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A new method to measure the linear polymerization shrinkage of composites using a particle tracking method with computer vision
In-Bog Lee, Sun-Hong Min, Deog-Gyu Seo, Sun-Young Kim, Youngchul Kwon
J Korean Acad Conserv Dent 2010;35(3):180-187.   Published online May 31, 2010
DOI: https://doi.org/10.5395/JKACD.2010.35.3.180
AbstractAbstract PDFPubReaderePub

Since the introduction of restorative dental composites, their physical properties have been significantly improved. However, polymerization shrinkage is still a major drawback. Many efforts have been made to develop a low shrinking composite, and silorane-based composites have recently been introduced into the market. In addition, many different methods have been developed to measure the polymerization shrinkage.

In this study, we developed a new method to measure the linear polymerization shrinkage of composites without direct contact to a specimen using a particle tracking method with computer vision. The shrinkage kinetics of a commercial silorane-based composite (P90) and two conventional methacrylate-based composites (Z250 and Z350) were investigated and compared. The results were as follows:

The linear shrinkage of composites was 0.33-1.41%. Shrinkage was lowest for the silorane-based (P90) composite, and highest for the flowable Z350 composite.

The new instrument was able to measure the true linear shrinkage of composites in real time without sensitivity to the specimen preparation and geometry.

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Polymerization shrinkage kinetics of silorane-based composites
Youngchul Kwon, In-Bog Lee
J Korean Acad Conserv Dent 2010;35(1):51-58.   Published online January 31, 2010
DOI: https://doi.org/10.5395/JKACD.2010.35.1.051
AbstractAbstract PDFPubReaderePub

Dental composites have improved significantly in physical properties over the past few decades. However, polymerization shrinkage and stress is still the major drawback of composites, limiting its use to selected cases. Much effort has been made to make low shrinking composites to overcome this issue and silorane-based composites have recently been introduced into the market.

The aim of this study was to measure the volumetric polymerization shrinkage kinetics of a silorane-based composite and compare it with conventional methacrylate-based composites in order to evaluate its effectiveness in reducing polymerization shrinkage.

Five commercial methacrylate-based (Beautifil, Z100, Z250, Z350 and Gradia X) and a silorane-based (P90) composites were investigated. The volumetric change of the composites during light polymerization was detected continuously as buoyancy change in distilled water by means of Archemedes'principle, using a newly made volume shrinkage measurement instrument. The null hypothesis was that there were no differences in polymerization shrinkage, peak polymerization shrinkage rate and peak shrinkage time between the silorane-based composite and methacrylate-based composites. The results were as follows:

The shrinkage of silorane-based (P90) composites was the lowest (1.48%), and that of Beautifil composite was the highest (2.80%). There were also significant differences between brands among the methacrylate-based composites.

Peak polymerization shrinkage rate was the lowest in P90 (0.13%/s) and the highest in Z100 (0.34%/s).

The time to reach peak shrinkage rate of the silorane-based composite (P90) was longer (6.7 s) than those of the methacrylate-based composites (2.4-3.1 s).

Peak shrinkage rate showed a strong positive correlation with the product of polymerization shrinkage and the inverse of peak shrinkage time (R = 0.95).

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Original Articles
The change of the initial dynamic visco-elastic modulus of composite resins during light polymerization
Min-Ho Kim, In-Bog Lee
J Korean Acad Conserv Dent 2009;34(5):450-459.   Published online September 30, 2009
DOI: https://doi.org/10.5395/JKACD.2009.34.5.450
AbstractAbstract PDFPubReaderePub

The aim of this study was to measure the initial dynamic modulus changes of light cured composites using a custom made rheometer. The custom made rheometer consisted of 3 parts: (1) a measurement unit of parallel plates made of glass rods, (2) an oscillating shear strain generator with a DC motor and a crank mechanism, (3) a stress measurement device using an electromagnetic torque sensor. This instrument could measure a maximum torque of 2Ncm, and the switch of the light-curing unit was synchronized with the rheometer.

Six commercial composite resins [Z-100 (Z1), Z-250 (Z2), Z-350 (Z3), DenFil (DF), Tetric Ceram (TC), and Clearfil AP-X (CF)] were investigated. A dynamic oscillating shear test was undertaken with the rheometer. A certain volume (14.2 mm3) of composite was loaded between the parallel plates, which were made of glass rods (3 mm in diameter). An oscillating shear strain with a frequency of 6 Hz and amplitude of 0.00579 rad was applied to the specimen and the resultant stress was measured. Data acquisition started simultaneously with light curing, and the changes in visco-elasticity of composites were recorded for 10 seconds. The measurements were repeated 5 times for each composite at 25±0.5℃. Complex shear modulus G*, storage shear modulus G', loss shear modulus G" were calculated from the measured strain-stress curves. Time to reach the complex modulus G* of 10 MPa was determined. The G* and time to reach the G* of 10 MPa of composites were analyzed with One-way ANOVA and Tukey's test (α= 0.05).

The results were as follows.

1. The custom made rheometer in this study reliably measured the initial visco-elastic modulus changes of composites during 10 seconds of light curing.

2. In all composites, the development of complex shear modulus G* had a latent period for 1~2 seconds immediately after the start of light curing, and then increased rapidly during 10 seconds.

3. In all composites, the storage shear modulus G' increased steeper than the loss shear modulus G" during 10 seconds of light curing.

4. The complex shear modulus of Z1 was the highest, followed by CF, Z2, Z3, TC and DF the lowest.

5. Z1 was the fastest and DF was the slowest in the time to reach the complex shear modulus of 10 MPa.

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Effect of instrument compliance on the polymerization shrinkage stress measurements of dental resin composites
Deog-Gyu Seo, Sun-Hong Min, In-Bog Lee
J Korean Acad Conserv Dent 2009;34(2):145-153.   Published online March 31, 2009
DOI: https://doi.org/10.5395/JKACD.2009.34.2.145
AbstractAbstract PDFPubReaderePub

The purpose of this study was to evaluate the effect of instrument compliance on the polymerization shrinkage stress measurements of dental composites. The contraction strain and stress of composites during light curing were measured by a custom made stress-strain analyzer, which consisted of a displacement sensor, a cantilever load cell and a negative feedback mechanism. The instrument can measure the polymerization stress by two modes: with compliance mode in which the instrument compliance is allowed, or without compliance mode in which the instrument compliance is not allowed.

A flowable (Filtek Flow: FF) and two universal hybrid (Z100: Z1 and Z250: Z2) composites were studied. A silane treated metal rod with a diameter of 3.0 mm was fixed at free end of the load cell, and other metal rod was fixed on the base plate. Composite of 1.0 mm thickness was placed between the two rods and light cured. The axial shrinkage strain and stress of the composite were recorded for 10 minutes during polymerization, and the tensile modulus of the materials was also determined with the instrument. The statistical analysis was conducted by ANOVA, paired t-test and Tukey's test (α<0.05).

There were significant differences between the two measurement modes and among materials. With compliance mode, the contraction stress of FF was the highest: 3.11 (0.13), followed by Z1: 2.91 (0.10) and Z2: 1.94 (0.09) MPa. When the instrument compliance is not allowed, the contraction stress of Z1 was the highest: 17.08 (0.89), followed by FF: 10.11 (0.29) and Z2: 9.46 (1.63) MPa. The tensile modulus for Z1, Z2 and FF was 2.31 (0.18), 2.05 (0.20), 1.41 (0.11) GPa, respectively. With compliance mode, the measured stress correlated with the axial shrinkage strain of composite; while without compliance the elastic modulus of materials played a significant role in the stress measurement.

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Slumping resistance and viscoelasticity of resin composite pastes
Hee Yeon Suh, In Bog Lee
J Korean Acad Conserv Dent 2008;33(3):235-245.   Published online May 31, 2008
DOI: https://doi.org/10.5395/JKACD.2008.33.3.235
AbstractAbstract PDFPubReaderePub

The aim of this study was to develop a method for measuring the slumping resistance of resin composites and to relate it to the rheological characteristics.

Five commercial hybrid composites (Z100, Z250, DenFil, Tetric Ceram, ClearFil) and a nanofill composite (Z350) were used to make disc-shaped specimens of 2 mm thickness. An aluminum mold with square shaped cutting surface was pressed onto the composite discs to make standardized imprints. The imprints were light-cured either immediately (non-slumped) or after waiting for 3 minutes at 25℃ (slumped). White stone replicas were made and then scanned for topography using a laser 3-D profilometer. Slumping resistance index (SRI) was defined as the ratio of the groove depth of the slumped specimen to that of the non-slumped specimen. The pre-cure viscoelasticity of each composite was evaluated by an oscillatory shear test and normal stress was measured by a squeeze test using a rheometer. Flow test was also performed using a flow tester. Correlation analysis was performed to investigate the relationship between the viscoelastic properties and the SRI.

SRI varied between the six materials (Z100 < DenFil < Z250 < ClearFil < Tetric Ceram < Z350). The SRI was strongly correlated with the viscous (loss) shear modulus G' but not with the loss tangent. Also, slumping resistance was more closely related to the resistance to shear flow than to the normal stress.

Slumping tendency could be quantified using the imprint method and SRI. The index may be applicable to evaluate the clinical handling characteristics of composites.

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Enamel adhesion of light- and chemical-cured composites coupled by two step self-etch adhesives
Sae-Hee Han, Eun-Soung Kim, Young-Gon Cho
J Korean Acad Conserv Dent 2007;32(3):169-179.   Published online May 31, 2007
DOI: https://doi.org/10.5395/JKACD.2007.32.3.169
AbstractAbstract PDFPubReaderePub

This study was to compare the microshear bond strength (µSBS) of light- and chemically cured composites to enamel coupled with four 2-step self-etch adhesives and also to evaluate the incompatibility between 2-step self-etch adhesives and chemically cured composite resin.

Crown segments of extracted human molars were cut mesiodistally, and a 1 mm thickness of specimen was made. They were assigned to four groups by adhesives used: SE group (Clearfil SE Bond), AdheSE group (AdheSE), Tyrian group (Tyrian SPE/One-Step Plus), and Contax group (Contax). Each adhesive was applied to a cut enamel surface as per the manufacturer's instruction. Light-cured (Filtek Z250) or chemically cured composite (Luxacore Smartmix Dual) was bonded to the enamel of each specimen using a Tygon tube. After storage in distilled water for 24 hours, the bonded specimens were subjected to µSBS testing with a crosshead speed of 1 mm/minute. The mean µSBS (n=20 for each group) was statistically compared using two-way ANOVA, Tukey HSD, and t test at 95% level. Also the interface of enamel and composite was evaluated under FE-SEM.

The results of this study were as follows;

1. The µSBS of the SE Bond group to the enamel was significantly higher than that of the AdheSE group, the Tyrian group, and the Contax group in both the light-cured and the chemically cured composite resin (p < 0.05).

2. There was not a significant difference among the AdheSE group, the Tyrian group, and the Contax group in both the light-cured and the chemically cured composite resin.

3. The µSBS of the light-cured composite resin was significantly higher than that of the chemically cured composite resin when same adhesive was applied to the enamel (p < 0.05).

4. The interface of enamel and all 2-step self-etch adhesives showed close adaptation, and so the incompatibility of the chemically cured composite resin did not show.

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RHEOLOGICAL PROPERTIES OF RESIN COMPOSITES ACCORDING TO THE CHANGE OF MONOMER AND FILLER COMPOSITIONS
In-Bog Lee, Jong-Hyuck Lee, Byung-Hoon Cho, Sang-Tag Lee, Chung-Moon Um
J Korean Acad Conserv Dent 2004;29(6):520-531.   Published online January 14, 2004
DOI: https://doi.org/10.5395/JKACD.2004.29.6.520
AbstractAbstract PDFPubReaderePub
ABSTRACT Objectives.

The aim of this study was to investigate the effect of monomer and filler compositions on the rheological properties related to the handling characteristics of resin composites.

Methods.

Resin matrices that Bis-GMA as base monomer was blended with TEGDMA as diluent at various ratio were mixed with the Barium glass (0.7 um and 1.0 um), 0.04 um fumed silica and 0.5 um round silica. All used fillers were silane treated. In order to vary the viscosity of experimental composites, the type and content of incorporated fillers were changed.

Using a rheometer, a steady shear test and a dynamic oscillatory shear test were used to evaluate the viscosity (η) of resin matrix, and the storage shear modulus (G′), the loss shear modulus (G″), the loss tangent (tanδ) and the complex viscosity (η *) of the composites as a function of frequency ω = 0.1-100 rad/s. To investigate the effect of temperature on the viscosity of composites, a temperature sweep test was also undertaken.

Results.

Resin matrices were Newtonian fluid regardless of diluent concentration and all experimental composites exhibited pseudoplastic behavior with increasing shear rate. The viscosity of composites was exponentially increased with increasing filler volume%. In the same filler volume, the smaller the fillers were used, the higher the viscosities were. The effect of filler size on the viscosity was increased with increasing filler content. Increasing filler content reduced tanδby increasing the G′further than the G″ . The viscosity of composites was decreased exponentially with increasing temperature.

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The effect of viscosity, specimen geometry and adhesion on the linear polymerization shrinkage measurement of light cured composites
In-Bog Lee, Ho-Hyun Son, Hyuk-Chun Kwon, Chung-Moon Um, Byeong-Hoon Cho
J Korean Acad Conserv Dent 2003;28(6):457-466.   Published online November 30, 2003
DOI: https://doi.org/10.5395/JKACD.2003.28.6.457
AbstractAbstract PDFPubReaderePub
Objectives

The aim of study was to investigate the effect of flow, specimen geometry and adhesion on the measurement of linear polymerization shrinkage of light cured composite resins using linear shrinkage measuring device.

Methods

Four commercially available composites - an anterior posterior hybrid composite Z100, a posterior packable composite P60 and two flowable composites, Filtek flow and Tetric flow - were studied. The linear polymerization shrinkage of composites was determined using 'bonded disc method' and 'non-bonded' free shrinkage method at varying C-factor in the range of 1~8 by changing specimen geometry. These measured linear shrinkage values were compared with free volumetric shrinkage values.

The viscosity and flow of composites were determined and compared by measuring the dropping speed of metal rod under constant load.

Results

In non-bonded method, the linear shrinkage approximated one third of true volumetric shrinkage by isotropic contraction. However, in bonded disc method, as the bonded surface increased the linear shrinkage increased up to volumetric shrinkage value by anisotropic contraction. The linear shrinkage value increased with increasing C-factor and approximated true volumetric shrinkage and reached plateau at about C-factor 5~6. The more flow the composite was, reduced linear shrinkage was measured by compensation radial flow.

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The amounts and speed of polymerization shrinkage and microhardness in LED cured composites
Sung-Ho Park, Su-Sun Kim, Yong-Sik Cho, Soon-Young Lee, Do-Hyun Kim, Yong-Joo Jang, Hyun-Sung Mun, Jung-Won Seo, Byung-Duk Noh
J Korean Acad Conserv Dent 2003;28(4):354-359.   Published online July 31, 2003
DOI: https://doi.org/10.5395/JKACD.2003.28.4.354
AbstractAbstract PDFPubReaderePub

This study evaluated the effectiveness of the light emitting diode(LED) units for composite curing. To compare its effectiveness with conventional quartz tungsten halogen (QTH) light curing unit, the microhardness of 2mm composite, Z250, which had been light cured by the LEDs (Ultralume LED2, FreeLight, Developing product D1) or QTH (XL 3000) were compared on the upper and lower surface. One way ANOVA with Tukey and Paired t-test was used at 95% levels of confidence. In addition, the amount of linear polymerization shrinkage was compared between composites which were light cured by QTH or LEDs using a custom-made linometer in 10s and 60s of light curing, and the amount of linear polymerization shrinkage was compared by one way ANOVA with Tukey.

The amount of polymerization shrinkage at 10s was

XL3000 > Ultralume 2, 40, 60> FreeLight, D1 (P<0.05)

The amount of polymerization shrinkage at 60s was

XL3000 > Ultralume 2, 60> Ultralume 2,40> FreeLight, D1 (P<0.05)

The microhardness on the upper and lower surface was as follows;

It was concluded that the LEDs produced lower polymerization shrinkage in 10s and 60s compared with QTH unit. In addition, the microhardness of samples which had been cured with LEDs was lower on the lower surfaces than the upper surfaces whereas there was no difference in QTH cured samples.

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