• Title/Summary/Keyword: IR and Raman spectroscopy

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The Formation of Metal (M=Co(II), Ni(II), and Cu(II)) Complexes by Aminosilanes Immobilized within Mesoporous Molecular Sieves

  • 박동호;박성수;최상준
    • Bulletin of the Korean Chemical Society
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    • v.20 no.3
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    • pp.291-296
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    • 1999
  • The immobilization of APTMS(3-(2-aminoethylamino)propyltrimethoxysilane) and AAPTMS(3-(2-(2-aminoethyl)aminoethylanino)propyltrimethoxysilane) on the surface of high quality mesoporous molecular sieves MCM-41 and MCM-48 have been confirmed by F.T.-IR spectroscopy, Raman spectroscopy, 29Si solid state NMR, and a surface polarity measurement using Reichardt's dye. The formation of metal (Co(Ⅱ), Ni(Ⅱ), and Cu(Ⅱ)) complexes by immobilized aminosilanes have been investigated by photoacoustic spectroscopy(PAS). The assignment of UV-Vis. PAS bands makes it possible to identify the structure of metal complexes within mesoporous molecular sieves. Co(Ⅱ) ion may be coordinated mainly in a tetrahedral symmetry by two APTMS onto MCM-41, and in an octahedral one by two AAPTMS. Both Ni(Ⅱ) and Cu(Ⅱ) coordinated by aminosilanes within MCM-41 form possibly the octahedral complexes such as [Ni(APTMS)2(H20)2]2+, [Ni(AAPTMS)2]2+, [Cu(APTMS)2(H2O)2]2+, and [Cu(AAPTMS)(H2O)3]2+, respectively. The PAS band shapes of complexes onto MCM-48 are similar to those of corresponding MCM-41 with the variation of PAS intensity. Most of metal ion(Ⅱ) within MCM-41 and MCM-48 are coordinated by aminosilanes without the impregnation on the surface.

Characterization of coated colorless synthetic moissanite (코팅된 무색 합성 모이사나이트의 특징)

  • Choi, Hyunmin;Kim, Youngchool;Jang, Hansoo;Seok, Jeongwon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.1
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    • pp.7-11
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    • 2022
  • Recently, Hanmi Gemological Institute & Laboratory (HGI) had an opportunity to examine 5 transparent synthetic moissanite. The round brilliants ranged from 0.93 to 0.96 ct and had a colorless, pink, yellow, blue, and red color. Advanced testing results, including Fourier-transform infrared (FTIR) and Raman spectroscopy, identified all the specimens as synthetic moissanite. Under the microscope, all samples except the colorless were confirmed to be a synthetic moissanite coated with a colored film. EDXRF chemical analysis detected very weak X-ray fluorescence peak characteristics of Ca, Ti, and Co in the colored samples. These features were not detected in the colorless sample. Raman spectroscopy investigation was unable to detect the 1332 cm-1 (produced by sp3 bonding of carbon atoms) or the ~1550 cm-1 (produced by graphite-related sp2 bonding) peak in the colorless sample. The SEM image of the colorless sample showed no indication of a coating. The TEM image of the colorless sample revealed the presence of a 3~8 nm thick layer on the moissanite. Moreover, from the corresponding STEM Z-contrast image combined with the energy-dispersive X-ray spectroscopy (EDX) line profiles and EDX elemental maps, this layer was estimated to be carbon, silicon and oxygen.

The Study of Sputtered SiGe Thin Film Growth for Photo-detector Application (광검출기 응용을 위하여 스퍼터된 미세결정 SiGe 박막성장 연구)

  • Kim, Do-Young;Kim, Sun-Jo;Kim, Hyung-Jun;Han, Sang-Youn;Song, Jun-Ho
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.6
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    • pp.439-444
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    • 2012
  • For the application of photo-detector as active layer, we have studied how to deposit SiGe thin film using an independent Si target and Ge target, respectively. Both targets were synthesized by purity of 99.999%. Plasma generators were generated by radio frequency (rf, 13.56 MHz) and direct current (dc) power. When Ge and Si targets were sputtered by dc and rf power, respectively, we could observe the growth of highly crystalline Ge thin film at the temperature of $400^{\circ}C$ from the result of raman spectroscopy and X-ray diffraction method. However, SiGe thin film did not deposit above method. Inversely, we changed target position like that Ge and Si targets were sputtered by rf and dc power, respectively. Although Ge crystalline growth without Si target sputtering deteriorated considerably, the growth of SiGe thin film was observed with increase of Si dc power. SiGe thin film was evaluated as microcrystalline phase which included (111) and (220) plane by X-ray diffraction method.

Effects of Manganese Precursors on MnOx/TiO2 for Low-Temperature SCR of NOx (NOx제거용 MnOx-TiO2 계 저온형SCR 촉매의 Mn전구체에 따른 영향)

  • Kim, Janghoon;Shin, Byeong kil;Yoon, Sang hyeon;Lee, Hee soo;Lim, Hyung mi;Jeong, Yongkeun
    • Korean Journal of Metals and Materials
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    • v.50 no.3
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    • pp.201-205
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    • 2012
  • The effects of various manganese precursors for the low-temperature selective catalytic reduction (SCR) of $NO_x$ were investigated in terms of structural, morphological, and physico-chemical analyses. $MnO_x/TiO_2$ catalysts were prepared from three different precursors, manganese nitrate, manganese acetate(II), and manganese acetate(III), by the sol-gel method. The manganese acetate(III)-$MnO_x/TiO_2$ catalyst tended to suppress the phase transition from the anatase structure to the rutile or the brookite after calcination at $500^{\circ}C$ for 2 h. It also had a high specific surface area, which was caused by a smaller particle size and more uniform distribution than the others. The change of catalytic acid sites was confirmed by Raman and FT-IR spectroscopy and the manganese acetate(III)-$MnO_x/TiO_2$ had the strongest Lewis acid sites among them. The highest de-NOx efficiency and structural stability were achieved by using the manganese cetate(III) as a precursor, because of its high specific surface area, a large amount of anatase $TiO_2$, and the strong catalytic acidity.

Structural Changes and Dielectric Properties of$Pb(Mg_{1}{3}Nb_{2}{3})O_3$Ceramics Substituted by$Na^+/La^{3+}$Ions ($Na^+/La^{3+}$이온으로 치환된$Pb(Mg_{1}{3}Nb_{2}{3})O_3$의 구조 변화 및 유전 성질)

  • Hong, Young-Sik;Park, Hyu-Bum;Ahn, Tae-Ho;Kim, Si-Joong
    • Journal of the Korean Chemical Society
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    • v.40 no.9
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    • pp.607-614
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    • 1996
  • The structural changes and dielectric properties of Pb1-x(Na1/2La1/2)x(Mg1/3Nb2/3)O3 compounds substituted by 0∼50 mol.% of Na+/La3+ mixed ions were investigated by X-ray diffraction method, IR and Raman spectroscopy, and LCR meter. The amount of perovskite phase increased with the increases of Na+/La3+ substituents and sintering temperatures. Although the superlattice lines due to 1:1 ordering were not detected by X-ray diffraction method, it was found, from the Raman spectroscopy and the increase of diffuseness coefficient, that the ordering behavior was related to the decrease of A site ion size. Dielectric properties in Pb1-x(Na1/2La1/2)x(Mg1/3Nb2/3)O3 were affected by the amount of perovskite phase, grain size, and density. The phase transitions were broadened and phase transition temperatures were lowered by the increase of Na+/La3+ ions.

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Characterization of Vanadium Oxide Supported on Zirconia and Modified with MoO3

  • Sohn, Jong-Rack;Seo, Ki-Cheol;Pae, Young-Il
    • Bulletin of the Korean Chemical Society
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    • v.24 no.3
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    • pp.311-317
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    • 2003
  • Vanadium oxides supported on zirconia and modified with MoO₃were prepared by adding Zr(OH)₄powder into a mixed aqueous solution of ammonium metavanadate and ammonium molybdate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using FTIR, Raman spectroscopy and solid-state $^{51}V$ NMR. In the case of a calcination temperature of 773 K, for samples containing low loading of $V_2O_5$, below 15 wt %, vanadium oxide was in a highly dispersed state, while for samples containing high loading of $V_2O_5$, equal to or above 15 wt %, vanadium oxide was well crystallized because the $V_2O_5$ loading exceeded the formation of a monolayer on the surface of $ZrO_2$. The $ZrV_2O_7$ compound was formed through the reaction of $V_2O_5\;and\;ZrO_2$ at 873 K and the compound decomposed into $V_2O_5\;and\;ZrO_2$ at 1073 K, which were confirmed by FTIR spectroscopy and solid-state $^{51}V$ NMR. IR spectroscopic studies of ammonia adsorbed on $V_2O_5-MoO_3/ZrO_2$ showed the presence of both Lewis and Bronsted acids.

Pulsed laser ablation of hydroxyapatite in ethanol

  • Lee, Jung-Il;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.5
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    • pp.219-223
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    • 2014
  • Pulsed laser ablation in liquid medium was successfully employed to synthesize hydroxyapatite colloidal nanoparticles. The crystalline phase, particle morphology, size distribution and microstructure of the hydroxyapatite nanoparticles were investigated in detail. The obtained hydroxyapatite nanoparticles had spherical shape with sizes ranging from 5 to 20 nm. The laser ablation and the nanoparticle forming process were discussed with explosive ejection mechanism by investigating change of surface morphology on target. The analytical results of XPS, FT-IR and Raman spectroscopy confirms that the stoichiometry and bonding properties of the hydroxyapatite nanoparticles are in good agreement with reported bulk hydroxyapatite materials.

Crystal Structure and Characterization of a New Eight Coordinated Cadmium Complex

  • Hakimi, Mohammad;Moeini, Keyvan;Mardani, Zahra;Khorrami, Farzaneh
    • Journal of the Korean Chemical Society
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    • v.57 no.3
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    • pp.352-356
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    • 2013
  • In this work, a new cadmium complex $[Cd(L)(CH_3COO)_2].2H_2O$ (1) with the ligand L, N,N'-bis(2-pyridinecarboxalidene)-1,2-cyclohexanediamine was prepared and identified by elemental analysis, FT-IR, Raman, $^1H$ NMR spectroscopy and single-crystal X-ray diffraction. The cadmium atom in the crystal structure of 1 has distorted triangular dodecahedral geometry by coordination of the four nitrogen atoms of L and four oxygen atoms of the two acetate ions. Two water molecules are also incorporated in the crystal network. The $O-H{\cdots}O$ hydrogen bonds present in the crystal structure of 1. In this work, three structural surveys including coordination numbers of the cadmium atom, coordination modes of L and resonance in pyridine-2-ylmethanimine-based compounds are presented.

Study on the fabrication of DLC thin films by pulsed laser deposition (펄스 레이저 증착법에 의한 DLC 박막 제작 연구)

  • Jeong, young-Sik;Eun, Dong-Seog;Lee, Sang-Yeol;Jung, Hae-Suk;Park, Hung-Ho
    • Proceedings of the KIEE Conference
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    • 1997.11a
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    • pp.285-287
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    • 1997
  • We have deposited hydrogen-free diamond-like carbon (DLC) films by pulsed laser deposition of graphite. Pulsed laser deposition (PLD) can be utilized to generate films with desired properties quite different from those of the starting material. Since DLC films grown by PLD using turbo pump are perpared without hydrogen, they have a higher density and a higher index of refraction than the hydrogenated DLC films. In this study, effects of the substrate temperature and laser energy density on the properties of DLC films were systematically investigated. The structure and properties of the films have been studied by scanning electron microscopy (SEM), Fourier Transform Infrared (FT-IR), X-ray diffraction (XRD), and Raman spectroscopy.

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Effects of hydrogen gas on the properties of DLC films deposited by plasma CVD (Plasma CVD에 의한 DLC 박막 제작시 수소가스의 영향)

  • Moon, Yang-Sik;Lee, Jai-Sung;Lee, Hae-Sung;Lee, Jae-Yup;Park, Jin-Seok
    • Proceedings of the KIEE Conference
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    • 1996.07c
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    • pp.1532-1535
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    • 1996
  • Diamond-like carbon (DLC) films have been prepared by a widely-used plasma CVD with an rf (13.56MHz) plasma of $CH_4$ gas. The hydrogen incorporated in DLC films plays an important role of determining the film properties, but its exact role has not been clear. In this study, the effect of hydrogen on the film properties of DLC has been examined by adding the hydrogen gas to the $CH_4$ gas during deposition and by exposing the prepared film to the hydrogen plasma. As the content of additive hydrogen gas increases, the density and hardness of the film increase, but the growth rate decreases. The FT-IR spectroscopy results show that the number of C-H bonds decreases with increasing the hydrogen gas. Also, the variation in the position of "G" and "D" peaks due to additive hydrogen, which has been measured by the Raman spectroscopy, indicates of $sp^3$ fraction.

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