• 공업화학
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• 제27권3호
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• pp.313-318
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• 2016

본 연구에서는 무정형 실리카의 세공 내를 아미노실란인 N-[(3-trimethoxysilyl)propyl]ethylenediamine (2NS)를 이용하여 표면 기능화한 후 표면 기능화된 실리카에 후전이 금속 촉매인 $(DME)NiBr_2$와 $PdCl_2$(COD)를 담지하여 노보넨 중합을 실시하였다. 중합 온도와 중합 시간, Al/Ni 몰비, 조촉매 종류를 변화시켜 중합 특성에 미치는 영향을 조사하였다. 담지되지 않은 촉매($(DME)NiBr_2$, $PdCl_2$(COD))로 노보넨 중합을 수행하였을 경우 중합반응은 일어나지 않았다. 그러나 조촉매로 MAO를 이용하여 중합한 경우 $SiO_2$/2NS/Ni 촉매는 중합 온도가 증가할수록 활성은 증가하였고 폴리노보넨(polynorbornene, PNB)의 분자량은 급격하게 감소하였다. $SiO_2$/2NS/Pd 촉매는 온도가 증가할수록 활성과 PNB의 분자량 모두 감소하는 경향을 보였다. $SiO_2$/2NS/Ni 촉매는 $SiO_2$/2NS/Pd 촉매보다 높은 온도에서 안정함을 확인하였다. 또한 두 촉매 모두 중합 시간이 길어질수록 노보넨의 전환율은 증가하였다. Al/Ni 몰비가 1000 : 1일 때 가장 높은 활성(15.3 kg-PNB/(${\mu}mol-Ni^*hr$))을 보이는 반면 가장 낮은 분자량($M_n$ = 124,000 g/mol)의 PNB를 합성하였다. 또한 조촉매로 Borate/TEAL을 이용하여 중합한 경우 $SiO_2$/2NS/Ni 촉매는 중합 온도가 증가할수록 활성과 분자량이 모두 감소하였다.

• 대한소아치과학회지
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• 제25권2호
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• pp.368-382
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• 1998

The purpose of this study is to evaluate and compare the results of argon laser for 5 seconds, argon laser for 10 seconds, and visible light for 40 seconds photo-polymerization in compressive strength, microhardness, curing depth, temperature rising during polymerization, and polymerization shrinkage. Hybrid type composite resin(Z-100) and compomer(Dyract) were used to be compared. The compressive strength was measured by an Instron(1mm/min cross head speed) in 60 specimens and the microhardness of the surface was expressed by Vickers Hardness Number(VHN) in 30 specimens. The curing depth was evaluated comparing the different values of upper and lower VHN according to irradiation time and thickness for the light source polymerization in 60 specimens. The temperature rising during photopolymerization was observed by the temperature change with thermocouple sensitizer beneath 40 specimens at the argon laser for 10 seconds and visible light 40 seconds irradiation. The polymerization shinkage was evaluated by calculating the decrease of % volume by using a dilatometer in 30 specimens. The results were as follows ; 1. In the case of compressive strength, the argon laser polymerization groups were higher than visible light group in Z-100 (p<0.05). In Dyract, the argon laser 5 seconds group did not show a significant difference with the visible light 40 seconds group. The argon laser 10 seconds group showed the markedly low value when compared with other groups (p<0.05) 2. In microhardness, Z-100 was better than Dyract when comparing by VHNs (p<0.05); however, there was not a significant difference between two materials in the visible light 40 seconds group and the argon laser 10 seconds group. 3. In the study of curing depth, Z-100 showed the consistent polymerization in argon laser irradiation because there was no difference in the VHN decrease according to the thickness change. Over the thickness control, the results did not show a significant difference between visible light and argon laser group in Z-100; however, in the case of Dyract, the visible light 40 seconds group was better than the argon laser groups(p<0.05). 4. There was a significant difference between the two materials in temperature rising during polymerization (p<0.05), but not a significant difference between irradiation times, 5. There was not a significant difference between the two materials in polymerization shrink age. The argon laser 5 seconds group was smaller than the other groups (p<0.05). It could be concluded that Z-100 polymerization was recommended to use the argon laser for reduction of the irradiation time while Dyract was recommended to use the visible light polymerization.

• Elastomers and Composites
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• 제37권1호
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• pp.31-38
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• 2002

카르복실화 스티렌-부타디엔 라텍스의 중합시간은 사용되는 부타디엔 모노머가 공액 이중결합을 가진 화학적 구조로 인하여 라디칼 중합시 홀 전파의 비편재화로 인해 아크릴 에멀젼의 제조시 보다 중합시간이 매우 길다. 또한 라텍스 자체가 고분자와 분산매의 분리 없이 사용되기 때문에 라텍스의 안정성은 대단히 중요하다. 물성의 저하없이 반응시간을 단축하기 위하여 기존에 사용하던 연쇄이동제인 사염화탄소 대신 tert-dodecylmercaptane 과 ${\alpha}$-methylstyrene dimer를 혼합 사용하여 반응시간을 14시간에서 12시간으로 줄일 수 있었다. 반응 성장단계에서 아크릴산의 투입량을 0.3 part로 제한하여 라텍스의 점도 상승을 막고 초기중합단계 직후에 아크릴아미드를 0.1 part 첨가하여 라텍스 입자의 내부영역과 외부영역의 고분자 사슬의 상호간확산을 막아 단단하면서도 접착력을 유지할 수 있는 라텍스의 합성 결과를 얻었다.

• 치위생과학회지
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• 제23권2호
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• pp.123-131
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• 2023

Background: As a restorative material used to treat dental caries, the light-curing type resin is widely used, but it has the disadvantage of polymerization shrinkage. The Bulk-Fill composite resin was developed to solve these shortcomings, but the existing research mainly focused on comparing the physical properties of a composite resin and a Bulk-Fill resin. A study on the light curing time and distance of the Bulk-Fill resin itself tend to be lacking. Methods: This study compares the surface microhardness of specimens prepared by varying the light curing time and distance of smart dentin replacement (SDR) as a flowable Bulk-Fill resin and Tetric N-ceram as a packable Bulk-Fill resin, and confirms the polymerization time and distance that becomes the optimum hardness. To determine the hardness of the specimen, it was measured using the Vickers Hardness Number (Matsuzawa MMT-X, Japan). Results: In SDR, the surface microhardness decreased as the distance increased in all time groups in the change distance from the curing tip. In the change of light curing time with respect to the distance from curing tip, the surface microhardness increased as the time increased. In Tetric N-ceram, the surface microharness showed no significant difference in the change of the distance of curing tip in the group of 20 and 60 second. But in the group of 10 and 40 seconds, decreased as the distance increased. The surface microharness increased as the light curing time increased in all distance groups. Conclusion: When using SDR and Tetric N-ceram in clinical practice, it is considered that as the distance from the polymerization reactor tip increases, a longer light curing time than the polymerization time recommended by the manufacturer is required.

• 한국세라믹학회지
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• 제55권2호
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• pp.126-134
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• 2018

Using aqueous solution free radical polymerization with glacial acrylic acid (GAA), maleic anhydride (MA) and sodium methallyl disulfonate (SMADS), a novel linear polycarboxylate dispersant was synthesized for ceramics. Dispersant linear structural characterization was done by FTIR, $^1H$ NMR, HPLC and GPC, and the ratio of monomers was determined using an orthogonal experiment. This research is focused on the effects of polymerization temperature, monomer mole ratios and dosage of initiator on ceramic slurry viscosity with linear polycarboxylate dispersant for ceramic dosage rate of 0.30% (based on dry slurry), all of which were investigated by single factor test. The best polymerization conditions for linear GAA-MA-SMADS are when n(AA) : n(MA) : n(SMADS) equals 3.0 : 1.0 : 0.5, the molecular weight of the polymer is 4600 daltons, the initiator sodium persulfate accounts for 7% of the total mass of polymerized monomers, the polymerization temperature is $90^{\circ}C$ and the reaction time is 2 h. The ceramic body slurry viscosity drops from $820mPa{\cdot}s$ to $46mPa{\cdot}s$ when the concentration of the polycarboxylate dispersant is 0.30%.

• Bulletin of the Korean Chemical Society
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• 제33권7호
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• pp.2345-2351
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• 2012

Conductive honeycomb-patterned polystyrene (PS) thin films were prepared by the formation of a polyaniline (PANI) thin layer on the surface of the patterned PS thin films using simple one-step chemical oxidative polymerization of aniline. The in situ chemical oxidation polymerization of aniline hydrochloride solution on the patterned structure of the PS films was conducted in the presence of multiwalled carbon nanotubes (MWCNT) to prepare the PANI-MWCNT/PS composite film. The concentration (wt %) of MWCNT was varied in the range of 1%-3% by weight. The dependence of surface morphology of the PANI/PS and PANI-MWCNT/PS composite film to the polymerization time was observed by scanning electron microscopy. The room temperature DC conductivity was obtained by the four-probe technique. The conductivity of the PANI-MWCNT/PS composite film was affected both by the MWCNT concentration and polymerization time. In addition, DC electrical field was loaded during the oxidative polymerization to affect the distribution of the MWCNT included in the composite film, varying the loading voltage in the range of 0.1-3.0 V. The conductivity of the PANI-MWCNT/PS composite film was increased as loading voltage rose. However, this increase stops at a voltage higher than the critical value.

• 한국재료학회지
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• 제28권12호
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• pp.685-690
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• 2018

In this study, a multifunctional ophthalmic lens material with an electromagnetic shielding effect, high oxygen permeability, and high water content is tested, and its applicability is evaluated. Metal oxide nanoparticles are applied to the ophthalmic lens material for vision correction to shield harmful electromagnetic waves; the pyridine group is used to improve the antibacterial effect; and silicone substituted with urethane and acrylate is employed to increase the oxygen permeability and water content. In addition, multifunctional tinted ophthalmic lens materials are studied using lens materials with an excellent antibacterial effect (2,6-difluoropyridine, 2-fluoro-4-pyridinecarboxylic acid) and functional (UV protection, high wettability) lens materials (2,4-dihydroxy benzophenone, 2-hydroxy-4-(methacryloyloxy)benzophenone). To solve problems such as air bubbles generated during the polymerization process for the manufacturing and turbidity of the lens surface, polymerization conditions in which the defect rate is minimized are determined. The results show that the polymerization temperature and time are most appropriate when they are $110^{\circ}C$ and 40 minutes, respectively. The optimum injection amount of the polymerization solution is 350 ms. The turbid phenomenon that appears in lens processing is improved by 10 to 95 % according to the test time and conditions.

• 대한치과보철학회지
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• 제45권6호
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• pp.735-742
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• 2007

Statement of problem. Although a number of previous investigations have been carried out on the polymerization shrinkage-strain kinetics of provisional crown and fixed partial denture (FPD) materials, the effect of the changes of liquid monomer to powder ratio on its polymerization shrinkage-strain kinetics has not been reported. Purpose. The purpose of this study was to investigate the influence of liquid monomer to powder ratio of polymer-based provisional crown and FPD materials on the polymerization shrinkage-strain kinetics. Material and methods. Chemically activated acrylic provisional materials (Alike, Jet, Snap) were investigated. Each material was mixed with different liquid monomer to powder ratios by volume (1.0:3.0, 1.0:2.5, 1.0:2.0, 1.0:1.5, 1.0:1.0). Time dependent polymerization shrinkage- strain kinetics of all materials was measured by the bonded-disk method as a function of time at $23^{\circ}C$. Five recordings were taken for each ratio. The results were statistically analyzed using one-way ANOVA and the multiple comparison Scheffe test at the significance level of 0.05. Trends were also examined by linear regression. Results. At 5 minutes after mixing, the polymerization shrinkage-strains of all materials ranged from only 0.01% to 0.49%. At 10 minutes, the shrinkage-strain of Alike was the highest, 3.45% (liquid monomer to powder ratio=1.0:3.0). Jet and Snap were 2.69% (1.0:2.0) and 1.58% (1.0:3.0), respectively (P>0.05). Most shrinkage (94.3%-96.5%) occurred at 30 minutes after mixing for liquid monomer to powder ratio, ranging from 1.0:3.0 to 1.0:1.0. The highest polymerization shrinkage-strain values were observed for the liquid monomer to powder ratio of 1.0:3.0. At 120 minutes after mixing, the shrinkage-strain values were 4.67%, 4.18%, and 3.07% for Jet, Alike, and Snap, respectively. As the liquid monomer to powder ratio increased, the shrinkage-strain values tend to be decreased linearly (r=-0.769 for Alike, -0.717 for Jet, -0.435 for Snap, $r^2=0.592$ for Alike, 0.515 for Jet, 0.189 for Snap; P<0.05). Conclusion. The increase of the liquid monomer to powder ratio from 1.0:3.0 to 1.0:1.0 had a significant effect on the shrinkage-strain kinetics of polymer-based crown and FPD materials investigated. This increased the working time and decreased the shrinkage-strain during polymerization.

• 제어로봇시스템학회:학술대회논문집
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• 제어로봇시스템학회 1996년도 Proceedings of the Korea Automatic Control Conference, 11th (KACC); Pohang, Korea; 24-26 Oct. 1996
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• pp.263-266
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• 1996

A method to determine an optimal temperature trajectory that guarantees polymer products having controlled molecular weight distribution and desired values of molecular weight is presented. The coordinate transformation method and the optimal control theory are applied to a batch PMMA polymerization system to calculate the optimal temperature trajectory. Coordinate transformation method converts the original fixed-end-point, free-end-time problem to a free-end-point, fixed-end-time problem. The idea is that by making the reactor temperature track the optimal temperature trajectory one may be able to produce polymer products having the prespecified physical property in a minimum time. The on-line control experiments with the PID control algorithm have been conducted to establish the validity of the scheme proposed in this study. The experimental results show that prespecified polymer product could be obtained with tracking the calculated optimal temperature trajectory.

• Macromolecular Research
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• 제11권5호
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• pp.311-316
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• 2003

The kinetics of photoinitiated polymerization of dimethacrylate macromonomers have been studied to determine the diffusion-controlled reaction parameters using attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). A predicted kinetic rate expression with a diffusion control factor was employed to estimate an effective rate constant and to define the reaction-controlled and diffusion-controlled regimes in the photopolymerization. An effective rate constant, k$_{e}$, can be obtained from the predicted kinetic rate expression. At the earlier stages of polymerization, the average values of kinetic rate constants do not vary during the reaction time. As the reaction conversion, $\alpha$, reaches the critical conversion, $\alpha$$_{c}$, in the predicted kinetic expression, the reaction becomes to be controlled by diffusion due to the restricted mobility of dimethacrylate macromonomers. A drop in value of effective rate constant causes a drastic decrease of reaction rate at the later stages of polymerization. By determining the effective rate constants, the reaction-controlled and diffusion-controlled regimes were properly defined even in the photopolymerization reaction system.m.m.