• Polymer(Korea)
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• v.34 no.1
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• pp.69-73
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• 2010

Effects of reaction time and temperature on the isomerization and dehydrobromination reactions of brominated butyl rubber were investigated. The structural composition of brominated butyl rubber was determined by Fourier transform infrared spectroscopy (FT-IR) and proton nuclear magnetic resonance spectroscopy($^1H$-NMR), Density functional theory (DFT) was used to study on the isomerization and dehydrobromination mechanisms of model compounds. The geometries for model compounds of 3-bromo-5,5,7,7-tetramethyl-2(2',2',4',4'-tetramethyl)pentyl-1-octylene (3BrOE), 1-bromo-5,5,7,7-tetramethyl-2(2',2',4',4'-tetramethyl)pentyl-2-octylene (1Br2OE) and 5,5,7,7-tetramethyl-2(2',2', 4',4'-tetramethyl)pentyl-1,3-octadiene (CD) had been optimized by using density functional theory at B3LYP/3-21G and B3LYP/6-31G levels. The predicted energy of 3BrOE lies higher than that of 1Br2OE which suggests that 1Br2OE configuration is more stable than the 3BrOE configuration. Compared with the energy barrier, the pathway of dehydrobromination is less competitive than that of isomerization. This is qualitatively consistent with the experimental results.

• Tribology and Lubricants
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• v.30 no.4
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• pp.224-233
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• 2014

We prepared polyester-polyamines to improve the effect of carbon black dispersibility for use in thermal transfer ink, and synthesized polymeric dispersing agents by two-step reactions. In the first step, we made polyester by polycondensing 1,6-hexanediol and adipic acid. The resulting polymers had carboxylic acid, which was linked with polyamine via an acid-base reaction. We then characterized the polyester-polyamine structure by NMR spectroscopy and Fourier transform infrared spectroscopy (FT-IR). We also determined the basic characterizations such as total acid numbers (TAN) (5.0-67.5 mgKOH/g), hydroxyl values (27.1-67.5 mgKOH/g), and molar masses ($M_n=1.6-8.4kg\;mol^{-1}$) for the polyester and total base numbers (TBN) (15.3-57.1 mgKOH/g), hydroxyl values (33.0-79.8 mgKOH/g), and nitrogen contents (1.02-3.48%) for the polyester-polyamine polymers. We thus prepared thermal transfer ink using carbon blacks and the polyester-polyamine dispersing agents, and evaluated the resulting mixtures for printability, adhesive force, storage stability, ink appearance, ink gloss, and processability. These mixtures showed significant dispersibility for carbon black in the ink. Thus, we concluded that the dispersibility of the polymeric materials depended on the polyamine structure and the hydrophilicity-hydrophobicity distribution of the polymeric dispersants.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.204-204
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• 1999

The plasma source ion implantation(PSII) technique which is a method using high negative voltage pulse in plasma system has the potential to change the surface properties of polymer. PSII technique increase the surface free energy by introducing polar functional groups on the surface so that it improves reactivity, hydrophilicity, adhension, biocompatability, etc. However, the mobility of polymer chains enables the modified surface layers to adapt their composition to interfacial force. This hydrophobic recovery interrupts the stability of modified surfaces to keep for the long time. In this study, poly(methyl methacrylate)(PMMA), poly(2-hydroxyethyl methacrylate)(PHEMA), and polu(2-hydroxypropyl methacylate)(PHPMA) for contact lens application, were modified to improve the wettability with PSII technique and were investigated the surface stabilities. Polymer film was prepared with solution casting(3 wt.% solution) and was annealed at 11$0^{\circ}C$ under vacuum oven to remove solvent completely and to eliminate physical ageing. The thickness of the film measured by scanning electron microscopy (SEM) and surface profilometer was about 10${\mu}{\textrm}{m}$. Polymers were treated with different kinds of gases, pulse frequency, pulse with, pulse voltage, and treatment time. Even though PMMA, PHEMA, and PHPMA have similar repeat unit structure, the optimal treatment conditions and the tendency to hydrophobic recovery were different. PHPMA, more hydrophilic polymer than PMMA and PHEMA showd better wettability and stability after mild treatment. Surface tensions were obtained by water and diiodomethane contact angle measurements to monitor the relation between hydrophobic recovery and polymer structure. Different ion species in plasma change the polar component and dispersion component of polymer surface. For better wettability surface, the increase of polar component was a dominant factor. We also characterized modified polymer surfaces using x-ray photoelectron spectroscopy(XPS), secondary ion mass spectrometry(SIMS), Fourier Transform infrared spectroscopy(FT-IR), and SEM.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.275.2-275.2
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• 2014

현재 자동차 분야에서 차량 경량화의 한 수단으로 자동차용 유리를 고강도 투명 플라스틱 소재인 Polycarbonate(PC)로 대체하고자 하는 연구가 이루어지고 있다. 하지만, PC의 낮은 내마모 특성과 자외선에 의한 열화 및 변색 현상은 해결하여야 할 문제점으로 지적되고 있으며, 에너지 소비 저감을 위하여 적외선 영역 반사율(reflectance)이 높은 저방사(low emissivity) 특성이 요구되고 있다. 본 연구에서는, ICP-assisted reactive magnetron sputtering 장비를 이용하여 투과율(transmittance)이 확보되고, 고경도 특성을 갖는 Al-Si-N와 300 nm 파장 이하의 자외선 차단 특성이 있는 SiN:H 그리고 저방사 특성을 위해 Al을 증착하였고, 박막의 증착 순서는 SiN:H 박막을 가장 아래에 증착하고 그 위에 Al/Al-Si-N 박막을 다층으로 형성하였다. 박막의 chemical state와 crystallinity를 확인하기 위하여 XPS(X-ray Photoelectron Spectroscopy), XRD (X-ray Diffraction)를 이용하여 분석하였다. Knoop ${\mu}$-hardness tester와 Taber tester를 이용하여 경도 및 내마모 특성을 분석하였다. 제작된 샘플의 Al-Si-N 박막 경도는 Si 비율에 따라 다른 경도 특성을 갖는데, 실제 Si/(Al+Si) 비율이 24%에서 최대 31 GPa의 경도 값을 갖는 것을 확인하였다. UV-Vis Spectrometer를 이용하여 250 nm~700 nm 파장의 투과율을 측정하였고, 자외선 영역의 경우 SiN:H 박막에 의해 300 nm 이하의 파장에서 2% 이하의 투과율을 확인하였다. 그리고 FT-IR(Fourier Transform Infrared Spectroscopy)를 이용하여 $2.5{\mu}m{\sim}15{\mu}m$ 파장의 반사율을 이용하여 방사율을 측정하였는데, 3*(Al/Al-Si-N) 구조의 다층 박막의 경우 방사율은 0.27로 측정되었다.

• Korean Journal of Materials Research
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• v.26 no.1
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• pp.47-53
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• 2016

Silicon nitride ($SiN_x:H$) films made by plasma enhanced chemical vapor deposition (PECVD) are generally used as antireflection layers and passivation layers on solar cells. In this study, we investigated the properties of silicon nitride ($SiN_x:H$) films made by PECVD. The passivation properties of $SiN_x:H$ are focused on by making the antireflection properties identical. To make equivalent optical properties of silicon nitride films, the refractive index and thickness of the films are fixed at 2.0 and 90 nm, respectively. This limit makes it easier to evaluate silicon nitride film as a passivation layer in realistic application situations. Next, the effects of the mixture ratio of the process gases with silane ($SiH_4$) and ammonia ($NH_3$) on the passivation qualities of silicon nitride film are evaluated. The absorption coefficient of each film was evaluated by spectrometric ellipsometry, the minority carrier lifetimes were evaluated by quasi-steady-state photo-conductance (QSSPC) measurement. The optical properties were obtained using a UV-visible spectrophotometer. The interface properties were determined by capacitance-voltage (C-V) measurement and the film components were identified by Fourier transform infrared spectroscopy (FT-IR) and Rutherford backscattering spectroscopy detection (RBS) - elastic recoil detection (ERD). In hydrogen passivation, gas ratios of 1:1 and 1:3 show the best surface passivation property among the samples.

• Korean Journal of Materials Research
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• v.9 no.8
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• pp.825-830
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• 1999

Characteristics of SiOF films deposited by a FTES/$O_2$-plasma enhanced chemical vapor deposition method have been investigated using Fourier transform infrared spectroscopy, X-ray photoelectro spectroscopy, and ellipsometry. Electrical properties such as dielectric constant, dielectric breakdown and leakage current density are investigated using C-V and I-V measurements with MIS(Au/SiOF/p-Si) capacitor structure. Stepcoverage of the films have been also characterized using scanning electron microscopy and ellipsometry. A high quality SiOF film was formed on that the flow rates of FTES and $O_2$were 300sccm, respectively. The dielectric constant of the deposited SiOF film was about 3.1. This value is lower than that of the oxide films obtained using other method. The dielectric breakdown field and leakage current are more than 10MV/cm and about $8[\times}10^{9}A/\textrm{cm}^2$, respectively. The deposited SiOF film with thickness as $2500{\AA}$ on the $0.3{\mu}{\textrm}{m}$ metal pattern shows a high step-coverage without a void.

• Microbiology and Biotechnology Letters
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• v.41 no.1
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• pp.60-69
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• 2013

Purified melanin pigment from Klebsiella sp. GSK was characterized by thermogravimetric, differential thermal, X-ray diffraction and elemental analysis. This melanin pigment is structurally amorphous in nature. It is thermally stable up to $300^{\circ}C$ and emits a strong exothermic peak at $700^{\circ}C$. Its carbon, hydrogen and nitrogen composition is 47.9%, 6.9% and 12.0%, respectively. It was used to scavenge metal ions and free radicals. After immobilizing the pigment and using it to adsorb copper and lead ions, the metal ion adsorption capacity was evaluated by atomic absorption spectroscopy (AAS) and the identity of melanin functional groups involved in the binding of metal ions was determined by Fourier transform infrared (FT-IR) spectroscopy. Batch adsorption studies showed that 169 mg/g of copper and 280 mg/g of lead were adsorbed onto melanin-alginate beads. The metal ion adsorption capacity of the melanin-alginate beads was relatively significant compared to alginate beads. The metal ion desorption capacity of HCl was greater (81.5% and 99% for copper and lead, respectively) than that of EDTA (80% and 71% for copper and lead, respectively). The ability of the melanin pigment to scavenge free radicals was evaluated by inhibition of the oxidation of 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and was shown to be about 74% and 98%, respectively, compared with standard antioxidants.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.170-170
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• 2011

태양전지와 박막 트랜지스터를 위한 유망한 재료로서 수소화된 비정질 실리콘과 나노결정 실리콘 박막이 관심을 받아 왔다. 특히, 수소화된 나노결정 실리콘 박막은 비정질 대비 높은 방향성과 조밀한 구조 덕에 박막 태양전지나 TFT(Thin film transistor) 소자의 성능 향상에 기여할 수 있는 물질로 연구되고 있다. 이러한 박막들은 보통 $SiH_4$같은 Si을 포함한 가스에 다량의 $H_2$를 희석시켜 플라즈마 화학 증착법(PECVD, Plasma Enhanced Chemical Vapor Deposition)에 의해 성장된다. 이러한 CVD증착 방식을 이용하여 결정화된 박막을 얻기 위해서는 대개 높은 수소 희석비를 이용하는 것이 일반적이나, 이러한 공정 방식은 실리콘이 결합되어야 할 결합위치에 bonding energy가 더 높은 수소의 결합을 촉진하게 된다. 이러한 특성은 박막 태양전지에서 효율을 떨어뜨리는 주요 요소로 작용하고 있다.(1) 본 연구에서는 수소의 결합 확률을 낮춘 결정화된 박막을 성장시키기 위해 수소를 대신하여 헬륨을 희석가스로 사용하여 박막을 증착하고 그 특성을 분석해 보았다. 박막의 구조적 특성, 결정화도(Xc), 플라즈마 내 활성 라디칼(Active radical in plasma), Si-H결합 특성, 전도도(Conductivity)와 같은 박막 특성을 알아보기 위해 주사전자현미경(SEM, Scanning Electron Microscopy), 라만 분광기(Raman spectroscopy), 광 방출 분광기(OES, Optical Emission Spectrocopy), 적외선 분광기(FT-IR, Fourier Transform-Infrared Spectroscopy), Keithley measurement kit이 사용되었다. 수소를 대신하여 헬륨을 사용함으로써 동일 결정화도 대비 10%이상 낮은 microstructure factor 값을 얻을 수 있었으며 인가되는 RF 전력을 140W까지 증가시켰을 때 약 80%의 결정화도를 관찰할 수 있었다.

• Macromolecular Research
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• v.16 no.8
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• pp.704-710
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• 2008

Injectable hydrogels are quite promising materials due to their potential to minimize invasive implantation and this provides versatile fitness irrespective of the damaged regions and facilitates the incorporation of bioactive agents or cells. In situ gel formation through stereocomplex formation is a promising candidate for injectable hydrogels. In this paper, a new series of enantiomeric, four-arm, PEG-PLA block copolymers and their stereocomplexed hydrogels were prepared by bulk ring-opening polymerization of D-lactide and L-lactide, respectively, with stannous octoate as a catalyst. The prepared polymers were characterized by $^1H$ nuclear magnetic resonance (NMR) spectroscopy, Fourier-transform infrared (FT IR) spectroscopy, gel permeation chromatography (GPC) and thermal gravitational analysis (TGA), confirming the tailored structure and chain lengths. The swelling and degradation behavior of the hydrogels formed from a selected copolymer series were observed in different concentrations. The degradation rate decreased with increasing polymer content in the solution. The rheological behavior indicated that the prepared hydrogel underwent in situ gelation and had favorable mechanical strength. In addition, its feasibility as an injectable scaffold was evaluated using a media dependence test for cell culture. A Tris solution was more favorable for in situ gel formation than PBS and DMEM solutions were. These results demonstrated the in situ formation of hydrogel through the construction of a stereocomplex with enantiomeric, 4-arm, PEG-PLA copolymers. Overall, enantiomeric, 4-arm, PEG-PLA copolymers are a new species of stereocomplexed hydrogels that are suitable for further research into injectable hydrogels.

• Journal of the Korean Chemical Society
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• v.59 no.2
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• pp.142-147
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• 2015

Two new chitosan derivatives, polyamine grafted chitosan copolymers have been synthesized for corrosion protection of carbon steel in acidic medium. First, methyl acrylate graft chitosan copolymer (CS-MAA) was prepared by the reaction of chitosan (CS) and methyl acrylate (MAA) via the Michael addition reaction. Then, CS-MAA was reacted with ethylene diamine (EN) and triethylene tetramine (TN) respectively to synthesize ethylene diamine grafted chitosan copolymer (CS-MAA-EN) and triethylene tetramine grafted chitosan copolymer (CS-MAA-TN), and the structures were characterized by Fourier-transform infrared spectroscopy (FT-IR). At last, the corrosion inhibition activities on Q235 carbon steel were investigated by using gravimetric measurements, metallographic microscope, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) measurements. The compounds CS-MAA-EN and CS-MAA-TN show an appreciable corrosion inhibition property against corrosion of Q235 carbon steel in 5% HCl solution at $25^{\circ}C$. It has been observed that CS-MAA-EN shows greater corrosion inhibition efficiency than CS-MAA-TN. The inhibition efficiency of CS-MAA-EN was close to 90% when the mass fraction concentration was 0.2%~0.3%; the inhibition efficiency of CS-MAA-TN was close to 85% when the mass fraction concentration was 0.02%. The present work provided very promising results in the preparation of green corrosion inhibitors.