• Title/Summary/Keyword: Condensation Reaction

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Surface Modification of Alumina Ceramic with Mg2Al4Si5O18 Glass by a Sol-Gel Process (졸-겔 공정으로 합성된 코디어라이트를 이용하여 알루미나의 표면개질)

  • Choi, Pil-Gyu;Chu, Min Cheol;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.24 no.1
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    • pp.48-52
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    • 2014
  • The Mg-enriched magnesium aluminum silicate (MAS) glass is known for its higher mechanical strength and chemical resistance. Among such glasses, cordierite ($Mg_2Al_4Si_5O_{18}$) is well known to have a low thermal expansion and low melting point. Polycrystalline engineering ceramics such as alumina can be strengthened by a surface modification with low thermal expansion materials. The present study involves the synthesis of cordierite by a sol-gel process and investigates the effect of glass penetration on the surface of alumina. The cordierite powders were prepared from $Al(OC_3H_7)_3$, $Mg(OC_2H_5)_2$ and tetraethyl orthosilicate by hydrolysis and condensation reaction. The cordierite powders were characterized by X-ray diffraction (XRD, Rigaku), scanning electron microscope (SEM, JEOL: JSM-5610), energy dispersive spectroscopy (EDS, JEOL: JSM-5610), and universal testing machine (UTM, INSTRON). The X-ray diffraction patterns showed that the synthesized particles were ${\mu}$-cordierite calcined at $1100^{\circ}C$ for 1 h. The shape of synthesized cordierite was changed from ${\mu}$-cordierite to ${\alpha}$-cordierite with increasing calcination temperature. Synthesized cordierite was used for surface modification of alumina. Cordierite powders penetrated deeply into the alumina sample along grain boundaries with increasing temperature. The results of surface modification tests showed that the strength of the prepared alumina sample increased after surface modification. The strength of a surface modified with synthesized cordierite increased the most, to about 134.6MPa.

Preparation and Characterization of Organic-inorganic Hybrid Composite Film with Plate-shaped Alumina by Electrophoretic Deposition as a Function of Aging Time of Sol-Gel Binder

  • Kim, Doo Hwan;Park, Hee Jeong;Choi, Jinsub;Lim, Hyung Mi
    • Journal of the Korean Ceramic Society
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    • v.52 no.5
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    • pp.366-373
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    • 2015
  • Sol-gel binder was prepared by hydrolysis and condensation reaction using boehmite sol and methyltrimethoxysilane as a function of aging-time. The coating slurry was composed of a plate-shape alumina in the sol-gel binder for the EPD process, in which particles dispersed in the slurry were deposited on the electrode under an electric field due to the surface charge. We studied the effects of three parameters: the content of boehmite, the aging time, and the applied voltage, on the physical, thermal, and electrical properties of the hybrid composite films by EPD. The amount of boehmite was 10 ~ 20 wt% and the aging time was 0.5 ~ 72, with a fixed amount of plate-shape alumina of 10 wt%. The condition of applied voltage was 5 ~ 30 V with a distance of 2 cm between the electrode during the EPD process. We confirmed that a structure of hybrid composite films of well-ordered plate alumina was deposited on the substrate when the film was prepared using a sol-gel binder composed of 15 wt% boehmite with 1 hr aging time and EPD at 10 V. The process shows a weight loss of 7% at $500^{\circ}C$ in TGA and a breakdown voltage of 8 kV at $87{\mu}m$.

Poling Field Effect on Absorption and Luminescence of Disperse Red-19 and TiO2 Composites

  • Kim, Byoung-Ju;Hwang, Un-Jei;Jo, Dong-Hyun;Lim, Sae-Han;Kang, Kwang-Sun
    • Current Photovoltaic Research
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    • v.3 no.1
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    • pp.5-9
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    • 2015
  • Absorption and luminescence characteristics of disperse red-19 (DR-19) and $TiO_2$ composite have been investigated with various poling electric field strengths. Two step synthetic processes were employed to employ the DR-19 to the $TiO_2$ sol-gel. Firstly, urethane bond formation between DR-19 (-OH) and 3-isocyanatopropyl triethoxysilane (ICPTES, -N=C=O) performed (ICPDR) prior incorporation to the $TiO_2$ sol-gel. Secondary, the hydrolysis of the ethoxy group from the ICPTES and condensation reaction between silanol groups from ICPTES and $TiO_2$ sol-gel were performed. The ICPDR and $TiO_2$ sol-gel ($DRTiO_2$) were mixed and stirred for several days. The composite was coated to the ITO coated glass substrate. Corona poling were performed before drying the composite with various electric field strengths. The absorption intensity decreased with the increase of the poling field strength, which resulted in the increase of poling efficiency. The photoluminescence also decreased as the poling field strength increased. There is long luminescence tail for the poled $DRTiO_2$ film compared with unpoled $DRTiO_2$ film. The luminescence long tail indicates that the self-trapped excitons and polarons were generated when the $DRTiO_2$ film was poled with electric field.

Solution-processed Dielectric and Quantum Dot Thin Films for Electronic and Photonic Applications

  • Jeong, Hyeon-Dam
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.37-37
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    • 2010
  • Silicate-silsesquioxane or siloxane-silsesquioxane hybrid thin films are strong candidates as matrix materials for ultra low dielectric constant (low-k) thin films. We synthesized the silicate-silsesquioxane hybrid resins from tetraethoxyorthosilicate (TEOS) and methyltrimethoxysilane (MTMS) through hydrolysis and condensation polymerization by changing their molar ratios ([TEOS]:[MTMS] = 7:3, 5:5, and 3:7), spin-coating on Si(100) wafers. In the case of [TEOS]:[MTMS] 7:3, the dielectric permittivity value of the resultant thin film was measured at 4.30, exceeding that of the thermal oxide (3.9). This high value was thought to be due to Si-OH groups inside the film and more extensive studies were performed in terms of electronic, ionic, and orientational polarizations using Debye equation. The relationship between the mechanical properties and the synthetic conditions of the silicate-silsesquioxane precursors was also investigated. The synthetic conditions of the low-k films have to be chosen to meet both the low orientational polarization and high mechanical properties requirements. In addition, we have investigated a new solution-based approach to the synthesis of semiconducting chalcogenide films for use in thin-film transistor (TFT) devices, in an attempt to develop a simple and robust solution process for the synthesis of inorganic semiconductors. Our material design strategy is to use a sol-gel reaction to carry out the deposition of a spin-coated CdS film, which can then be converted to a xerogel material. These devices were found to exhibit n-channel TFT characteristics with an excellent field-effect mobility (a saturation mobility of ${\sim}\;48\;cm^2V^{-1}s^{-1}$) and low voltage operation (< 5 V). These results show that these semiconducting thin film materials can be used in low-cost and high-performance printable electronics.

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Castor oil based hyperbranched polyester/bitumen modified fly ash nanocomposite

  • Bhagawati, Deepshikha;Thakur, Suman;Karak, Niranjan
    • Advances in nano research
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    • v.4 no.1
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    • pp.15-29
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    • 2016
  • A low cost environmentally benign surface coating binder is highly desirable in the field of material science. In this report, castor oil based hyperbranched polyester/bitumen modified fly ash nanocomposites were fabricated to achieve the desired performance. The hyperbranched polyester resin was synthesized by a three-step one pot condensation reaction using monoglyceride of castor oil based carboxyl terminated pre-polymer and 2,2-bis (hydroxymethyl) propionic acid. Also, the bulk fly ash of paper industry waste was converted to hydrophilic nano fly ash by ultrasonication followed by transforming it to an organonano fly ash by the modification with bitumen. The synthesized polyester resin and its nanocomposites were characterized by different analytical and spectroscopic tools. The nanocomposite obtained in presence of 20 wt% styrene (with respect to polyester) was found to be more homogeneous and stable compared to nanocomposite without styrene. The performance in terms of tensile strength, impact resistance, scratch hardness, chemical resistance and thermal stability was found to be improved significantly after formation of nanocomposite compared to the pristine system after curing with bisphenol-A based epoxy and poly(amido amine). The overall results of transmission electron microscopic (TEM) analysis and performance showed good exfoliation of the nano fly ash in the polyester matrix. Thus the studied nanocomposites would open up a new avenue on development of low cost high performing surface coating materials.

Study on Manufacture of High Purity TiCl4 and Synthesis of High Purity Ti Powders (고순도 TiCl4 제조 및 이를 활용한 고순도 Ti 분말 제조 공정 연구)

  • Lee, Jieun;Yoon, Jin-Ho;Lee, Chan Gi
    • Journal of Powder Materials
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    • v.26 no.4
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    • pp.282-289
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    • 2019
  • Ti has received considerable attention for aerospace, vehicle, and semiconductor industry applications because of its acid-resistant nature, low density, and high mechanical strength. A common precursor used for preparing Ti materials is $TiCl_4$. To prepare high-purity $TiCl_4$, a process based on the removal of $VOCl_3$ has been widely applied. However, $VOCl_3$ removal by distillation and condensation is difficult because of the similar physical properties of $TiCl_4$ and $VOCl_3$. To circumvent this problem, in this study, we have developed a process for $VOCl_3$ removal using Cu powder and mineral oil as purifying agents. The effects of reaction time and temperature, and ratio of purifying agents on the $VOCl_3$ removal efficiency are investigated by chemical and structural measurements. Clear $TiCl_4$ is obtained after the removal of $VOCl_3$. Notably, complete removal of $VOCl_3$ is achieved with 2.0 wt% of mineral oil. Moreover, the refined $TiCl_4$ is used as a precursor for the synthesis of Ti powder. Ti powder is fabricated by a thermal reduction process at $1,100^{\circ}C$ using an $H_2-Ar$ gas mixture. The average size of the Ti powder particles is in the range of $1-3{\mu}m$.

Preparation of PDMS Surface Modifier Using Silane-Functionalized Polymer Precursor Manufacture and Their Properties (실란 기능화 아크릴 고분자 전구체를 이용한 PDMS 표면 개질제 제조 및 표면 물성)

  • Shin, Jae-Hyeon;Kim, Nahae;Kim, Juyoung
    • Journal of Adhesion and Interface
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    • v.19 no.4
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    • pp.154-162
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    • 2018
  • Plasma treatment and corona treatment have been used for surface modification of polydimethylsiloxane (PDMS) film by activating its surface with the -OH group. Adhesion promoter or coupling agent was also used to improve adhesion of PDMS film with various materials. However, obtained hydrophilicity onto the surface of PDMS films with those processes was transient and vulnerable. In this study, a new alkoxysilane-functionalized acrylic polymer precursor was first synthesized by copolymerization process, and then was reacted with HO-terminated PDMS through condensation reaction to prepare a new surface modifier for PDMS film. The structure and molecular weight of the prepared surface modifier were confirmed by 1H-NMR and GPC measurement. Surface properties of surface modifier-coated PDMS films were also investigated by using XPS, ATR and WCA analysis. The adhesion between the PDMS film and the surface modifier was tested using cross-cut test.

Dispersion Stability and Mechanical Properties of ZrO2/High-temp Composite Resins by Nano- and Micro-particle Ratio for Stereolithography 3D Printing (나노 및 마이크로 입자 비율에 따른 광조형 3D 프린팅용 ZrO2/High-temp 복합 수지의 분산 안정성 및 기계적 특성)

  • Song, Se Yeon;Park, Min Soo;Yun, Ji Sun
    • Korean Journal of Materials Research
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    • v.29 no.4
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    • pp.221-227
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    • 2019
  • This study examines the role of the nano- and micro-particle ratio in dispersion stability and mechanical properties of composite resins for SLA(stereolithography) 3D printing technology. VTES(vinyltriethoxysilane)-coated $ZrO_2$ ceramic particles with different nano- and micro-particle ratios are prepared by a hydrolysis and condensation reaction and then dispersed in commercial photopolymer (High-temp) based on interpenetrating networks(IPNs). The coating characteristics of VTES-coated $ZrO_2$ particles are observed by FE-TEM and FT-IR. The rheological properties of VTES-coated $ZrO_2/High-temp$ composite solution with different particle ratios are investigated by rheometer, and the dispersion properties of the composite solution are confirmed by relaxation NMR and Turbiscan. The mechanical properties of 3D-printed objects are measured by a tensile test and nanoindenter. To investigate the aggregation and dispersion properties of VTES-coated $ZrO_2$ ceramic particles with different particle ratios, we observe the cross-sectional images of 3D printed objects using FE-SEM. The 3D printed objects of the composite solution with nano-particles of 80 % demonstrate improved mechanical characteristics.

Syntheses and Characterization of Polyurethane Polymers with Versatile Stilbene Chromophores (Stilbene 발광 유도체를 가지는 Polyurethane을 기본으로 하는 고분자의 합성 및 특성)

  • Jin, Youngeup;Noh, Ji Young;Park, Seong Soo;Ju, Changsik;Suh, Hongsuk
    • Applied Chemistry for Engineering
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    • v.22 no.4
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    • pp.348-352
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    • 2011
  • In this research, we have synthesized new pendant-type polyurethane polymers by introducing various chromophores with stilbene derivatives in the side-chain of the polymer backbone. The Stilbene monomers, N,N-bis(2-hydroxyethyl) amino-4'-cyanostilbene, N,N-bis(2-hydroxyethyl)amino-4'-methoxy stilbene, N,N-bis(2-hydroxyethyl)amino-4'-acetylstilbene, and N,N-bis(2-hydroxyethyl) amino stilbene, were synthesized by Wittig reaction. Another stilbene monomer, N,N-bis(2-hydroxyethyl)amino-4'-nitrostilbene, was synthesized by Knoevenagel condensation. By the measurement of UV-Vis absorption and Photoluminescence (PL) spectrum, we found that introduction of the electron-withdrawing group as a substituent shifts both UV-Vis and PL spectra to longer wavelength, and the introduction of the electron-donating group results in blue-shift of the spectrum. In case of polymer with $NO_2$ group as a substituent, PL is quenched.

Modification of NiO Using 2PACz for P-i-n Perovskite Solar Cells (P-i-n 페로브스카이트 태양전지 응용을 위한 2PACz을 이용한 NiO의 개질)

  • Seon-Min Lee;Seok-Soon Kim
    • Applied Chemistry for Engineering
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    • v.35 no.2
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    • pp.100-106
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    • 2024
  • To improve charge transfer and surface contact between NiO and perovskite, sol-gel derived NiO is modified with [2-(9H-car-bazol-9-yl)ethyl] phosphonic acid (2PACz) in p-i-n structured perovskite solar cells (PeSCs). The phosphonic acid head group in the 2PACz can bind to the hydroxyl groups on the surface of NiO by a condensation reaction, which results in a better-matched energy level with the valence band of perovskite layers, reducing nonradiative recombination and energy loss. Furthermore, the formation of pin-hole free perovskite films is observed in the 2PACz modified NiO system. Consequently, the combination of sol-gel processed NiO with optimal 2PACz exhibits a higher efficiency of 17.08% and superior stability under ambient air conditions without any encapsulation, compared to a bare NiO based device showing 13.69%.