Curing efficiency of dental resin composites formulated with camphorquinone or trimethylbenzoyl-diphenyl-phosphine oxide
Luis Felipe J. Schneider, Larissa Maria Cavalcante, Scott A. Prah, Carmem S. Pfeifer, Jack L. Ferracane. “Curing efficiency of dental resin composites formulated with camphorquinone or trimethylbenzoyl-diphenyl-phosphine oxide” Dental Materials. December 2011: Online
Summary:
This research presents trimethylbenzoyl-diphenyl-phosphine oxide (TPO) as an alternative to camphorquinone (CQ) photoinitiator systems for dental resins. An immediate advantage is the low color of TPO in comparison to the strong yellow color of CQ. Testing using a spectrophotometer and differential scanning calorimetry (DSC) revealed that TPO had higher reactivity than CQ. CQ exhibited higher absorbed power density, (PDabs) and better depth of cure.
Materials
Testing of each photoinitiator was performed using 50:50 formulations of 2,2-bis[4-2(2-hydroxy-3-
methacroyloxypropoxy)phenyl]propane (Bis-GMA, Esstech) and triethyleneglycol dimethacrylate (TEGDMA, Esstech).
Micro-Raman spectroscopic analysis of the degree of conversion of composite resins containing different initiators cured by polywave or monowave LED units
Vesna Miletic a, Ario Santini b,
a Clinical Lecturer, University of Belgrade, School of Dentistry, Department of Restorative Odontology and Endodontics, Rankeova 4, Belgrade, Serbia
b Director of Biomaterials Research, The University of Edinburgh, Edinburgh Postgraduate Dental Institute, Lauriston Place, Edinburgh EH3 9HA, United Kingdom
Received 20 August 2011; revised 28 October 2011; Accepted 30 October 2011. Available online 6 November 2011.
Objectives
To determine the degree of conversion (DC) over 48 h post-curing of resin mixtures containing trimethylbenzoyl-diphenylphosphine oxide (TPO) initiator cured by a polywave or a monowave LED light-curing unit (LCU).
Methods
In resin mixtures based on equal weight percent (wt%) of BisGMA and TEGDMA the following initiators were added: 0.2wt% camphorquinone (CQ) + 0.8wt% ethyl-4-dimethylaminobenzoate (EDMAB) (Group 1); 1wt% TPO (Group 2) and 0.1wt% CQ + 0.4wt% EDMAB + 0.5wt% TPO (Group 3). Half of the samples in each group (n = 5) were cured using a polywave (bluephase® G2, Ivoclar Vivadent) or a monowave LED LCU (bluephase®, Ivoclar Vivadent). The DC was measured using micro-Raman spectroscopy within 5 min and then 1, 3, 6, 24 and 48 h post-irradiation. The data were analyzed using general linear model and two-way ANOVA for the factors ‘time’, ‘material’, ‘surface’ and ‘LCU’ at α=0.05.
Results
The initial DC values obtained upon light curing remained similar over a 48 h period. bluephase® G2 produced the highest DC in Group 2 followed by Group 3, and Group 1. bluephase® resulted in the highest DC in Group 1, followed by Group 2 and Group 3 (p < 0.05).
Conclusions
Unfilled resin materials containing both TPO- and CQ-amine initiators are effectively cured using bluephase® G2. Resin mixture with the same wt% of initiators is better cured when TPO is the only initiator, compared to CQ-amine only or combined TPO and CQ-amine system. After initial light cure, no additional conversion of uncured monomers was detected in an unfilled resin material over 48 h at 37 °C.
Results: Rockwell hardness for LC resins showed that resins could be cured with up to 0.15% AgBz, while the hardness of CC resins were unaffected in the concentrations tested. UV–Vis spectroscopy and transmission electron microscopy confirmed the presence of AgNPs in both LC and CC resins. Generally, CC resins had better distribution of and much smaller AgNPs as compared to LC resins overall. In some samples, especially in LC resins, nanoclusters were visible. An in vitro release study over four-weeks showed that CC resins released the most Ag+ ions, with release detected in all samples. However, LC resins only released Ag+ ions when AgBz concentration was greater than 0.1% (w/w). AgNP-loaded CC resins made with 0.2 and 0.5% (w/w) AgBz were tested for antibacterial activity in vitro against Streptococcus mutans, and results showed 52.4% and a 97.5% bacterial inhibition, respectively. Further work is now warranted to test mechanical properties and to optimize the initiator system to produce commercially useful dental and medical resins.
Significance: Success in this work could lead to a series of antimicrobial medical and dental biomaterials that can prevent secondary caries and infection of implants.
The efficiency of 4,4′-bis(N,N-diethylamino)benzophenone (DEABP) for the polymerization of dimethacrylate monomers in thick sections (1–2 mm) was studied. DEABP (λmax = 365 nm) represents a complete initiating system as it contains both ketone and amine functional groups. During irradiation, DEABP photobleaches at a fast rate causing deeper penetration of light through the underlying layers, but the photoinitiation efficiency (rate of polymerization per photon absorption rate) is relatively poor. As a result, irradiation of methacrylate monomers at 365 nm results in a slow average polymerization rate and a reduced monomer conversion for thick sections due to the light attenuation caused by the high absorptivity of DEABP and photolysis products. These results highlight the inherent interlinking of light attenuation and photobleaching rate in polymerization of thick sections.
BisGMA/TEGDMA ratio and filler content effects on shrinkage stress
Abstract
Objective
To investigate the contributions of BisGMA:TEGDMA and filler content on polymerization stress, along with the influence of variables associated with stress development, namely, degree of conversion, reaction rate, shrinkage, elastic modulus and loss tangent for a series of experimental dental composites.
Methods
Twenty formulations with BisGMA:TEGDMA ratios of 3:7, 4:6, 5:5, 6:4 and 7:3 and barium glass filler levels of 40, 50, 60 or 70wt% were studied. Polymerization stress was determined in a tensilometer, inserting the composite between acrylic rods fixed to clamps of a universal test machine and dividing the maximum load recorded by the rods cross-sectional area. Conversion and reaction rate were determined by infra-red spectroscopy. Shrinkage was measured by mercury dilatometer. Modulus was obtained by three-point bending. Loss tangent was determined by dynamic nanoindentation. Regression analyses were performed to estimate the effect of organic and inorganic contents on each studied variable, while a stepwise forward regression identified significant variables for polymerization stress.
Results
All variables showed dependence on inorganic concentration and monomeric content. The resin matrix showed a stronger influence on polymerization stress, conversion and reaction rate, whereas filler fraction showed a stronger influence on shrinkage, modulus and loss tangent. Shrinkage and conversion were significantly related to polymerization stress.
Significance
Both the inorganic filler concentration and monomeric content affect polymerization stress, but the stronger influence of the resin matrix suggests that it may be possible to reduce stress by modifying resin composition without sacrificing filler content. The main challenge is to develop formulations with low shrinkage without sacrificing degree of conversion.
Synthesis of Nanosilica Fillers for Experimental Dental Nanocomposites and Their Characterisations
Tuan Noraihan Azila Tuan Rahim1, Dasmawati Mohamad1*, Abdul Rashid Ismail1 and Hazizan Md Akil2
1School of Dental Sciences, Universiti Sains Malaysia,
2School of Material and Mineral Resources Engineering, Universiti Sains Malaysia
The aim of this study was to synthesise nanosilica fillers for use in the fabrication of experimental dental nanocomposites and to evaluate their properties, including surface and mechanical properties. Monodispersed, spherical silica nanoparticles were synthesised via a sol-gel process, and a size range of 10–20 nm was obtained. Surface treatment of the nanosilica was carried out with the silane coupling agent γ-methacryloxypropyltrimethoxysilane (MPS) to reduce agglomeration of nanosilica. Experimental dental nanocomposites with two different filler contents, 30 and 35 wt%, were fabricated and polymerised with a light curing unit for 40 s. The surface morphology, surface roughness, flexural strength and elastic modulus were evaluated and compared. A nanocomposite with 35% filler content showed higher filler compaction, lower surface roughness and higher elastic modulus than a nanocomposite filled with 30% filler. However, the nanocomposite filled with 30% filler content showed higher flexural strength. Based on the results obtained, the synthesised nanosilica is a promising material for the fabrication of dental nanocomposites for tooth-filling applications.
Preparation and characterization of light-cured methacrylate/montmorillonite nanocomposites
Veronica Mucci, Javier Perez, Claudia I Vallo
ABSTRACT
Polymer/clay nanocomposites were prepared from dimethacrylate monomers, commonly used in dental restorative resins, and an organically modified silicate (montmorillonite). The photopolymerization process was hardly affected by the presence of the silicate filler, and thus 2 mm thick samples containing 3 wt% clay were extensively cured. Transmission electron microscopy revealed that the montmorillonite platelets were either intercalated or exfoliated. Nevertheless, for all formulations, intermediate-sized aggregates of about 1 µm were present and their fraction increased as the amount of filler increased. The presence of the clay was found to have no major effect on the flexural modulus and compressive yield strength of the nanocomposites. Moreover, the water uptake of nanocomposites containing 3 wt% clay was about 10–15% higher than that of unfilled monomers. Modification of the clay surface with alternative organic cations is certainly necessary in order to achieve an optimal dispersion of the clay in the polymer matrix.
Forming Clear, wettable silicone hydrogel articles without surface treatments
Document Type and Number: Kind Code: A1
Inventors: Vanderlaan, Douglas C. (Jacksonville, FL, US), Petisce, James R. (San Diego, CA, US), Alli, Azaam (Jacksonville, FL, US), Mccabe, Kevin P. (St. Augustine Beach, FL, US)
ABSTRACT
The present invention is a composition, which may be used to form contact lenses, comprising at least one silicone containing component, at least one hydrophilic component, at least one high molecular weight hydrophilic polymer and at least one diluent with an alpha value of about 0.5 to about 1 and a Hansen solubility parameter of less than about 10.
…Some of the diluents from Example 1 were used to make contact lenses from the monomer mix shown in Table 3…
Objectives: To establish the relationship of resin composition and resin hydrophilicity (indicated by solubility parameters and logP) to water sorption (WS), solubility, and degree of double bond conversion (DC) of resin mixtures designed for adhesive restoratives by varying the concentration of pyromellitic glycerol dimethacrylate (PMGDM) and various co-monomers.
Methods: Sixteen resin mixtures were prepared with (30–70) mass fraction % PMGDM. At given PMGDM concentrations there were up to five compositions with increasing logP. Polymer disks (13mm×0.7mm) were exposed to 96% relative humidity (RH) to determine water sorption in humid atmosphere (WSH) and subsequently immersed in water for immersion water sorption (WSI) and solubility. DC was assessed by near infrared spectroscopy.
Results: WSI was somewhat higher than WSH, which ranged from (2.1 to 5.3) mass fraction %. Both data were positively correlated to PMGDM concentrations [Pearson correlation, p<0.02; R2=0.74, 0.73 (WSI)] and solubility (R2=0.64), but not to logP. When grouped by structural similarities, i.e., base resins with bisphenol A core (Group B), Group O containing diluent monomers, or Group U containing urethane dimethacrylate, WS within each group was inversely correlated to logP with R2=0.98, 0.81, 0.95, and WS/solubility correlation improved with R2=0.88, 0.92 and 0.75, respectively. Solubility ranging from 0.3% to 2.3% was inversely related to DC (r=−0.872). Conversion ranging from 41% to 81% was lower for resins with high base monomer concentrations and highest in mixtures with UDMA.
Significance: LogP was a good predictor of WS after grouping the resins according to functional, compositional and structural similarities. WS and conversion were reasonably well predicted from Hoy’s solubility parameters and other physical resin properties.
Objectives: The role of inorganic content on physical properties of resin composites is well known. However, its influence on polymerization stress development has not been established. The aim of this investigation was to evaluate the influence of inorganic fraction on polymerization stress and its determinants, namely, volumetric shrinkage, elastic modulus and degree of conversion.
Methods: Eight experimental composites containing 1:1 BisGMA (bisphenylglycidyl dimethacrylate):TEGDMA (triethylene glycol dimethacrylate) (in mol) and barium glass at increasing concentrations from 25 to 60vol.% (5% increments) were tested. Stress was determined in a universal test machine using acrylic as bonding substrate. Nominal polymerization stress was obtained diving the maximum load by the cross-surface area. Shrinkage was measured using a water picnometer. Elastic modulus was obtained by three-point flexural test. Degree of conversion was determined by FT-Raman spectroscopy.
Results: Polymerization stress and shrinkage showed inverse relationships with filler content (R2=0.965 and R2=0.966, respectively). Elastic modulus presented a direct correlation with inorganic content (R2=0.984). Degree of conversion did not vary significantly. Polymerization stress showed a strong direct correlation with shrinkage (R2=0.982) and inverse with elastic modulus (R2=0.966).
Significance: High inorganic contents were associated with low polymerization stress values, which can be explained by the reduced volumetric shrinkage presented by heavily filled composites.
Share This Post!
wt% were studied. Polymerization stress was determined in a tensilometer, inserting the composite between acrylic rods fixed to clamps of a universal test machine and dividing the maximum load recorded by the rods cross-sectional area. Conversion and reaction rate were determined by infra-red spectroscopy. Shrinkage was measured by mercury dilatometer. Modulus was obtained by three-point bending. Loss tangent was determined by dynamic nanoindentation. Regression analyses were performed to estimate the effect of organic and inorganic contents on each studied variable, while a stepwise forward regression identified significant variables for polymerization stress.