Light exposure required for optimum conversion of light activated resin systems

OBJECTIVE: The aim of this study was to evaluate the relationship between the degree of conversion (DC) of composites and the light intensity using LED-curing units and also to determine the amount of exposure required to achieve optimal curing. METHOD: The light outputs of light-curing units and the depths of cure of composites exposed to these units were determined using the methods outlined in modified ISO standards, ISO/TS10650 and ISO 4049, respectively. The distributions of DC in composites were investigated by IR spectra of microareas obtained at various depths from the irradiated surface of thin specimens cut out from the cured composites. IR spectra were measured using a Fourier transform infrared spectrometer equipped with a microscopic unit. DC was calculated from the changes in the amount of C=C double bonds in the IR spectra. RESULTS: The light intensity at various depths through the cured composite was calculated from the attenuation coefficient of each material, obtained from the linear relationship between the depth of cure and the logarithm of the amount of exposure, which is defined as the product of the irradiance and irradiation time. There was a third or fourth order regression relationship between DC and the logarithm of total light energy at a particular depth. SIGNIFICANCE: The minimum light energy required to produce a saturated DC was about 1000 s mW/cm2.     

The use of bioactive glass (BAG) in dental composites: A critical review

ObjectiveIn recent years, numerous studies have analyzed the role of bioactive glass (BAG) as remineralizing additives in dental restorative composites. This current review provides a critical analysis of the existing literature, particularly focusing on BAGs prepared via the melt-quench route that form an “apatite-like” phase when immersed in physiological-like solutions.MethodsOnline databases (Science Direct, PubMed and Google Scholar) were used to collect data published from 1962 to 2020. The research papers were analyzed and the relevant papers were selected for this review. Sol–gel BAGs were not included in this review since it is not a cost-effective manufacturing technique that can be upscaled and is difficult to incorporate fluoride.ResultsBAGs release Ca²⁺, PO₄^3? and F^? ions, raise the pH and form apatite. There are numerous published papers on the bioactivity of BAGs, but the different glass compositions, volume fractions, particle sizes, immersion media, time points, and the characterization techniques used, make comparison difficult. Several papers only use certain characterization techniques that do not provide a full picture of the behavior of the glass. It was noted that in most studies, mechanical properties were measured on dry samples, which does not replicate the conditions in the oral environment. Therefore, it is recommended that samples should be immersed for longer time periods in physiological solutions to mimic clinical environments.SignificanceBAGs present major benefits in dentistry, especially their capacity to form apatite, which could potentially fill any marginal gaps produced due to polymerization shrinkage.     

Photoinitiator type and applicability of exposure reciprocity law in filled and unfilled photoactive resins

Objectives

To test the influence of photoinitiator type and filler particle inclusion on the validity of exposure reciprocity law.

Materials and methods

50/50 wt% Bis-GMA/TEGDMA resins were prepared with equimolar concentrations of camphorquinone/DMAEMA (0.20/0.80 mass%) (CQ) or Lucirin-TPO (0.42 mass%), and were used either unfilled or filled to 75 mass%. Specimens were cured with a halogen Swiss Master Light (EMS, Switzerland) using four different curing protocols: 400 mW/cm² for 45 s as reference protocol (18 J/cm²), 1500 mW/cm² for 12 s (18 J/cm²), 3000 mW/cm² for 6 s (18 J/cm²) and 3 s (9 J/cm²). Degree of conversion (DC) was measured in real time for 70 s by FT-NIRS and temperature rise using a thermocouple. Depth of cure was determined with a penetrometer technique.

Results

With respect to DC and depth of cure, exposure reciprocity law did not hold for any tested material, except for the depth of cure of filled CQ-based materials. At similar radiant exposure, DC was significantly higher (p < 0.05) for all unfilled and filled TPO-based materials compared with CQ-based materials. As exposure time was reduced and irradiance increased, TPO-based materials exhibited higher DC whilst an opposite trend was observed for CQ-based materials (p < 0.05). For similar curing regimes, depth of cure of CQ-based materials remained significantly greater than that of TPO-based materials. Adding fillers generally reduced DC, except at higher irradiance for CQ-based materials where a positive effect was observed (p < 0.05).

Significance

The validity of exposure reciprocity law was dependent on several factors, among which photoinitiator type and filler content were important. Lucirin-TPO is a highly reactive and efficient photoinitiator, which may allow the potential for a reduction in curing time of TPO-based photoactive materials in thin sections.     

Influence of resin matrix on the rheology,translucency, and curing potential of experimental flowable composites for bulk-fill applications

ObjectiveTo propose monomer formulations that show an optimal degree of conversion as a function of depth for bulk-fill applications.MethodsFour resin blends were formulated with methacrylate-based monomers: BisGMA + TEGDMA (control); BisEMA + BisGMA + TEGDMA (BisEMA-based); UDMA + BisGMA + TEGDMA (UDMA-based) and BisEMA + UDMA + BisGMA + TEGDMA (BisEMA + UDMA-based). For each material, a photoinitiating system and silanized filler particles were added. The rheological analyses were performed with a rotational rheometer using the cone/plate geometry. CIELab coordinates were assessed over black and white backgrounds using a bench spectrophotometer (SP60, X-Rite) to calculate the translucency parameter (TP) for samples with 0.5, 4, and 6 mm thickness. The degree of CC conversion (DC) was determined by infrared spectroscopy (FTIR/ATR) at 0.05 mm (top), 4, and 6 mm depths (bottom), and the bottom-to-top ratio was considered. A broad spectrum–based LED was used for light activation. Analysis of variance and Tukey’s test (95%) were performed on the results.ResultsThe materials tested showed pseudoplastic and thixotropic behavior and a predominance of viscous effects over elastics. The control resin yielded the lowest viscosity for the entire shear rate investigated, followed by the BisEMA-based, BisEMA + UDMA-based, and UDMA-based group, which had the highest viscosity. The UDMA-based material showed the lowest TP as a function of thickness. Both the materials’ formulations and depths significantly influenced the DC. The UDMA-based group promoted the highest DC ??on the top (71 ± 1%) and 4 mm depth (68 ± 1%) but exhibited lower bottom-to-top DC ratio. The BisEMA + UDMA-based material promoted the highest bottom-to-top DC ratio at 4 mm (99%) and 6 mm (97%).SignificanceThe resin matrix interferes in the rheological behavior, translucency parameter, and polymerization capacity as a function of depth. The material formulated with the addition of UDMA and BisEMA demonstrated the highest curing potential as a function of depth and can be useful for bulk-fill applications.     

Effect of calcium orthophosphate particle size and CaP:glass ratio on optical,mechanical and physicochemical characteristics of experimental composites

ObjectiveEvaluate light transmittance (%T), color change (ΔE), degree of conversion (DC), bottom-to-top Knoop microhardness (KHN), flexural strength (BFS) and modulus (FM), water sorption/solubility (WS/SL) and calcium release of resin composites containing different dicalcium phosphate dihydrate (DCPD)-to-barium glass ratios (DCPD:BG) and DCPD particle sizes.MethodsTen resin-based composites (50 vol% inorganic fraction) were prepared using BG (0.4 µm) and DCPD particles (12 µm, 3 µm or mixture) with DCPD:BG of 1:3, 1:1 or 3:1. A composite without DCPD was used as a control. DC, KHN, %T and ΔE were determined in 2-mm thick specimens. BFS and FM were determined after 24 h. WS/SL was determined after 7 d. Calcium release was determined by coupled plasma optical emission spectroscopy. Data were analyzed by ANOVA/Tukey test (alpha: 0.05).Results%T was significantly reduced in composites with milled, compared to pristine DCPD (p < 0.001). ΔE > 3.3 were observed with DCPD:BG of 1:1 and 3:1 formulated with milled DCPD (p < 0.001). DC increased at 1:1 and 3:1 DCPD:BG (p < 0.001). All composites presented bottom-to-top KHN of at least 0.8. BFS was not affected by DCPD size but was strongly dependent on DCPD:BG (p < 0.001). Reductions in FM were observed with milled DCPD (p < 0.001). WS/SL increased with DCPD:BG (p < 0.001). At 3DCPD: 1BG, using small DCPD particles led to a 35 % increase in calcium release (p < 0.001).SignificanceA trade-off between strength and Ca²⁺ release was observed. In spite of its low strength, the formulation containing 3 DCPD: 1 glass and milled DCPD particles is preferred due to its superior Ca²⁺ release.     

Polymerization shrinkage kinetics and degree of conversion of commercial and experimental resin modified glass ionomer luting cements (RMGICs)

ObjectivesTetrahydrofurfuryl-methacrylate (THFM) and hydroxypropyl-methacrylate (HPM) were used to partially or fully replace HEMA in experimental RMGICs. The experimental materials were compared with home and commercial products in terms of degree of conversion, polymerization shrinkage and exotherm.MethodsTwo commercial RMGICs used were Fuji-Plus (FP, GC, Japan) and RelyX-Luting (RX, 3M-ESPE, USA). Two additional in-house liquids were prepared based on the commercial materials liquids. Eight experimental liquid compositions (F1, F2, F3 and F4 based on Fuji-Plus; R1, R2, R3 and R4 based on RelyX-Luting) were prepared replacing 100% HEMA with HPM in F1 and R1 or 70%/30% HPM/THFM in F2 and R2. 50% HEMA was replaced with THFM in F3 and R3 compared to 30% in F4 and R4. All liquids were mixed with the corresponding commercial powder. Degree of conversion was determined using Fourier-transform infrared spectroscopy (FT-IR). Polymerization shrinkage and exotherm were measured using the bonded-disk method.ResultsCompositions containing HPM (F1 and R1) showed lower degree of conversion compared to experimental compositions containing THFM, home and commercial materials (p < 0.0001). FP-commercial showed significantly higher polymerization shrinkage and exotherm compared to all other materials in both groups (p < 0.0001). FP-commercial showed higher degree of polymerization shrinkage and exotherm at 5 min compared to all materials due to the incorporation of an additional cross-linker (glycerol-dimethacrylate). In general, compositions containing THFM, presented polymerization shrinkage and degree of conversion values similar to their corresponding commercial products.SignificanceTHFM monomer showed promising results and could be potentially useful in the development of new RMGICs with improved properties.     

Acid neutralizing,mechanical and physical properties of pit and fissure sealants containing melt-derived 45S5 bioactive glass

Objectives

The aim of this study was to examine the effects of 45S5 bioactive glass (BAG) on the acid neutralizing, mechanical and physical properties of pit and fissure sealants.

Methods

45S5BAG (<25 μm) was mixed with the silanized glass (180 ± 30 nm) and added into a resin matrix [Bis-GMA/TEGDMA 50/50 (wt%) containing 1% of DMAEMA/CQ 2:1 (wt%)] with varying filler proportions; 0% 45S5BAG + 50% glass (BAG0); 12.5% 45S5BAG + 37.5% glass (BAG12.5); 25% 45S5BAG + 25% glass (BAG25); 37.5% 45S5BAG + 12.5% glass (BAG37.5); and 50% 45S5BAG + 0% glass (BAG50). To evaluate the acid neutralizing properties, specimens were immersed in lactic acid solution (pH 4.0). Then, the change in pH and the time required to raise the pH from 4.0 to 5.5 were measured. In addition, flexural strength, water sorption and solubility were analyzed.

Results

The acid neutralizing properties of each group exhibited increasing pH values as more 45S5BAG was added, and the time required to raise the pH from 4.0 to 5.5 became shorter as the proportion of 45S5BAG increased (P < 0.05). Additionally, the flexural strength decreased according to the increasing proportions of 45S5BAG added (P < 0.05). Water sorption showed an increasing trend with increasing proportions of 45S5 BAG added (P < 0.05). However, the solubility results were similar among the groups (P > 0.05), except for BAG50.

Significance

The novel pit and fissure sealants neutralized the acid solution (pH 4.0) and exhibited appropriate mechanical and physical properties. Therefore, these compounds are suitable candidates for caries-inhibiting dental materials.     

Simultaneous measurement of polymerization stress and curing kinetics for photo-polymerized composites with high filler contents

ObjectivesPhotopolymerized composites are used in a broad range of applications with their performance largely directed by reaction kinetics and contraction accompanying polymerization. The present study was to demonstrate an instrument capable of simultaneously collecting multiple kinetics parameters for a wide range of photopolymerizable systems: degree of conversion (DC), reaction exotherm, and polymerization stress (PS).MethodsOur system consisted of a cantilever beam-based instrument (tensometer) that has been optimized to capture a large range of stress generated by lightly-filled to highly-filled composites. The sample configuration allows the tensometer to be coupled to a fast near infrared (NIR) spectrometer collecting spectra in transmission mode.ResultsUsing our instrument design, simultaneous measurements of PS and DC are performed, for the first time, on a commercial composite with ≈80% (by mass) silica particle fillers. The in situ NIR spectrometer collects more than 10 spectra per second, allowing for thorough characterization of reaction kinetics. With increased instrument sensitivity coupled with the ability to collect real time reaction kinetics information, we show that the external constraint imposed by the cantilever beam during polymerization could affect the rate of cure and final degree of polymerization.SignificanceThe present simultaneous measurement technique is expected to provide new insights into kinetics and property relationships for photopolymerized composites with high filler content such as dental restorative composites.     

Material properties and bioactivity of a resin infiltrant functionalized with polyhedral oligomeric silsesquioxanes

ObjectivesTo investigate the effect of methacrylate polyhedral oligomeric silsesquioxanes (POSS-8) on various material properties and mineral precipitation potential of a resin infiltrant.MethodsA TEGDMA-based resin infiltrant was mixed with 0.5, 1, 3, 5 or 10 wt% POSS-8 or left unchanged (control). Degree of conversion (DC), water sorption (WS), viscosity, elastic modulus (E-modulus), flexural strength (FS), Knoop microhardness (KHN) and softening ratio (SR) were assessed. Growth of calcium phosphate (Ca/P) precipitates infiltrant-treated bovine enamel and dentin specimens immersed in artificial saliva or artificial dentinal fluid, respectively, for 28 days was analyzed by scanning electron microscopy and energy-dispersive X-ray spectroscopy. For viscosity assessment, pure TEGDMA filled with 0–10 wt% POSS-8 was used. Statistical analyses were performed using ANOVA and Tukey's post-hoc tests (p < 0.05).ResultsPOSS-8 did not change the flexural strength, water sorption and softening ratio. The apparent degree of conversion was increased at lower concentrations only while E-modulus remained constant in almost all groups. The particles led to a slight decrease of KHN at concentrations below 3%. The effect on viscosity is comparable to the reinforcement effect. Ca/P precipitates formed on dentin specimens treated with POSS-8-filled infiltrant after 4 weeks of immersion, but were not detected on the control infiltrant. The mineral precipitation on enamel was not improved by POSS-8.SignificancePOSS-8 particles did not worsen the material properties of the resin infiltrant, while the Ca/P precipitation on dentin was stimulated.     

Clinical comparison between a resin-reinforced self-cured glass ionomer cement and a composite resin for direct bonding of orthodontic brackets Part 1: wetting with water

The purpose of this study was to compare the clinical performance of a resin-reinforced self-cured glass ionomer cement to a standard composite resin in a split mouth design, by using both systems for direct bonding of orthodontic stainless steel brackets in every patient. Forty eight patients (34 females and 14 males, of which 29 were adults > 18 years of age) with fixed appliances were followed for a mean period of 10 months (range 4–16 months). The performance of 864 stainless steel brackets was evaluated: 404 brackets were bonded with GC Fuji Ortho glass ionomer cement (GC Industrial, Tokyo, Japan) onto teeth soaked with water, and 460 were bonded with System 1 + composite resin (Ormco, Glendora, CA). System 1 + recorded an overall failure rate (18.2%) significantly higher (p < 0.05) than GC Fuji Ortho (7.9%). There were no statistically significant differences (p> 0.05) between the failure rates in the upper and lower arches with either material. Both in the upper and lower arches, System 1 + exhibited a failure rate significantly higher (p < 0.05) than GC Fuji Ortho. When the bonding performance of the six anterior teeth was compared with first and second premolars, no statistically significant differences were found (p> 0.05) between bonding agents in either arch. System 1 + exhibited a failure rate significantly higher (p < 0.05) than GC Fuji Ortho, both in the anterior and posterior segments. Both bonding agents failed mainly at the enamel—adhesive interface, without causing any damage to the enamel.