• Title/Summary/Keyword: Thermal reaction

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Preparation and Characterization of Fluorenyl Polymer Electrolyte Membranes Containing PFCB Groups (PFCB Group을 포함한 Fluorene계 고분자 전해질막 제조 및 특성연구)

  • Kim Jeong-Hoon;Kim Dong-Jin;Chang Bong-Jun;Shin Chong-Kyu;Lee Soo-Bok;Joo Hyeok-Jong
    • Membrane Journal
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    • v.16 no.1
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    • pp.16-24
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    • 2006
  • We report on the preparation and characterization of sulfonated polymer membranes containing perfluorocyclobutane (PFCB) units and fluorene units. The polymers were prepared through three synthetic steps, that is, the synthesis of a trifluorovinylether-terminated monomer, its thermal polymerization, and post-sulfonation using chlorosulfonic acid. A series of sulfonated polymers with different ion exchange capacity (IEC) were prepared by changing the content of chlorosulfonic acid during the post-sulfonation reaction. All the synthesized compounds were characterized by FT-IR, $^{1}H-NMR,\;^{19}F-NMR$, and Mass spectroscopy. As the content of chlorosulfonic acid increased, the SD, IEC, water uptake, and ion conductivity of the sulfonated polymer membranes increased. The sulfonated polymer 4 showed higher values of ion conductivity than the Nafion-$115^{\circledR}$ in a wide range of temperatures ($25{\sim}80^{\circ}C$).

Solid-phase PEGylation for Site-Specific Modification of Recombinant Interferon ${\alpha}$-2a : Process Performance, Characterization, and In-vitro Bioactivity (재조합 인터페론 알파-2a의 부위 특이적 수식을 위한 고체상 PEGylation : 공정 성능, 특성화 및 생물학적 활성)

  • Lee, Byung-Kook;Kwon, Jin-Sook;Lee, E.K.
    • KSBB Journal
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    • v.21 no.2
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    • pp.133-139
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    • 2006
  • In 'solid-phase' PEGylation, the conjugation reaction occurs as the proteins are attached to a solid matrix, and thus it can have distinct advantages over the conventional, solution-phase process. We report a case study: rhIFN-${\alpha}$-2a was first adsorbed to cation exchange resin and then N-terminally PEGylated by aldehyde mPEG of 5, 10, and 20 kD through reductive alkylation. After the PEGylation, salt gradient elution efficiently recovered the mono-PEGylate in a purified form from the unwanted species such as unmodified IFN, unreacted PEG, and others. The mono-PEGylation and its purification were integrated in a single chromatographic step. Depending on the molecular weight of the mPEG aldehyde used, the mono-PEGylation yield ranged 50-64%. We could overcome the major problems of random, or uncontrollable, multi-PEGylation and the post-PEGylation purification difficulties associated with the solution-phase process. N-terminal sequencing and MALDI-TOF MS confirmed that a PEG molecule was conjugated only to the N-terminus. Compared with the unmodified IFN, the mono-PEGylate showed the reduced anti-viral activity as measured by the cell proliferation assay. The bioactivity was reduced more as the higher molecular weight PEG was conjugated. Immunoreactivity, evaluated indirectly by antibody binding activity using a surface plasmon resonance biosensor, also decreased. Nevertheless, trypsin resistance as well as thermal stability was considerably improved.

Effect of h-BN Content on Microstructure and Mechanical Properties of AIN Ceramics (AIN 세라믹스의 미세조직과 기계적 성질에 미치는 h-BN 첨가의 영향)

  • 이영환;김준규;조원승;조명우;이은상;이재형
    • Journal of the Korean Ceramic Society
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    • v.40 no.9
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    • pp.874-880
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    • 2003
  • The effect of h-BN content on microstructure, mechanical properties, and machinability of AlN-BN based machinable ceramics were investigated. The relative density of sintered compact decreased with increasing h-BN content. The four-point flexural strength also decreased from 238 MPa of monolith up to 182 MPa by the addition of 30 vol% h-BN. Both low Young's modulus and residual tensile stress, formed by the thermal expansion coefficient difference between AIN and h-BN, might cause the strength drop in AlN-BN composite. The crack deflection, and pull-out phenomena increased by the plate-like h-BN. However, the fracture toughness decreased with h-BN content. The second phases, consisted of YAG and ${\gamma}$-Al$_2$O$_3$, were formed by the reaction between Al$_2$O$_3$ and Y$_2$O$_3$. During end-milling process, feed and thrust forces measured for AlN-(10~30) vol% BN composites decreased with increasing h-BN particles, showing excellent machinability. Also, irrespective of h-BN content, relatively good surfaces with roughness less than 0.5 m (Ra) could be achieved within short lapping time.

Thermal Characteristics of Waste Organic Sludges Discharged from an Chemical Product Manufacturing Industry (화학제품제조업에서 배출되는 폐 유기성슬러지의 열적 특성)

  • Kim, Min-Choul;Lee, Gang-Woo;Lee, Man-Sig;Shon, Byung-Hyun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.6
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    • pp.1745-1753
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    • 2008
  • We analyzed the physical and chemical properties such as proximate analysis, ultimate analysis, heating values, thermogravimetric analysis, and combustion test for the organic sludge discharged from chemical and petrochemical product manufacturing industries in the industrial complex. The average combustible and ash content of organic sludges from chemical and petrochemical product manufacturing industries were 17.42%, 7.45%, and 18.25%, 4.22%, respectively. The C, H, O, N, and S compositions for chemical and petrochemical product manufacturing industries were 33.06, 4.34, 24.81, 5.18, and 0.72%. And those compositions for petrochemical product manufacturing industries were 36.58, 4.74, 26.79, 5.09, and 0.49%, respectively. From the TGA test, the minimum temperature for combustion of the sludge discharged from B company was $700^{\circ}C$ for direct use for energy and 2 sludges(F and N companies) were about $600^{\circ}C$. According to the basic combustion test, high concentration of CO was formed because oxidation and pyrolysis reaction take place in the batch type reactor at the same time. From this phenomena we could obtain the significant data for the overheating and breakage of furnace.

Early-Age Deformation of Very-Early Strength Latex- Modified Concrete with Ultra-Fine Fly Ash Contents (울트라파인 플라이 애시 혼입률에 따른 VES-LMC의 초기거동 특성)

  • Choi, Pan-Gil;Park, Won-Il;Yun, Kyong-Ku;Lee, Bong-Hak
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.11 no.3
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    • pp.1040-1046
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    • 2010
  • The main disadvantage of rapid setting concrete is the occurrence of cracking because of fast hydration reaction due to high thermal expansion and shrinkage. However, if the fly ash is used in concrete, it is possible to prevent cracking since the hydration heat can be decreased. Although Very-Early Strength-Latex Modified Concrete(VES-LMC) is an excellent material, occurrence of cracking has been reported because of high hydration heat. In the present study, new method which can apply the fly ash to the VES-LMC was developed. Research for the new method to improve the safety for the cracking was conducted. Safety was confirmed by reducing the shrinkage and hydration heat in the condition of overcoming the low early-age strength. Detailed conclusions are follows. Early-age compressive strength was decreased a little with increase of UFFA content. However, 28-d compressive strength was statistically insignificant regardless of UFFA contents. If the UFFA is replaced 15% to 20% of unit cement weight in concrete, maximum shrinkage can be reduced up to 43% to 47%. Usage of UFFA in VES-LMC guarantees the safety for cracking since it is very effective to control of early-age shrinkage.

Study on the Improved Abrasion Resistance of Polycarbonate Substrate by UV-curable Organic/Inorganic Hybrid Coatings (자외선 경화형 유기/무기 복합코팅에 의한 폴리카보네이트의 내마모성 향상 연구)

  • 윤석은;우희권;김동표
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.389-398
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    • 2000
  • Transparent, abrasion resistant coatings with 4~13 ${\mu}{\textrm}{m}$ thickness were prepared by spin-coating on polycarbonates with organic/inorganic hybrid solutions, followed by UV curing and heat treatment at 12$0^{\circ}C$ for 12 hours. The coating solutions were composed of inorganic phase and organic phase in 0:100, 20:80, 30:70, 50:50, 80:20 wt% ratios, respectively, mixed with photoinitiator, senaitizer and surfactant. The inorganic phase was formed by sol-gel reaction of TEOS and silane coupling agent MPTMS in 1 : 2 or 2 : 1 molar ratios, the organic phase consisted of difunctional urethane acrylate oligomeric resin, multifunctional acrylate TMPTA and HDDA in 4 : 3 : 3 wt% ratio. The coating systems were investigated by FT-IR, $^{29}$ Si-NMR spectra. In addition, TGA/DSC for thermal analysis and SEM, AFM observation for coated surface were examined. Gererally, the homogeneity of phases, the surface smoothness of coating and abrasion resistance were improved with the higher content of inorganic component. Namely, coating system with below 10 $\AA$ surface roughness and T$_{g}$ of 15$0^{\circ}C$ showed only 10% decrease in light transmittance after abrasion test, whereas uncoated polycarbonate substrate exhibited 46% decrease..

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Effects of Crosslinking Agent and Flame Retardant on the Dielectric Properties of Poly(phenylene ether)-based Polymer Substrate Material (폴리페닐렌에테르계 고분자 기판 소재의 유전특성에 대한 가교제 및 난연제의 영향)

  • Kim, Dong-Kook;Park, Seong-Dae;Yoo, Myong-Jae;Lee, Woo-Sung;Kang, Nam-Kee;Lim, Jin-Kyu;Kyoung, Jin-Bum
    • Polymer(Korea)
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    • v.33 no.1
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    • pp.39-44
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    • 2009
  • Polymer substrates were fabricated by using poly (phenylene ether) as a base resin, N,N'-m-phenylenedimaleimide (PDMI) as a crosslinking agent and decabromodiphenylethane as a flame retardant. The effects of crosslinking agent and flame retardant on physical properties such as dielectric property of the substrate were investigated. Thermal curing feature of PDMI with or without an initiator was analyzed by DSC, and then, PPE-PDMI test compositions were designed based on this result. Composite sheets were cast by film coater, laminated under vacuum and pressure, and then, the changes of dielectric constant, dielectric loss, peel strength, solder heat resistance and inflammability according to increasing amount of PDMI and flame retardant were evaluated, Dielectric constant and dielectric loss showed increasing trend with increasing amount of PDMI and flame retardant, but solder heat resistance and inflammability were improved. Peel strength was obtained higher than 1 kN/m when PDMI above 10 wt% was added, but slightly decreased as the amount of flame retardant increased. From the measured gel contents, the reaction mechanism of PPE-PDMI system was deduced to the formation of network structure by crosslinking PDMI with PPE rather than the formation of semi-IPN structure. In conclusion, the polymer composite substrate materials with dielectric constant of 2.52$\sim$2.65 and dielectric loss below 0.002 at 1 GHz were obtained and they will be proper for high frequency applications.

CuO Nanograss as a Substrate for Surface Enhanced Raman Spectroscopy

  • Lee, Jun-Young;Park, Jiyun;Kim, Jeong-Hyun;Yeo, Jong-Souk
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.249-249
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    • 2013
  • Surface-enhanced Raman spectroscopy (SERS) is a sensitive approach to detect and to identify a variety of molecules. To enhance the Raman signal, optimization of the gap between nanostructures is quite important. One-dimensional materials such as nanowires, nanotubes, and nanograsses have great potential to be used in SERS due to their unique sizes and shape dependent characteristics. In this study we investigate a simple way to fabricate SERS substrates based on randomly grown copper oxide (CuO) nanowires. CuO nanograss is fabricated on pre-cleaned Cu foils. Cu oxidized in an ammonium ambient solution of 2.5 M NaOH and 0.1 M $(NH_4)_2S_2O_8$ at $4^{\circ}C$ for 10, 30, and 60 minutes. Then, Cu(OH)2 nanostructures are formed and dried at $180^{\circ}C$ for 2 h. With the drying process, the Cu(OH)2 nanostructure is transformed to CuO nanograss by dehydration reaction. CuO nanograss are grown randomly on Cu foil with the average length of 10 ${\mu}m$ and the average diameter of a 100 nm. CuO nanograsses are covered by Ag with various thicknesses from 10 to 30 nm using a thermal evaporator. Then, we immerse uncoated and Ag coated CuO nanowire samples of various oxidation times in a 0.001M methanol-based 4-mercaptopyridine (4-Mpy) in order to evaluate SERS enhancement. Raman shift and SERS enhancement are measured using a Raman spectrometer (Horiba, LabRAM ARAMIS Spectrometer) with the laser wavelength of 532 nm. Raman scattering is believed to be enhanced by the interaction between CuO nanograss and Ag island film. The gaps between Ag covered CuO nanograsses are diverse from <10 nm at the bottom to ~200 nm at the top of nanograsses. SERS signal are improved where the gaps are minimized to near 10s of nanometers. There are many spots that provide sufficiently narrow gap between the structures on randomly grown CuO nanograss surface. Then we may find optimal enhancement of Raman signal using the mapping data of average results. Fabrication of CuO nanograss based on a solution method is relatively simple and fast so this result can potentially provide a path toward cost effective fabrication of SERS substrate for sensing applications.

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Metalorganic Chemical Vapor Deposition of Copper Films on TiN Substrates Using Direct Liquid Injection of (hfac)Cu(vtmos) Precursor ((hfac)Cu(vtmos)의 액체분사법에 의한 TiN 기판상 구리박막의 유기금속 화학증착 특성)

  • Jun, Chi-Hoon;Kim, Youn-Tae;Kim, Dai-Ryong
    • Korean Journal of Materials Research
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    • v.9 no.12
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    • pp.1196-1204
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    • 1999
  • We have carried out copper MOCVD(metalorganic chemical vapor deposition) onto the reactive sputtered PVD-TiN and rapid thermal converted RTP-TiN substrates using direct liquid injection for effective delivery of the (hfac)Cu(vtmos) [$C_{10}H_{13}O_{5}CuF_{6}$Si: 1,1,1,5,5,5-hexafluoro-2,4- pentadionato (vinyltrimethoxysilane) copper (I)] precursor. Especially, the influences of deposition conditions and the substrate type on growth rate, crystal structure, microstructure, and electrical resistivity of copper deposits have been discussed. It is found that the film growth with 0.2ccm precursor flow rate become mass-transfer controlled up to Ar flow rate of 200sccm and pick-up rate controlled at a vaporizer above 1.0Torr reactor pressure. The surface-reaction controlled region from 155 to 225$^{\circ}C$ at 0.6Torr reactor pressure results in the apparent activation energies of 12.7~14.1kcal/mol, and above 224$^{\circ}C$ the growth rate with $H_2$ addition could be improved compared to the pure Ar carrier. The Cu/RTP-TiN structures which have high copper nucleation density in initial stage of growth show more pronounced (111) preferred orientations and lower electrical resistivities than those on PVD-TiN. The variation of electrical resistivity with substrate temperature reflects the three types of film microstructure changes, showing the lowest value for the deposit at 165$^{\circ}C$ with small grains of good contacts.

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Formation of Thin $CoSi_2$by Layer Inversion of Co/Nb bi-layer (Co/Nb 이중층 구조의 막역전을 이용한 박막 $CoSi_2$의 형성)

  • Lee, Jong-Mu;Gwon, Yeong-Jae;Lee, Byeong-Uk;Kim, Yeong-Uk;Lee, Su-Cheon
    • Korean Journal of Materials Research
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    • v.6 no.8
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    • pp.779-785
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    • 1996
  • Thin $700^{\circ}C$films were formed through layer inversion of Co/Nb bilayer during rapid thermal annealing(RTA). The Nb interlayer seems to effectively prevent over-consumption of Si and to control the silicidation reaction by forming Co-Nb intermetallic compounds and removing the native oxide formed on Si substrate which interferes the uniform Co-Si interaction. The final layer structure of the Co/Nb bilayer after $700^{\circ}C$ RTA was found to be ${Nb}_{2}{O}_{3}$/${Co}_{2}$Si.CoSi/${NbCo}_{x}$/Nb(O, C)/${CoSi}_{2}$/ Si. The layer inversion and the formation of a stable CoSi, phase occurred above $700^{\circ}C$, and the Nb silicides were not found at any annealing temperature. These may be due to the formation of very stable Co-Nb intermetallic compounds and Nb oxides which limit the moving of Co and Si.

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