• Title/Summary/Keyword: Thermal reaction

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Synthesis and Characteristics of Diphosphine-digold complexes as Light-Emitting Materials (발광 재료용 다이포스핀-다이골드 착물의 합성과 특성 연구)

  • Kim, Jun-Ho;Sohn, Byung-Chung;Ha, Yun-Kyoung
    • Journal of the Korean Applied Science and Technology
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    • v.19 no.2
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    • pp.103-107
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    • 2002
  • Diphosphine dinuclear gold(I) complexes were synthesized from the reaction of bridged diphosphines and gold ions. As a bridged diphosphine, 1,2-bis(diphenylphosphino)metbane (dppm) or 1,1'-Bis(diphenylphosphino) ferrocene (dppf) was introduced. As anionic ligands, CI was first coordinated to Au, resulting in (diphosphine)$(AuCl)_{2}$. Then, the ligand, SPh, was substituted for Cl in the chloride complex to give (diphosphine)$(AuSPh)_{2}$. As a result, three digold complexes, (dppm)$(AuCl)_{2}$. (I), (dppf)$(AuCl)_{2}$. (II), and (dppf)$(AuSPh_{2}$. (III) were prepared in this study. The thermal properties were investigated at first hand to confirm that the gold complexes were in fact formed. The digold complexes were decomposed above $200^{\circ}C$ while the ligand, dppm or dppf, melts under $180^{\circ}C$ The photoluminescence (PL) spectra of the spin-coated thin films showed the maximum peak at 590, 595, and 540nm for the complex, I, II, and III, respectively. These complexes were found to give the orange color phosphorescence. Therefore, these digold complexes can be candidates for orange-red phosphorescent materials in organic electroluminescent devices (OELD). Further studies on application of the complexes as a dopant in an emitting layer are in progress in our laboratory.

Synthesis of Organic salt Oxidizer, Guanidine Dinitramide (유기염 고체산화제 Guanidine Dinitramide의 합성연구)

  • Kim, Woo-Ram;Kwon, Youn-Ja;Jo, Young-Min;Jung, Sun-Tae
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.3
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    • pp.345-351
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    • 2014
  • Dinitramide ($N(NO_2)_2$) salts are one of plausible oxidizing agents for a high efficient propellant. Guanidine dinitramide (GDN) is an organic salt improving its stability against moisture, so that enables massive production and long term storage. Several types of GDN (GDN-1,2,3,4,5) were synthesized using some types of starting materials such as guanidine acetate, chloride, carbonate, nitrate and sulfate. As a result of the experimental work, synthesized GDN from the carbonate salt appeared fairly pure relatively higher yield (99%) than the other samples. The absorption wave length of all prepared GDNs by FTIR were found at 3452, 3402, 3354, 3278, 3208, 1642, 1570, 1492, 1416, 1337, 1179 and $1000cm^{-1}$. DSC analysis found a thermal phase change at $130^{\circ}C$, and indicated exothermic reaction at about $150^{\circ}C$ to $160^{\circ}C$.

Syntheses of Alternating Head-to Head Vinyl Copolymers and Vinyl Terpolymers via Ring-Opening Mechanism. Ring-Opening Polymerization of Substituted-3,4-dihydro-2H-pyrans

  • Lee, Ju-Yeon;Cho, I-Whan
    • Bulletin of the Korean Chemical Society
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    • v.8 no.2
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    • pp.96-101
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    • 1987
  • 2-Ethoxy-6-methoxy-5-cyano-3,4-dihydro-2H-pyran (1_a$), 2-n-butoxy-6-methoxy-5-cyano-3,4-dihydro-2H-pyr an (1b), 2-isobutoxy-6-methoxy-5-cyano-3,4-dihydro-2H-py ran ($1_c$), and 2-ethoxy-6-methoxy-3-methyl-5-cyano-3,4-dihydro -2H-pyran ($1_d$) were prepared by (4 + 2) cycloaddition reaction of methyl $\alpha$-cyanoacrylate with the corresponding alkyl vinyl ethers. Compounds $1_{a-d}$ were ring-open polymerized by cationic catalyst to obtain alternating head-to-head (H-H) copolymers. For comparison, head-to-tail (H-T) copolymer $3_a$ was also prepared by free radical copolymerization of the corresponding monomers. The H-H copolymer exhibited minor differences in its $1_H% NMR and IR spectra, but in the $^{13}C$ NMR spectra significant differences were observed between the H-H and H-T copolymers. Glass transition temperature ($T_g$) of H-H copolymer was higher than that of the H-T copolymer, but thermal decomposition temperature of the H-H copolymer was lower than that of the H-T copolymer. Compounds $1_a$, $a_b$, and $1_c$, copolymerized well with styrene by cationic catalyst, but compound 1d failed to copolymerize with styrene. All of the H-H and H-T copolymers were soluble in common solvents and the inherent viscosities were in the range 0.2-0.4 dl/g.

Study on the Development of CVD Precursors I-Synthesis and Properties of New Titanium β-Diketonates

  • 홍성택;임종태;이중철;Ming Xue;이익모
    • Bulletin of the Korean Chemical Society
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    • v.17 no.7
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    • pp.637-642
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    • 1996
  • Preparation and properties of potential CVD (Chemical Vapor Deposition) precursors for the TiO2, a major component of the perovskite materials such as PT, PLT, PZT, and PLZT were investigated. Reactions between β-diketones and TiMe3, formed in situ failed to produce stable Ti(β-diketonate)3 complexes but a stable purple solid, characterized as (OTi(BPP)2)2 (BPP=1,3-biphenyl-1,3-propanedione) was obtained when BPP was used. Several new Ti(Oi-Pr)2(β-diketonate)2 complexes with aromatic or ring substituents were synthesized by the substitution reaction of Ti(OiPr)4by β-diketones and characterized with 1H NMR, IR, ICP, and TGA. Solid complexes such as Ti(Oi-Pr)2(BAC)2 (BAC=1.-phenyl-2,4-pentanedione), Ti(Oi-Pr)2(BPP)2, Ti(Oi-Pr)2(1-HAN)2 (1-HAN=2-hydroxy-1-acetonaphthone), Ti(Oi-Pr)2(2-HAN)2 (2-HAN=1-hydroxy-2-acetonaphthone), Ti(Oi-Pr)2(ACCP)2 (ACCP=2-acetylcyclopentanone), and Ti(Oi-Pr)2(HBP)2 (HBP=2-hydroxybenzophenone) were found to be stable toward moisture and air. Ti(Oi-Pr)2(ACCP)2 and Ti(Oi-Pr)2(HBP)2 were proved to have lower melting points and higher decomposition temperatures. However, these complexes are thermally stable and pyrolysis under an inert atmosphere resulted in incomplete decomposition. Ti(Oi-Pr)2(DPM)2 (DPM=dipivaloylmethane) and Ti(Oi-Pr)2(HFAA)2 (HFAA=hexafluoroacetylacetone) were sublimed substantially during the thermal decomposition. Pyrolysis mechanism of these complexes are dependent on type of β-diketone but removal of Oi-Pr ligands occurs before the decomposition of β-diketonate ligands.

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.

Role of Features in Plasma Information Based Virtual Metrology (PI-VM) for SiO2 Etching Depth (플라즈마 정보인자를 활용한 SiO2 식각 깊이 가상 계측 모델의 특성 인자 역할 분석)

  • Jang, Yun Chang;Park, Seol Hye;Jeong, Sang Min;Ryu, Sang Won;Kim, Gon Ho
    • Journal of the Semiconductor & Display Technology
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    • v.18 no.4
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    • pp.30-34
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    • 2019
  • We analyzed how the features in plasma information based virtual metrology (PI-VM) for SiO2 etching depth with variation of 5% contribute to the prediction accuracy, which is previously developed by Jang. As a single feature, the explanatory power to the process results is in the order of plasma information about electron energy distribution function (PIEEDF), equipment, and optical emission spectroscopy (OES) features. In the procedure of stepwise variable selection (SVS), OES features are selected after PIEEDF. Informative vector for developed PI-VM also shows relatively high correlation between OES features and etching depth. This is because the reaction rate of each chemical species that governs the etching depth can be sensitively monitored when OES features are used with PIEEDF. Securing PIEEDF is important for the development of virtual metrology (VM) for prediction of process results. The role of PIEEDF as an independent feature and the ability to monitor variation of plasma thermal state can make other features in the procedure of SVS more sensitive to the process results. It is expected that fault detection and classification (FDC) can be effectively developed by using the PI-VM.

Optical Properties of Y3Al5O12;Ce3+,Pr3+ Transparent Ceramic Phosphor for High Power White Lighting (고출력 백색 광원용 Y3Al5O12;Ce3+,Pr3+ 투명 세라믹 형광체의 광학특성)

  • Kang, Taewook;Lim, Seokgyu;Kim, Jongsu;Jeong, Yongseok
    • Korean Journal of Materials Research
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    • v.29 no.2
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    • pp.116-120
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    • 2019
  • We prepared $Y_3Al_5O_{12};Ce^{3+},Pr3^{+}$ transparent ceramic phosphor using a solid state reaction method. By XRD pattern analysis and SEM measurement, our phosphors reveal an Ia-3d(230) space group of cubic structure, and the transparent ceramic phosphor has a polycrystal state with some internal cracks and pores. In the Raman scattering measurement with an increasing temperature, lattice vibrations of the transparent ceramic phosphor decrease due to its more perfect crystal structure and symmetry. Thus, low phonon generation is possible at high temperature. Optical properties of the transparent ceramic phosphor have broader excitation spectra due to a large internal reflection. There is a wide emission band from the green to yellow region, and the red color emission between 610 nm and 640 nm is also observed. The red-yellow phosphor optical characteristics enable a high Color Rendering Index (CRI) in combination with blue emitting LED or LD. Due to its good thermal properties of low phonon generation at high temperature and a wide emission range for high CRI characteristics, the transparent ceramic phosphor is shown to be a good candidate for high power solid state white lighting.

Germanium-based pinning dopants for MgB2 bulk superconductors

  • Chung, K.C.;Ranot, M.;Shinde, K.P.;Oh, Y.S.;Kang, S.H.;Jang, S.H.;Hwang, D.Y.
    • Progress in Superconductivity and Cryogenics
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    • v.21 no.2
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    • pp.36-39
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    • 2019
  • Effects of the spherically shaped Ge and the rod-like carbon-coated Ge on the superconducting properties of $MgB_2$ were investigated. Pure Ge and carbon-coated Ge nano-powders were synthesized under the different amount of $CH_4$ (0 to 5 kPa) by using DC thermal plasma method. When the $CH_4$ was added ~100 nm sized Ge with a spherical shape changed to rod-like morphology with a diameter of ~30-70 nm and a length of ~400-500 nm. Also it was confirmed that thin carbon layers of a few nanometers were formed along the rod length and the agglomerated carbons were found on the edges of rods. Pure spherical Ge and Ge/C rods were mixed and milled with Mg & B precursor to form the doped $MgB_2$ bulk samples by the solid-state reaction method. Almost no change of $T_c$ was noticed for the pure Ge-added $MgB_2$, whereas $T_c$ was found to decrease with the Ge/C-added $MgB_2$ samples. It was found that the pure spherical Ge showed to have a negative effect on the flux pinning of $MgB_2$. However, Ge/C rods can enhance the flux pinning property of $J_c$ due to the coated carbon on Ge rods.

Accelerated Aging Characteristics of a Double Base Propellant (복기추진제의 가속 노화 특성 연구)

  • Go, Cheongah;Park, Youngchul;Seo, Taeseok;Moon, Youngtaek;Kim, Junhyung
    • Journal of the Korean Society of Propulsion Engineers
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    • v.23 no.4
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    • pp.61-69
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    • 2019
  • Accelerated aging test for the double base propellant was carried out at three different temperatures (60, 70, and $75^{\circ}C$) for over a year. To evaluate the aging characteristics of the double base propellant, the stabilizer contents and thermal decomposition kinetics were analyzed by using high performance liquid chromatography (HPLC) and AKTS-Thermokinetics software. As a result, stabilizer contents in the double base propellant gradually decreased according to the aging temperature and aging duration. The consumption rate of 2-NDPA in the accelerated aged propellants showed that it was two times faster at $75^{\circ}C$ in compared with ther rate at $70^{\circ}C$. These experimental values were simulated by the SB kinetic model, and it was shown that the two-step model with constant reaction orders n1=1 and n2=0 best describes the process of the stabilizer depletion for the double base propellant.

Inactivation of Human Norovirus GII. 4 on Oyster Crassostrea gigas by Electron Beam Irradiation (전자선 조사에 의한 신선굴(Crassostrea gigas) 중 휴먼노로바이러스 GII. 4의 저감화)

  • Kim, Ji Yoon;Jeon, Eun Bi;Choi, Man-Seok;Park, Shin Young
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.54 no.1
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    • pp.16-22
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    • 2021
  • This study investigated the reduction in human norovirus (HNV) GII. 4 count in pacific oyster Crassostrea gigas using electron beam irradiation. Infectious HNV GII. 4 was detected using RT-qPCR (real time reverse transcription-quantitative polymerase chain reaction) with PMA (propidium monoazide)/sarkosyl. At electron beam doses 1, 5, 7, and 10 kGy, the count of HNV GII. 4 was 2.74, 2.37, 2.06, and 1.55 log copies/μL (control, 3.01 log copy/μL), respectively, confirming that as the irradiation dose increased, norovirus count reduced significantly (P<0.05). After PMA/sarkosyl treatment, the counts further reduced at the same irradiation dose, and 10 kGy showed significant differences between the non-treated and PMA/sarkosyl-treated samples (P<0.05). The Ed (decimal reduction dose of electron beam) value based on the first-order kinetic model was 7.33 kGy (R2=0.98). No significant difference was observed in the pH values of the control (6.2) and electron beam-irradiated samples at all doses (6.1). For sensory evaluation, the non-treated sample scored the highest in all categories (5.25-6.17), while the samples treated with 10 kGy showed the lowest score (4.67-5.33), although without statistical significance (P>0.05). Overall, our results suggest that 7 kGy electron beam is sufficient for the non-thermal sterilization of oysters without causing significant changes in quality.