• Title/Summary/Keyword: curing shrinkage

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STRAIN AND TEMPERATURE CHANGES DURING THE POLYMERIZATION OF AUTOPOLYMERIZING ACRYLIC RESINS

  • Ahn Hyung-Jun;Kim Chang-Whe;Kim Yung-Soo
    • The Journal of Korean Academy of Prosthodontics
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    • v.39 no.6
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    • pp.709-734
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    • 2001
  • The aims of this experiment were to investigate the strain and temperature changes simultaneously within autopolymerzing acrylic resin specimens. A computerized data acquisition system with an electrical resistance strain gauge and a thermocouple was used over time periods up to 180 minutes. The overall strain kinetics, the effects of stress relaxation and additional heat supply during the polymerization were evaluated. Stone mold replicas with an inner butt-joint rectangular cavity ($40.0{\times}25.0mm$, 5.0mm in depth) were duplicated from a brass master mold. A strain gauge (AE-11-S50N-120-EC, CAS Inc., Korea) and a thermocouple were installed within the cavity, which had been connected to a personal computer and a precision signal conditioning amplifier (DA1600 Dynamic Strain Amplifier, CAS Inc., Korea) so that real-time recordings of both polymerization-induced strain and temperature changes were performed. After each of fresh resin mixture was poured into the mold replica, data recording was done up to 180 minutes with three-second interval. Each of two poly(methyl methacrylate) products (Duralay, Vertex) and a vinyl ethyl methacrylate product (Snap) was examined repeatedly ten times. Additionally, removal procedures were done after 15, 30 and 60 minutes from the start of mixing to evaluate the effect of stress relaxation after deflasking. Six specimens for each of nine conditions were examined. After removal from the mold, the specimen continued bench-curing up to 180 minutes. Using a waterbath (Hanau Junior Curing Unit, Model No.76-0, Teledyne Hanau, New York, U.S.A.) with its temperature control maintained at $50^{\circ}C$, heat-soaking procedures with two different durations (15 and 45 minutes) were done to evaluate the effect of additional heat supply on the strain and temperature changes within the specimen during the polymerization. Five specimens for each of six conditions were examined. Within the parameters of this study the following results were drawn: 1. The mean shrinkage strains reached $-3095{\mu}{\epsilon},\;-1796{\mu}{\epsilon}$ and $-2959{\mu}{\epsilon}$ for Duralay, Snap and Vertex, respectively. The mean maximum temperature rise reached $56.7^{\circ}C,\;41.3^{\circ}C$ and $56.1^{\circ}C$ for Duralay, Snap, and Vertex, respectively. A vinyl ethyl methacrylate product (Snap) showed significantly less polymerization shrinkage strain (p<0.01) and significantly lower maximum temperature rise (p<0.01) than the other two poly(methyl methacrylate) products (Duralay, Vertex). 2. Mean maximum shrinkage rate for each resin was calculated to $-31.8{\mu}{\epsilon}/sec,\;-15.9{\mu}{\epsilon}/sec$ and $-31.8{\mu}{\epsilon}/sec$ for Duralay, Snap and Vertex, respectively. Snap showed significantly lower maximum shrinkage rate than Duralay and Vertex (p<0.01). 3. From the second experiment, some expansion was observed immediately after removal of specimen from the mold, and the amount of expansion increased as the removal time was delayed. For each removal time, Snap showed significantly less strain changes than the other two poly(methyl methacrylate) products (p<0.05). 4. During the external heat supply for the resins, higher maximum temperature rises were found. Meanwhile, the maximum shrinkage rates were not different from those of room temperature polymerizations. 5. From the third experiment, the external heat supply for the resins during polymerization could temporarily decrease or even reverse shrinkage strains of each material. But, shrinkage re-occurred in the linear nature after completion of heat supply. 6. Linear thermal expansion coefficients obtained from the end of heat supply continuing for an additional 5 minutes, showed that Snap exhibited significantly lower values than the other two poly(methyl methacrylate) products (p<0.01). Moreover, little difference was found between the mean linear thermal expansion coefficients obtained from two different heating durations (p>0.05).

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EFFECT OF INTERMITTENT POLYMERIZATION ON THE RATE OF POLYMERIZATION SHRINKAGE AND CUSPAL DEFLECTION IN COMPOSITE RESIN (복합 레진의 간헐적 광중합 방법이 중합 수축 속도와 치아의 교두 변위에 미치는 영향)

  • Kim, Min-Kyung;Park, Sung-Ho;Seo, Deog-Gyu;Song, Yun-Jung;Lee, Yoon;Lee, Chan-Young
    • Restorative Dentistry and Endodontics
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    • v.33 no.4
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    • pp.341-351
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    • 2008
  • This study investigated the effect of intermittent polymerization on the rate of polymerization shrinkage and cuspal deflection in composite resins. The linear polymerization shrinkage of each composite was measured using the custom-made linometer along with the light shutter specially devised to block the light at the previously determined interval. Samples were divided into 4 groups by light curing method; Group 1) continuous light (60s with light on); Group 2) intermittent light (cycles of 3s with 2s light on & 1s with light off for 90s): Group 3) intermittent light (cycles of 2s with 1s light on & 1s with light off for 120s); Group 4) intermittent light (cycles of 3s with 1s light on & 2s with light off for 180s). The amount of linear polymerization shrinkage was measured and its maximum rate (Rmax) and peak time (PT) in the first 15 seconds were calculated. For the measurement of cuspal deflection of teeth, MOD cavities were prepared in 10 extracted maxillary premolars. Reduction in the intercuspal distance was measured by the custom-made cuspal deflection measuring machine. ANOVA analysis was used for the comparison of the light curing groups and t-test was used to determine significant difference between the composite resins. Pyramid showed the greater amount of polymerization shrinkage than Heliomolar (p < 0.05). There was no significant difference in the linear polymerization shrinkage among the groups. The Rmax was group 4 < 3, 2 < 1 in Heliomolar and group 3 < 4 < 2, 1 in Pyramid (p < 0.05). Pyramid demonstrated greater cuspal deflection than Heliomolar. The cuspal deflection in Heliomolar was group 4 < 3 < 2, 1 and group 4, 3 < 2, 1 in Pyramid (p < 0.05). It was concluded that the reduced rate of polymerization shrinkage by intermittent polymerization can help to decrease the cuspal deflection.

Characteristics of Compressive Strength and Drying-shrinkage Equation of Alkali-activated Mortar (알칼리 활성화 결합재 모르타르의 압축강도 특성 및 건조수축 추정식에 관한 연구)

  • Park, Kwang-Min;Kim, Hyung-Suk;Cho, Young-Keun
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.21 no.2
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    • pp.114-121
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    • 2017
  • The purpose of this study is to understand a compressive strength and propose a dry shrinkage strain equation being able to predict dry shrinkage of alkali-activated materials(AAM) mortar samples manufactured using fly-ash(FA) and ground granulated blast furnace slag(GGBFS). The main parameters investigated were the GGBFS replace ratios(30, 50, 70 and 100%) and sodium silicate modules(Ms[$SiO_2/Na_2O$] 1.0, 1.5 and 2.0). The compressive strength of AAM increased with increases GGBFS replace ratios or Ms contents. The dry shrinkage strain of AAM decreased with increases Ms contents. But, the dry shrinkage strain of AAM increased as the GGBFS replace ratio increases. Therefore, the GGBFS replace ratio seems to have very significant and important consequences for the mix design of the AAM mortar. The results indicated the R-square of single regression analysis based on each mix properties was the highest value; 0.7539~0.9786(average 0.9359). And the presumption equation of dry shrinkage strain with all variables(GGBFS, Ms and material age) has higher accuracy and its R-square was 0.8020 at initial curing temperature 23 degrees Celsius and 0.8018 at initial curuing temperature 70 degrees Celsius.

Drying Shrinkage Properties of Latex Modified Concrete with Ordinary Cement and Rapid-Setting Cement (초속경 및 일반시멘트를 이용한 라텍스개질 콘크리트의 건조수축 특성)

  • Yun, Kyong-Ku;Jeong, Won-Kyong;Kim, Sung-Hwan;Lee, Joo-Hyung
    • Journal of the Korea Concrete Institute
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    • v.15 no.1
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    • pp.95-101
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    • 2003
  • Drying shrinkage cracking which may be caused by the relatively large specific surface is a matter of grave concern for latex modified concrete(LMC) overlay and rapid-setting cement latex modified concrete(RSLMC) overlay. LMC and RSLMC were studied for field applications very actively in terms of strength and durability in Korea. However, there were no considerations in drying shrinkage. Therefore, the purpose of this dissertation was to study the drying shrinkage properties of LMC and RSLMC with the main experimental variables such as cement types(ordinary portland cement, rapid setting cement), latex contents(0, 5, 10, 15, 20%) and curing days at a same controlled environment of 60% of relative humidity and $20^{\circ}C$ of temperature. The drying shrinkage for specimens was measured with a digital dial gauge of Demec. The test results showed that the drying shrinkage of LMC and RSLMC were considerably lower than that of OPC and RSC, respectively. This might be attributed to the interlocking of hydrated cement and aggregates by a film of latex particles, water retention due to hydrophobic, and colloidal properties of the latexes resulting in reduced water evaporation.

Temperature changes under demineralized dentin during polymerization of three resin-based restorative materials using QTH and LED units

  • Mousavinasab, Sayed-Mostafa;Khoroushi, Maryam;Moharreri, Mohammadreza;Atai, Mohammad
    • Restorative Dentistry and Endodontics
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    • v.39 no.3
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    • pp.155-163
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    • 2014
  • Objectives: Light-curing of resin-based materials (RBMs) increases the pulp chamber temperature, with detrimental effects on the vital pulp. This in vitro study compared the temperature rise under demineralized human tooth dentin during light-curing and the degrees of conversion (DCs) of three different RBMs using quartz tungsten halogen (QTH) and light-emitting diode (LED) units (LCUs). Materials and Methods: Demineralized and non-demineralized dentin disks were prepared from 120 extracted human mandibular molars. The temperature rise under the dentin disks (n = 12) during the light-curing of three RBMs, i.e. an Ormocer-based composite resin (Ceram. X, Dentsply DeTrey), a low-shrinkage silorane-based composite (Filtek P90, 3M ESPE), and a giomer (Beautifil II, Shofu GmbH), was measured with a K-type thermocouple wire. The DCs of the materials were investigated using Fourier transform infrared spectroscopy. Results: The temperature rise under the demineralized dentin disks was higher than that under the non-demineralized dentin disks during the polymerization of all restorative materials (p < 0.05). Filtek P90 induced higher temperature rise during polymerization than Ceram.X and Beautifil II under demineralized dentin (p < 0.05). The temperature rise under demineralized dentin during Filtek P90 polymerization exceeded the threshold value ($5.5^{\circ}C$), with no significant differences between the DCs of the test materials (p > 0.05). Conclusions: Although there were no significant differences in the DCs, the temperature rise under demineralized dentin disks for the silorane-based composite was higher than that for dimethacrylate-based restorative materials, particularly with QTH LCU.

Structural and Property Changes in Glass-like Carbons Formed by Heat Treatment and Addition of Filler

  • Kim, Jangsoon;Kim, Myung-Soo;Hahm, Hyun-Sik;Lim, Yun-Soo
    • Macromolecular Research
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    • v.12 no.4
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    • pp.399-406
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    • 2004
  • Glass-like carbon precursors shrink significantly during curing and carbonization, which leads to crack formation and bending. Cured furan resin powder and ethanol were added to furan resin to diminish the weight loss, to suppress the shrinkage and bending, and to readily release the gases evolved during polymerization and curing. Curing and carbonization were controlled by pressure and slow heating to avoid damage to the samples. The effect of the filler and ethanol on the fabrication process was examined by measuring the properties of the glass-like carbon, such as the specific gravity, bending strength, electrical resistivity, and microstructural change. The specific gravities of the filler-added glass-like carbons were higher than those of the ethanol-added samples because of the formation of macropores from the vaporization of ethanol during the curing and polymerization processes. Although the ethanol-added glass-like carbons exhibited lower bending strengths after carbonization than did the filler-added samples, the opposite result was observed after aging at 2,600$^{\circ}C$. We found that the macropores created from ethanol were contracted and removed upon heat treatment. The electrical resistivity of the glass-like carbon aged at 2,600$^{\circ}C$ was lower than those of the samples carbonized at 1,000$^{\circ}C$. We attribute this phenomenon to the fact that aging at high temperature led to well-developed microstructures, the removal of macropores, and the reduction of the surface area.

Preparation and Characterization of Polyurethane/Organoclay Nanocomposites by UV Curing (UV경화에 의한 폴리우레탄/유기화클레이 나노복합재료 제조와 물성 연구)

  • Shin, Geumsig;Chang, Young-Wook;Kim, Seong Woo
    • Journal of Adhesion and Interface
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    • v.13 no.4
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    • pp.156-162
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    • 2012
  • Polyurethane (PU)/organoclay nanocomposites were prepared by mixing UV curable urethane acrylate oligomer with organoclay, and a subsequent curing by UV irradiation. As organoclays, commercially available Cloisite 20A (C20A) and acrylsilane modified C20A were used. XRD and TEM analyses revealed that the UV cured PU/clay nanocomposites formed intercalated nanocomposites, and acrylsilane modified C20A are dispersed more finely than unmodified C20A in PU matrix. DMTA, pencil hardness and adhesion test onto PET substrate showed that the clay nanolayers induced an increase in the properties, and the enhancement in the properties was more pronounced in the PU/acrylsilane modified C20A nanocomposites than in the PU/unmodified C20A nanocomposites. It was also observed that the PU/surface modified clay nanocomposites showed remarkably lower shrinkage upon UV curing than the unfilled PU. The nanocomposites showed excellent optical transparency but lower gloss as compared to unfilled PU.

COMPARISON OF POLYMERIZATION SHRINKAGE AND STRAIN STRESS OF SEVERAL COMPOSITE RESINS USING STRAIN GUAGE (스트레인 게이지를 이용한 수종의 복합레진의 중합수축 및 수축응력의 비교)

  • Kim, Young-Kwang;Yoo, Seung-Hoon;Kim, Jong-Soo
    • Journal of the korean academy of Pediatric Dentistry
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    • v.31 no.3
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    • pp.516-526
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    • 2004
  • Polymerization shrinkage of photoinitiation type composite resin cause several clinical problems. The purpose of this study was to evaluate the shrinkage strain stress, linear polymerization shrinkage, compressive strength and microhardness of recently developed composite resins. The composite resins were divided into four groups according to the contents of matrix and filler type. Group I : $Denfil^{TM}$(Vericom, Korea) with conventional matrix, Group II : $Charmfil^{(R)}$(Dentkist, Korea) with microfiller and nanofller mixture, Group III : $Filtek^{TM}$ Z250(3M-ESPE, USA) TEGDMA replaced by UDMA and Bis-EMA(6) in the matrix, and Group IV : $Filtek^{TM}$ Supreme(3M-ESPE, USA) using pure nanofiller. Preparation of acrylic molds were followed by filling and curing with light gun. Strain gauges were attached to each sample and the leads were connected to a strainmeter. With strainmeter shrinkage strain stress and linear polymerization shrinkage was measured for 10 minutes. The data detected at 1 minute and 10 minutes were analysed statistically with ONE-way ANOVA test. To evaluate the mechanical properties of tested materials, compressive hardness test and microhardness test were also rendered. The results can be summarized as follows : 1. Filling materials in acrylic molds showed initial temporary expansion in the early phase of polymerization. This was followed by contraction with the rapid increase in strain stress during the first 1 minute and gradually decreased during post-gel shrinkage phase. After 1 minute, there's no statistical differences of strain stress between groups. The highest strain stress was found in group IV and followed by group III, I, II at 10 minutes-measurement(p>.05). In regression analysis of strain stress, group III showed minimal inclination and followed by group II, I, IV during 1 minute. 2. In linear polymerization shrinkage test, the composite resins in every group showed initial increase of shrinkage velocity during the first 1 minute, followed by gradually decrease of shrinkage velocity. After 1 minute, group IV and group III showed statistical difference(p<.05). After 10 minutes, there were statistical differences between group IV and group I, III(p<.05) and between group II and group III(p<.05). In regression analysis of linear polymerization shrinkage, group II showed minimal inclination and followed by group IV, III, I during 1 minute. 3. In compressive strength test, group III showed the highest strength and followed by group II, IV, I. There were statistical differences between group III and group IV, I(p<.05). 4. In microhardness test, upper surfaces showed higher value than lower surfaces in every group(p<.05).

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A Study on the Release Characteristics During Wafer-Level Lens Molding Using Thermosetting Materials (열경화성 소재를 사용한 웨이퍼 레벨 렌즈 성형 중 이형 특성에 관한 연구)

  • Park, Si-Hwan;Hwang, Yeon;Kim, Dai-Geun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.1
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    • pp.461-467
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    • 2021
  • Among the defect factors that can occur when a wafer-level lens is molded using a thermosetting material, the mold sticking problem of a molded lens during the release process can damage the molded substrate and deform the substrate at the wafer level. An experiment was conducted to examine the factors affecting the demolding force in the lens forming process. The demolding force was examined according to the coating material of the molds. The mold was surface-treated with ITO and Ti, followed by plasma treatment in an O2 atmosphere. A DLC coating was then performed, and the curing and releasability were examined. A coating method for the pull-off experiment was selected based on the results. To measure the demolding force according to the curing process conditions, a method of curing at a constant pressure and a method of curing at a constant position were applied. As a result, the TiO2 surface treatment reduced the release force. When cured by controlling the location, curing shrinkage can reduce the adhesion energy of the interface during curing, resulting in better demolding.

A Study on Durability Improvement of Concrete Using Glycol Ether Chemical Admixture (글리콜에테르계 혼화제가 콘크리트의 내구성 향상에 미치는 영향에 관한 연구)

  • Kim, Kwang-Ki;Song, In-Myung;Jung, Sang-Jin
    • Journal of the Korea Institute of Building Construction
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    • v.7 no.4
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    • pp.117-124
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    • 2007
  • Focused on the material-related aspect for enhancing the durability of concrete, the present study analyzed the effect of glycol ether admixture, which is a chemical admixture that can compact the structure of concrete by entraining air inside the concrete, on the basic physical properties and durability characteristic of the concrete. In analyzing the results of experiment, we examined the basic physical properties and durability characteristic of concrete according to addition rate based on OPC and selected the optimal addition rate. In addition, with the optimal addition rate, we added glycol ether admixture to concrete, which contained fly ash used as binder and high-performance water reducing agent for reducing the unit quantity, and examined changes in the characteristics of the concrete. According to the result, the optimal addition rate of glycol ether admixture was 3% of the unit quantity of cement, and the addition of binder and chemical admixture did not have a significant effect on unhardened concrete but reduced the air content. In addition, concrete showed resistance performance of around 30% to carbonation and around 40% to drying shrinkage. In addition, as for resistance to freezing and thawing, the relative dynamic modulus of elasticity was over around 85% through atmospheric curing. These performances prove the effect.