05). The statistical analyses were performed separately for each resin-composite. RESULTS: No statistically significant differences were observed between standard and pulse-delay modes for initial Knoop hardness values. After storage in 75% ethanol solution, KHN was decreased in all cases but no significant differences were detected between light-activation modes (Filtek Z250: PD=12.6%, S=13.5%; Filtek Z100: PD=13.5%, S=11.8%) regardless of the resin-composite tested. After absolute ethanol storage, higher decrease in KHN were observed. Samples light-activated by the PD mode (Filtek Z250=20.4% and Filtek Z100=16.9%) exhibited significantly higher percentage decrease of KHN than specimens light-activated by the standard mode (Filtek Z250=14.1% and Filtek Z100=8.8%), regardless of the resin-composite tested. CONCLUSION: The ethanol concentration affected the outcomes of the softening test.

Effect of light-curing method on marginal adaptation, microleakage, and microhardness of composite restorations.

The objective of this study was to investigate the effects of different light-curing methods on microleakage, marginal adaptation, and microhardness of composite restorations. Slot-type preparations were made in bovine teeth, with gingival margins on dentin. Specimens were divided into 12 groups (n = 12) according to composite-light-curing unit (LCU) combinations. Three composites were used: Filtek Supreme, Herculite XRV, and Heliomolar. All restorations were placed using the same adhesive. Four LCUs were used: a quartz-tungsten-halogen (QTH) LCU (Optilux 501), a first-generation light-emitting diode (LED) LCU (FreeLight 1), and two second-generation LED LCUs (FreeLight 2 and Translux Power Blue). After finishing and polishing, specimens were subjected to mechanical load cycling (100,000 cycles). Gingival margin adaptation was determined as a function of gap formation using epoxy replicas. Microleakage was evaluated by measuring dye penetration across the gingival wall in cross-sectioned specimens. Microhardness was measured as Knoop Hardness number (KHN) at different occluso-gingival locations in cross-sectioned specimens. Data were analyzed for statistical significance (p = 0.05) using appropriate statistical tests. Marginal adaptation was affected by load-cycling in most specimens, but no significant differences were observed among composites and LCUs. Microleakage was not affected by LCU, except for Heliomolar specimens which when cured with Optilux 501 resulted in higher microleakage scores than those obtained with the other LCUs. For microhardness, Translux Power Blue generally produced the highest values and the FreeLight 1 produced the lowest. The performance of the second-generation LED LCUs generally was similar to that of the QTH control, and better than that of the first-generation LED unit.