• Title/Summary/Keyword: Crosslinking temperature

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Structure and Property Analysis of Nanoporous Low Dielectric Constant SiCOH Thin Films

  • Heo, Gyu-Yong;Lee, Mun-Ho;Lee, Si-U;Park, Yeong-Hui
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2009.05a
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    • pp.167-169
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    • 2009
  • We have carried out quantitative structure and property analysis of the nanoporous structures of low dielectric constant (low-k) carbon-doped silicon oxide (SiCOH) films, which were deposited with plasma enhanced chemical vapor deposition (PECVD) using vinyltrimethylsilane (VTMS), divinyldimethylsilane (DVDMS), and tetravinylsilane (TVS) as precursor and oxygen as an oxidant gas. We found that the SiCOH film using VTMS only showed well defined spherical nanopores within the film after thermal annealing at $450^{\circ}C$ for 4 h. The average pore radius of the generated nanopores within VTMS SiCOH film was 1.21 nm with narrow size distribution of 0.2. It was noted that thermally labile $C_{x}H_{y}$ phase and Si-$CH_3$ was removed to make nanopore within the film by thermal annealing. Consequently, this induced that decrease of average electron density from 387 to $321\;nm^{-3}$ with increasing annealing temperature up to $450^{\circ}C$ and taking a longer annealing time up to 4 h. However, the other SiCOH films showed featureless scattering profiles irrespective of annealing conditions and the decreases of electron density were smaller than VTMS SiCOH film. Because, with more vinyl groups are introduced in original precursor molecule, films contain more organic phase with less volatile characteristic due to the crosslinking of vinyl groups. Collectively, the presenting findings show that the organosilane containing vinyl group was quite effective to deposit SiCOH/$C_{x}H_{y}$ dual phase films, and post annealing has an important role on generation of pores with the SiCOH film.

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Acrylic/Urea Crosslinked Polymers for High-Solid Coatings Applications (아크릴/우레아 가교 폴리머의 하이솔리드 도료에의 적용)

  • Chung, Dong-Jin;Park, Hyong-Jin;Kim, Sung-Rae;Hahm, Hyun-Sik;Park, Hong-Soo;Kim, Seong-Kil
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.1
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    • pp.8-19
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    • 2003
  • Environmental friendly acrylics/urea high-solid paints (BEHCU) were prepared through the curing reaction of acrylics resin(BEHC) containing 70wt% of solids content and butylated urea curing agent. BEHC was synthesized by addition copolymerization of caprolactone acrylate(CLA), 2-hydroxypropyl methacrylate(2-HPMA), ethyl methacrylate, and n-butyl acrylate. The addition polymerization of these monomers, especially including flexible CLA monomer and 2-HPMA monomer with OH funtional group, under appropriate reaction conditions resulted in polymers with controlled glass transition temperature($T_g$) and crosslinking density. The molecular weight($M_w$) of these polymers(BEHCs) was 2940${\sim}$3240 and polydispersity ($M_w/M_n$) was in the range of 1.61${\sim}$1.72. The viscosity and the molecular weight of these acrylic resins increased with increasing $T_g$. The coated films were prepared using curing reaction between BEHC resin and butylated urea curing agent at 100$^{\circ}C$ for 30 minutes. Our experimental resulted showed that enhancement of the coating properties such as adhesion, flexibility, impact resistance, water resistance, and abrasion resistance could be expected through introducing CLA component in acrylic resin for the high-solid content acrylics/urea coatings.

Pervaporation Separation of Water-Isopropyl Alcohol Mixtures Using PVA/PAN Hollow Fiber Composite Membranes (PVA/PAN 중공사 복합막을 이용한 IPA수용액의 투과증발분리)

  • Kim, Ji Seon;Cho, Eun Hye;Kang, Su Yeon;Cheong, Seong Ihl;Park, Hun Whee;Seo, Chang Hee;Rhim, Ji Won
    • Membrane Journal
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    • v.23 no.2
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    • pp.170-175
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    • 2013
  • Poly (vinyl alcohol) (PVA) solution containing the glutaraldehyde (GA) as a crosslinking agent was coated onto the polyacrylonitrile (PAN) hollow fiber membrane as the supporter. Pervaporation experiments were carried out to characterize the prepared PVA/PAN composite membrane for water-isopropyl alcohol mixture. The flux and separation factor were measured at 30, 50, $90^{\circ}C$ for the feed mixture of aqueous 85 wt% IPA solution with varying the reaction temperature and composition of coating solutions. Typically the flux showed 1,870 $g/m^2{\cdot}hr$ at $90^{\circ}C$ feed mixture and the coating concentration of 3.5 wt% and the highest separation factor of 804 was obtained at $30^{\circ}C$ feed mixture and the coating concentration of 7 wt% as well.

Preparation and Characteristics of Polyurethane Hybrid Sealant Modified with Polydimethylsiloxane (Polydimethylsiloxnae 변성 Polyurethane Hybrid Sealant의 제조와 그 특성)

  • Kang, Doo-Whan;Park, Seung-Woo
    • Polymer(Korea)
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    • v.35 no.5
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    • pp.488-492
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    • 2011
  • Three isocyanatopropyldimethoxysilylpolydimethylsiloxanes(IDMSi-PDMS) were synthesised from the reaction of isocyanatopropyltrimethoxysilane with monohydroxyl group termainated PDMS having different molecular weight($M_n$=5000, 10000, and 20000). Then PDMS modified polyurethane hybrid elastomer(PSMPH) were prepared from the reaction of IDMSi-PDMS with ${\alpha}$, ${\omega}$-hydroxyl group terminated polyurethane. PSMPH sealant was prepared by compounding PSMPH elastomer with additives such as plasticizer, adhesion promoter, crosslinking agent, vicosity increasing agent, inorganic filler, and catalyst at room temperature under nitrogen atmosphere. The methoxy group in the PSMPH sealant should be crosslinked with the hydroxyl group in the building stone or moisture by typical sol-gel reaction. The adhesive strength of the sealant having PDMS of $M_n$=5000 showed 40.28 kg of maxium load and 20.14 kg of break load. The shrinkage rate of the sealant having PDMS of $M_n$=20000 was 5.7% as the best result. Also, their skin over time, slump, oil content after 8 days under oil soaked paper and alkaline resistance characteristics show good results.

Partially Hydrolyzed Crosslinked Alginate-graft-Polymethacrylamide as a Novel Biopolymer-Based Superabsorbent Hydrogel Having pH - Responsive Properties

  • Pourjavadi A.;Amini-Fazi M. S.;Hosseinzadeh H.
    • Macromolecular Research
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    • v.13 no.1
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    • pp.45-53
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    • 2005
  • In this study, a series of highly swelling hydrogels based on sodium alginate (NaAlg) and polymethacryl­amide (PMAM) was prepared through free radical polymerization. The graft copolymerization reaction was performed in a homogeneous medium and in the presence of ammonium persulfate (APS) as an initiator and N,N'-methylenebis­acrylamide (MBA) as a crosslinker. The crosslinked graft copolymer, alginate-graft-polymethacrylamide (Alg-g­PMAM), was then partially hydrolyzed by NaOH solution to yield a hydrogel, hydrolyzed alginate-graft-poly­methacrylamide (H-Alg-g-PMAM). During alkaline hydrolysis, the carboxamide groups of Alg-g-PMAM were converted into hydrophilic carboxylate anions. Either the Alg-g-PMAM or the H-Alg-g-PMAM was characterized by FTIR spectroscopy. The effects of the grafting variables (i.e., concentration of MBA, MAM, and APS) and the alkaline hydrolysis conditions (i.e., NaOH concentration, hydrolysis time, and temperature) were optimized systematically to achieve a hydrogel having the maximum swelling capacity. Measurements of the absorbency in various aqueous salt solutions indicated that the swelling capacity decreased upon increasing the ionic strength of the swelling medium. This behavior could be attributed to a charge screening effect for monovalent cations, as well as ionic cross-linking for multivalent cations. Because of the high swelling capacity in salt solutions, however, the hydrogels might be considered as anti-salt superabsorbents. The swelling behavior of the superabsorbing hydrogels was also measured in solutions having values of pH ranging from 1 to 13. Furthermore, the pH reversibility and on/off switching behavior, measured at pH 2.0 and 8.0, suggested that the synthesized hydrogels were excellent candidates for the controlled delivery of bioactive agents. Finally, we performed preliminary investigations of the swelling kinetics of the synthesized hydrogels at various particle sizes.

Synthesis of Novel Network Polyesters Containing Malonate Group in Main Chain and Their Fluorescence Image Patterning via Photodegradation (주사슬에 말로네이트기를 가지는 신규 폴리에스테르의 합성과 광분해 특성을 이용한 형광 이미지 패터닝)

  • Jeong, Seon-Ju;Kwak, Gi-Seop;Jung, In-Tae;Lee, Dong-Ho;Roh, Hyung-Jin;Yoon, Keun-Byoung
    • Polymer(Korea)
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    • v.32 no.1
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    • pp.56-62
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    • 2008
  • Three types of network polyesters have been newly synthesized by a two-step condensation reaction by the various combination of several diols and diacids. When these polymer films were thermally treated at $240^{\circ}C$, they exhibited absorptions in a visible range despite the forbidden transition of carbonyl group. When excited at wavelengths above 330 nm, the polymers showed fluorescences in a wide visible range from blue to near yellow. These fluorescence phenomena are due to the formation of certain conjugated structures by the Knoevenagel type self-condensation under the high-temperature thermal treatment. These polymers showed significant difference in the thermal properties as a function of the degrees of chemical crosslinking. They also underwent photodegradation. Highly resolved, fluorescent image patterns were successfully obtained by the photodegradation of malonate group under a strong UV-light irradiation.

Preparation of Composite Membranes for Recovery of Unreacted Olefin Monomers (미반응 올레핀계 모노머 회수를 위한 복합막의 제조)

  • Kim, Hyun-Gi;Kim, Sang-Yong;Kim, Sung-Soo
    • Membrane Journal
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    • v.20 no.4
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    • pp.297-303
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    • 2010
  • Composite membranes were prepared for membrane/cold condensation process for recovery of unreacted olefin monomer from the polyolefin polymerization process by solution coating and plasma polymerization processes. Poly(dimethylsiloxane) (PDMS) solution was coated on polysulfone (PSF) support and increase of prepolymer content in solution made more dense membrane structure to result in the increase of separation factor while absolute flux decreased. Permeation of organic materials through the composite membranes follows the sorption and diffusion mechanism, which brought about the results that separation factor increased with critical temperature of the organic materials, and that flux increased with the increase of the molar volume. Crosslinking period affected the permeation characteristics. Other types of composite membranes were fabricated by plasma polymerization of siloxane materials on polypropylene (PP) and PSF supports. PP was tested as a support for composite membranes, which had not been used so far in solution coating process, and plasma polymerization made the composite membranes equivalent performances to those of membranes prepared by solution coating process.

Physicochemical Characterization of Extrudate Solid Formulation of Angelica gigas Nakai Prepared by Hot Melt Extrusion Process

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Koo, Ja Seong;Park, Cheol Ho;Kang, Wie Soo
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2018.04a
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    • pp.72-72
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    • 2018
  • The root of Angelica gigas Nakai (AGN) is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, a major challenge associated with the usage of the active compounds from AGN is their poor water solubility. Therefore, this work aimed to enhance the solubility of active compounds by a chemical (viz. surfactant) and physical (hot melt extrusion) crosslinking method (CPC). Infrared Fourier transform spectroscopy (FT-IR) revealed multiple peaks in extrudate solids representing new functional groups including carboxylic acid, alkynes and benzene derivatives. Differential scanning calorimetry (DSC) analysis of the extrudate showed lower glass transition temperature (Tg) and lower enthalpy (${\Delta}H$) (Tg: $43^{\circ}C$; ${\Delta}H$: <6 (J/g)) compared to the non-extrudate (Tg $68.5^{\circ}C$; ${\Delta}H$: 123.2) formulations. X-ray powder diffraction (XRD) analysis revealed amorphization of crystal materials in extrudate solid. In addition, nanonization, enhanced solubility and higher extraction of phenolic compounds were achieved in the extrudate solid. Among the different extrudates, acetic acid- and Span 80-mediated formulations showed superior extractions. We conclude that the CPC method successfully enhanced the production of amorphous nano dispersions from extrudate solid formulations.

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Decrosslinking of Cross-linked Polyethylene using Supercritical Methanol (초임계 메탄올을 이용한 가교 폴리에틸렌의 탈가교화)

  • Hong, Soon Man;Cho, Hang-kyu;Koo, Chong Min;Lee, Jang Hoon;Park, Wan Yong;Lee, Hong-Shik;Lee, Youn-Woo
    • Korean Chemical Engineering Research
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    • v.46 no.1
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    • pp.63-68
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    • 2008
  • We investigated the recycling method to re-plasticize cross-linked polyethylene by using supercritical methanol. The cross-linked polyethylene is successfully fragmented to thermoplasticized polyethylene with little degradation reactions in supercritical fluids. The thermo-plasticization reaction was accelerated with increase in temperature in the range from $360^{\circ}C$ to $400^{\circ}C$, resulting in decrease in crosslinking density, molecular weight and mechanical properties. However, the thermoplasticized polyethylene at $360^{\circ}C$ showed comparable tensile strength and impact strength with a raw resin of crosslinked polyethylene. Chemical structure of main chain of polyethylene was not affected by reaction condition.

Studies on Whole Cell Immobilized Glucose Isomerase - I. Preparation and Properties of Whole Cell Immobilized Glucose Isomerase - (포도당 이성화 효소의 세포 고정화에 관한 연구 - I. 세포 고정화 효소의 제조와 성질 -)

  • Ahn, Byung-Yoon;Byun, Si-Myung
    • Korean Journal of Food Science and Technology
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    • v.11 no.3
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    • pp.192-199
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    • 1979
  • With cells of Streptomyces spp K-45 isolated from soil, the immobilization of glucose isomerase by a series of treatments ; heat, carefully manipulated drying, extrusion with a thickening agent, and glutaraldehyde-induced crosslinking, was presented. This was aimed to obtain a mechanically stable form of whole cell containing glucose isomerase. The resulted pellet form had a good mechanical strength, compared with a commercial product, and showed 26 % of the activity recovery. The specific activity was 48.1 units per g of the dry material. The immobilized glucose isomerase generally showed properties similar to those of the soluble enzyme ; optimal pH at $7.5{\sim}9.0$, optimal temperature at $80{\sim}85^{\circ}C$, activation energy of 10.9 kcal/mole, and $K_m$ for glucose of 10.9M. The immobilized enzyme was very thermostable and pH stable.

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