Bum Soon Lim

Reduction of polymerization contraction stress for dental composites by two-step light-activation

OBJECTIVESnThe goal of this study was to assess the reduction of polymerization contraction stress of composites during a two-step light-activation process and to relate this reduction to the process of polymerization shrinkage and specimen thickness.nnnMETHODSnThree test procedures were performed to compare two-step light-activation with delay with one-step continuous irradiation of composites: polymerization contraction stress using a closed-loop servohydraulic testing instrument, polymerization shrinkage by a mercury dilatometer, and degree of conversion by FTIR. For the one-step continuous curing method, the samples were light-activated for 60s at 330 mW/cm(2). For the two-step curing method, a 5s light exposure at 60 mW/cm(2) was followed by 2 min without light exposure, and then a second light exposure for 60s at 330 mW/cm(2). The same light parameters were used for measurements of stress, shrinkage, and degree of conversion. Three composites, Heliomolar, Herculite and Z100 were evaluated. The contraction stress experiments were repeated with varying thickness for Herculite using the one-step and two different two-step techniques.nnnRESULTSnPolymerization contraction stress 10 min after light-activation was significantly reduced (P<0.05) by the two-step method: 29.7% for Heliomolar, 26.5% for Herculite, and 19.0% for Z100. Total volumetric shrinkage and degree of conversion were not significantly different for composites cured by the two different techniques. Increasing the thickness of the composite sample reduced the measured contraction stress, especially for one of the two-step curing methods.nnnSIGNIFICANCEnA combination of low initial energy density followed by a lag period before a final high-intensity light irradiation provides a reduction of polymerization contraction stresses in dental composites. The stress reductions cannot be attributed to reductions in degree of conversion or unrestrained volumetric shrinkage.

Effect of filler fraction and filler surface treatment on wear of microfilled composites

OBJECTIVESnThe aim of this study was to determine the effect of filler content and surface treatment on the wear of microfilled composites.nnnMETHODSnFour microfilled composites with different filler contents (A=20, B=25, C=30, and D=35 vol.%) were made with a light-cured resin (Bis-GMA/UDMA/TEGDMA). The surface treatment of the colloidal silica in each varied: F=functional silane, NF=non-functional silane, U=untreated. Silux Plus served as a control. Specimens were made in steel molds and cured in a light curing unit Triad II (40s/side). Abrasion and attrition wear were evaluated in vitro in a wear tester (OHSU oral wear simulator) with an abrasive slurry (poppy seeds + PMMA) and a human enamel antagonist. The average of five specimens was computed and compared using a ANOVA/Tukeys test at P < or = 0.05. The surface of the wear patterns and the distribution of filler particles were examined using a scanning electron microscope and digital imaging.nnnRESULTSnAs filler volume increased, wear was reduced regardless of filler treatment. Amounts of wear for specimens C and D were significantly lower than specimens A and B. Composites with functional silane treated microfiller (Group F) produced significantly less wear than those with non-functional microfiller (Group NF) at 30 and 35 vol.%, and less than the untreated microfiller (Group U) at 30 vol.%. Scanning electron microscopy of specimens of group NF showed large filler agglomerates (size > 1 microm) in the resin matrix, while specimens of group F and U showed fewer agglomerates. Digital imaging analysis revealed small filler clusters (size < or = 1 microm) in the resin matrix of all specimens.nnnSIGNIFICANCEnWear resistance of microfilled composites is enhanced by higher filler volumes irrespective of surface treatment, but good filler/matrix adhesion is needed to minimize wear.

Dynamic mechanical analysis of storage modulus development in light-activated polymer matrix composites.

OBJECTIVESnThe goal of this study was to evaluate the potential for using dynamic mechanical analysis of tubular geometry in a three-point flexure fixture for monitoring the storage modulus development of a light-activated polymer matrix composite.nnnMETHODSnComposite samples were inserted into PTFE tubes and tested in a three-point bend fixture in a dynamic mechanical analyzer (DMA) at 200 Hz with 20 microm amplitude. Samples were light activated for 60s (385 mW/cm(2) at the composite surface) and storage modulus (E) was measured continuously for the seven light-activated composites studied (one microfill, four hybrids and two unfilled resins). Cores of composite were removed from the PTFE sheath after 13.5 min and evaluated with the same parameters in the DMA. A finite element model of the test configuration was created and used to estimate operating parameters for the DMA. Degree of conversion (DC) was measured using micro-Fourier Transform Infrared (FTIR) spectroscopy for the microfilled composite samples and one hybrid 13.5 and 60 min after light activation.nnnRESULTSnThe E for a generic hybrid and microfilled composite was 13,400+/-1100 and 5900+/-200 MPa, respectively, when cured within the tube and then removed and tested in the DMA. DC was 54.6% for the hybrid and 60.6% for the microfill. A linear regression of E for the sheath and core vs core alone (r(2)=0.986) indicated a linear scaling of the sheath and core values for E enabling a correction for estimated E values of the composite core.nnnSIGNIFICANCEnThis method estimates the storage modulus growth during light-activated polymerization of highly filled dimethacrylates. Although the approach is phenomenological in that quantitative measurements of E are not made directly from the DMA, estimates of early polymerization kinetics appear to be validated by three different approaches.

Effects of different fluoride recharging protocols on fluoride ion release from various orthodontic adhesives

OBJECTIVEnThe purpose of this study was to find the most effective fluoride recharging protocol for orthodontic adhesives.nnnMETHODSnFive orthodontic adhesives were used: a non-fluoride-releasing composite, a fluoride-releasing composite, a polyacid-modified composite (compomer), and two resin-modified glass-ionomer cements (RMGICs). Each specimen was placed into deionized water (DW) and the initial fluoride ion release was measured for 2 months. Each specimen was then subjected to four different treatments to simulate a fluoride recharge: 1000ppm NaF solution, acidulated phosphate fluoride gel (APF), fluoride-containing dentifrice and DW (control). After topical fluoride treatment, each specimen was submitted to fluoride re-release tests.nnnRESULTSnFluoride-containing adhesives initially showed higher rates of fluoride ion release, but significantly declined to lower levels. The overall cumulative fluoride ion release during the initial period was RMGICs>compomer>fluoride-containing composite>non-fluoride-releasing composite. After topical fluoride treatment, the amount of fluoride ion re-released was proportional to the amount of fluoride ion previously released from the adhesives. However, the amount of fluoride ions released only lasted for 2 days and then returned to the levels before fluoride application. The overall cumulative fluoride ion re-release according to the fluoride treatments was APF and NaF solution>dentifrice.nnnCONCLUSIONnThis study suggests that using the combination of RMGICs and a fluoride-containing mouth rinse solution is the most effective protocol for long-term fluoride re-release from orthodontic adhesives, given the difficulty of routine use of APF at home, although all topical fluoride treatments can recharge fluoride ion in adhesives.

Conjugated vinyl derivatives of chitooligosaccharide: Synthesis and characterization

The introduction of a conjugated vinyl group to chitooligosaccharide (COS) has been easily accomplished by the coupling of glycidyl methacrylate (GMA) to COS in aqueous solution without an additional catalyst. Depolymerization of chitosan was carried out by deaminative cleavage using sodium nitrite. The average degree of polymerization of COS could be controlled by varying the molar ratio of sodium nitrite and the amino group of chitosan. The degree of substitution (percentage), as determined by 1H NMR, of GMA to COS increased up to 60% at a reaction time of 48 h. The structure of products (COS-GMAs) were identified by Fourier transform infrared spectroscopy, 1H NMR, and 13C NMR. The resulting COS-GMAs were readily soluble in neutral water, like the original COS, and exhibited an excellent antimicrobial activity. The reactivity of COS-GMA was investigated by the reaction with poly(vinyl alcohol) (PVA). The reaction products were found to have a lower crystallinity than PVA because of the introduction of the COS-GMA units.

Osteoblast-Like Cell Behaviors on Non-Woven Silica Fabric

The biological activity of osteoblast-like MC3T3-E1 cells on the newly developed non-woven silica fabric was investigated. The attachment, proliferation, and differentiation of osteoblast-like MC3T3-E1 cells were evaluated by MTS and alkaline phosphatase activity assays, respectively. The non-woven silica fabric showed higher biological activities than those of tissue culture plates with regard to attachment and proliferation while there was no significant difference with respect to differentiation. These results suggest that the non-woven silica fabric has a potential application as a bone grafting materia

Bioactive Non-Woven Silica Fabric Made Through Electro-Spinning Method

Non-woven silica fabric was made by electro-spinning method for the application as a bone grafting material. The silica gel, the source material for electro-spinning, was prepared by the hydrolysis of tetraethyl orthosilicate in the presence of water, hydrochloric acid and ethanol. It was transferred to a syringe (spinneret), which was connected to the high voltage supply generating a high electric field between the spinneret and the ground collecting drum. The silica fibers were spun under the electric field of 2 KV/cm. Their diameters were in the range from about 100 nm to 5 µm. After soaking in the SBF for 4 week, low crystalline apatite crystals were observed to occur partly on their surfaces. From the results, it can be concluded that the non-woven silica fabric made by electro-spinning method has the apatite forming ability in the SBF and it means it has a potential to be used as a bone grafting material because of its apatite-forming ability, high surface area to volume ratio and high porosity.

Evaluation of a Chitosan Nano-Hybrid Material Containing Silanol Group and Calcium Salt as a Bioactive Bone Graft

A bioactive chitosan-siloxane nano-hybrid material was newly developed and evaluated for the potential application as a bone graft material. The chitosan which can be dissolved in organic solvent was synthesized by the reaction with phtalic anhydride (Ph-Chitosan) and it was then reacted with 3-isocyanatopropyl triethoxysilane (Si-Chitosan) in dimethylformamide. Following this, the Si-Chitosan was hydrolyzed and condensed to yield a hybrid sol-gel material (Si-O-Chitosan). The gelation was carried out for 1 week at ambient condition in a covered Teflon mold with a few pinholes and then dried under vacuum at room temperature for 48 h. The bioactivity of the chitosan nano-hybrid material was evaluated by examining the apatite forming ability in the simulated body fluid (SBF). The surface microstructure and functional groups of the specimen was analyzed by field emission scanning electron microscopy and Fourier transformed infrared spectroscopy, respectively. The crystal phases of the specimen before and after the bioactivity testing were analyzed by thin film X-ray diffractometry. Newly developed chitosan nano-hybrid material showed apatite-forming ability in the SBF within 1 week soaking and this ability was believed to come from the silanol group formed on the surface of Si-O-Chitosan and calcium salt which increased the ionic activity product of apatite in the SBF.

Apatite Forming Ability of a Non-Woven Silica Fabric Containing Calcium

Non-woven silica fabric was made by electro-spinning method for the potential application as a bone grafting material. The silica gel, the source material for electro-spinning, was prepared by the hydrolysis of tetraethyl orthosilicate in the presence of calcium salt, water, hydrochloric acid and ethanol. It was transferred to a syringe, which was connected to the high voltage supply generating a high electric field between the spinneret and the ground collecting drum. The silica fibers containing calcium were spun under the electric field of 2 KV/cm. Their diameters were in the range from about 0.3 μm to 8 μm. It was heat-treated at 300 oC for 3 hours. After soaking in the SBF for 1 week, low crystalline apatite crystals were observed to occur on their surfaces. From the results, it can be concluded that the non-woven silica fabric containing calcium made by electro-spinning method and then heat-treated has a bioactivity. It means it has a potential to be used as a bone grafting material because of its apatite-forming ability, high surface area to volume ratio and high porosity.

Effect of Silica Content in the PMMA/Silica Nano-Composite on the Mechanical Properties and Growth Behavior of Calcium Phosphate Crystals during Cell Culture

The effect of silica content in the PMMA/silica nano-composite on the mechanical properties and the growth behavior of apatite crystals were investigated. The PMMA/silica nano-composites with different silica content were synthesized through the sol-gel reaction with triethoxysilane end-capped PMMA and tetraethyl orthosilicate (TEOS). The compressive strength showed its maximum value when the content of TEOS was 20 wt% while the elastic modulus showed its maximum value when the content of TEOS was 60 wt%. The growth behavior of the apatite crystals following the cell culture showed different response according to the silica content. As increasing the TEOS content, the shape of the apatite crystals changed from globule-like structure to fiber-like one.