• 제목/요약/키워드: Solid-state NMR

검색결과 225건 처리시간 0.03초

The Organization of Nanoporous Structure Using Controlled Micelle Size from MPEG-b-PDLLA Block Copolymers

  • Chang, Jeong-Ho;Kim, Kyung-Ja;Shin, Young-Kook
    • Bulletin of the Korean Chemical Society
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    • 제25권3호
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    • pp.351-356
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    • 2004
  • Selected MPEG-b-PDLLA block copolymers have been synthesized by ring-opening polymerization with systematic variation of the chain lengths of the resident hydrophilic and hydrophobic blocks. The size and shape of the micelles that spontaneously form in solution are then controlled by the characteristics of the block copolymer template. All the materials prepared in this study showed the tunable pore size of 20-80 ${\AA}$ with the increase of hydrophobic chain lengths and up to 660 $m^2$/g of specific surface area. The formation mechanism of these nanoporous structures obtained by controlling the micelle size has been confirmed using both liquid and solid state $^{13}C\;and\;^{29}Si$ NMR techniques. This work verifies the formation mechanism of nanoporous structures in which the pore size and wall thickness are closely dependent on the size of hydrophobic cores and hydrophilic shells of the block copolymer templates.

Synthesis and Characterization of Cobalt(II)/(III), Nickel(II) and Copper(II) Complexes of New 14, 15 and 16-Membered Macrocyclic Ligands

  • El-Tabl, Abdou Saad
    • Bulletin of the Korean Chemical Society
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    • 제25권12호
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    • pp.1757-1763
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    • 2004
  • A new series of nickel(II), cobalt(II)/(III) and copper(II) complexes of 14, 15 and 16-membered of macrocyclic ligands have been prepared and characterized by elemental analyses, IR, UV-VIS and $^1H-NMR$ spectra, magnetic susceptibilities, conductivities, DTA and ESR measurements. Molar conductances in DMF solution indicate that, the complexes are nonelectrolytes except (9-12) complexes. The electronic spectra show that, all complexes are square planar or distorted octahedral geometry. The ESR spectra of solid complexes (4), (8) and (11) show square planar of axial type symmetry $(d_{x2-y2})$ with considerable covalent bond character. However, complex (12) shows a spectrum of octahedral geometry with $d_{z2}$ ground state. Complex (12) shows exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Carbon-Silica Membranes Derived from Polyimide/Silica Composites for Gas Separation

  • Lee, Young-Moo;Park, Ho-Bum;Kim, Myung-Jun;Jang, Jeong-Gyu
    • 한국막학회:학술대회논문집
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    • 한국막학회 2003년도 The 4th Korea-Italy Workshop
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    • pp.47-50
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    • 2003
  • Carbon-silica membranes were Prepared by Pyrolyzing polyimide/silica composite obtained from ill-situ polymerization of alkoxy silanes via sol-gel reaction. In this study, effects of silica content and silica network in polyimide matrix were focused on the gas permeation and separation properties of the final carbon-silica membrane. The membranes prepared were characterized with a field emission scanning electron microscopy (FE-SEM), a solid state $^{29}$ Si nuclear magnetic resonance spectroscopy ($^{29}$ Si-NMR), an electron spectroscopy for chemical analysis (ESCA), a thermogravimetric analysis (TGA) and gas permeation tests.

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Tailoring Molecular Precursors for Multicomponent Oxides

  • Hubert-Pfalzgraf, Liliane G.
    • The Korean Journal of Ceramics
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    • 제6권4호
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    • pp.370-379
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    • 2000
  • Simple ways to build up mixed-metal molecules which can act as potential single-source precursors to multimetallic oxides are reviewed. Emphasis is given to Lewis acid-base reactions between metal alkoxides M(OR)/sub n/, and between metal alkoxides and more accessible oxide precursors, carboxylates M(O₂CR)/sub n/ and β-diketonates M(β-dik)/sub n/. Characterization of the precursors is achieved in the solid state (single crystal X-ray diffraction, FT-IR) and by multinuclear NMR in solution. The reactions proceed toward the formation of aggregates in which the different metals display their usual coordinations numbers, often six for transition metals, as shown. Strategies for fixing the stoichiometry between the metals are developed. The reactivity of the MM species (dissociation, effects of chemical modifiers, of other metallic species, hydrolytic or non-hydrolytic condensation, etc.) will be indicated. Transformations into oxides are illustrated on precursors for titanates or niobates.

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Effect of V2O5 Modification in V2O5/TiO2-ZrO2 Catalysts on Their Surface Properties and Catalytic Activities for Acid Catalysis

  • Sohn, Jong-Rack;Lee, Cheul-Kyu
    • Bulletin of the Korean Chemical Society
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    • 제28권12호
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    • pp.2459-2465
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    • 2007
  • V2O5/TiO2-ZrO2 catalyst modified with V2O5 was prepared by adding Ti(OH)4-Zr(OH)4 powder into an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using XRD, DSC, solid-state 51V NMR, and FTIR. In the case of calcination temperature of 500 oC, for the catalysts containing low loading V2O5 below 25 wt % vanadium oxide was in a highly dispersed state, while for catalysts containing high loading V2O5 equal to or above 25 wt % vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2. The strong acid sites were formed through the bonding between dispersed V2O5 and TiO2-ZrO2. The larger the dispersed V2O5 amount, the higher both the acidity and catalytic activities for acid catalysis.

Endo- and Exo-Coordinated Mercury(II) Complexes of O3S2 Macrocycles: Effect of Dibenzo-Substituents on Coordination Mode

  • Lee, Ji-Eun;Kim, Hyun-Jee;Lee, So-Young;Lee, Jai-Young;Jin, Yong-Nu;Lee, Shim-Sung
    • Bulletin of the Korean Chemical Society
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    • 제28권11호
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    • pp.2041-2044
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    • 2007
  • The reactions of mercury(II) chloride with O3S2-donor macrocyclic ligands with (L1) and without (L2) dibenzosubunit afforded respective exo- (1) and endo-coordinated (2) complexes depending on the ring rigidity of the ligands. From the X-ray crystal structures and comparative NMR studies for the complexes 1 and 2, it is confirmed that the resulting species with different coordination modes exist not only in solid state but also in solution state.

전기적 활성을 갖는 폴리티오펜 유도체들의 합성과 생체계면에의 응용 (I) (Synthesis of Electroactive Polythiophene Derivatives and Its Application for Biointerface (I))

  • 정선형;배진영;김지흥;정동준
    • 폴리머
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    • 제26권1호
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    • pp.28-36
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    • 2002
  • 본 연구에서는 바이오칩 등에 응용 가능한 전도성 고분자 필름을 제조하기 위해 3-triophene acetic acid을 선택하여, 쉽게 전기적으로 산화되어 전기적 활성을 나타내는 고분자들을 형성하였다. 3-Thiophene acetic acid에 있는 카르복실기의 보호기들은 solid state에서 쉽게 제거되어질 수 있고, 그 결과 반응성 카르복실기가 전기적 활성을 나타내는 고분자 표면 위에 재생되어질 수 있었다. 즉, 카르복실기의 보호를 통한 전기중합과 뒤이은 보호기의 제거로 반응성인 카르복실기를 갖는 새로운 고분자 담체를 제조할 수 있었고, 기존의 방법으로 합성한 macromonomer를 필름 표면에 도입하여 전기적 활성을 나타내며 동시에 고분자 전해질이 도입된 전도성 고분자 필름을 얻었다. 합성한 전도성 단량체들과 macromonomer의 도입여부는 FT-IR과 $^1H-NMR$ 및 ESCA측정으로 확인하였고, 전극표면에 형성된 필름들의 형태는 SEM을 통해서 관찰하였다. 전기적 활성은 cyclic voltammogram(CV)을 통하여 확인하였으며, 얻어진 고분자 필름들은 0.7~0.9 V의 영역에서 전형적인 poly(3-alkylthiophene)의 전기 화학적 거동을 나타내었다.

Swallow-Tail Terrylene Bisimide 적색 유기 형광체 제조 및 특성 연구 (Preparation and Characterization of Swallow-Tail Terrylene Bisimide as Organic Phosphor)

  • 정성봉;정연태
    • 한국전기전자재료학회논문지
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    • 제33권3호
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    • pp.194-200
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    • 2020
  • Perylene bisimide derivatives are developed for red organic phosphor because of their advantages, such as excellent luminous efficiency and high thermal stability. Despite these advantages, they have poor solubility characteristics in organic solvents and short emission wavelength as red organic phosphor for hybrid light-emitting diodes (LEDs). In this study, we prepared terrylene bisimide using a coupling reaction and swallow-tail imide group, which has excellent solubility. The structures and properties of swallow-tail terrylene bisimide (9C) were analyzed using 1H-nuclear magnetic resonance (1H-NMR), Fourier-transform infrared (FT-IR), UV/Vis spectroscopy, and thermal gravimetric analysis (TGA). The maximum absorption wavelength of (9C) in the UV/Vis spectrum was 647 nm, and the maximum emission wavelength was 676 nm. In the TGA, (9C) demonstrated good thermal stability with less than 5 wt% weight loss up to 415℃. In the solubility test, (9C) has a good solubility of more than 5 wt% in chloroform and dichloromethane. When the compounds (9C) were mixed with PMMA (polymethly methacrylate), the films showed peaks at 680 nm in the PL spectra. The results verify the suitability of (9C) as a red organic phosphor for hybrid LEDs.

사성분계 비정질 Ca-Na 알루미노규산염의 산소주변의 원자구조 : O-17 고상핵자기 공명분광학분석 (Oxygen Sites in Quaternary Ca-Na Aluminosilicate Classes : O-17 Solid-State NMR Study)

  • 성소영;이성근
    • 한국광물학회지
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    • 제19권4호
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    • pp.347-353
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    • 2006
  • 자연계에 존재하는 다양한 지구물질의 조성은 여러 성분들로 구성된 다성분계이므로 자연계의 현상을 이해하기 위해서는 이러한 다성분계 지구물질의 구조를 규명하는 것이 필수적이다. 이러한 중요성에도 불구하고 다성분계 비정질의 자세한 원자-나노 구조는 비정질 자체가 갖고 있는 여러 가지고유의 무질서도 등으로 인하여 최근까지도 정확히 알려지지 않았다. 본 연구에서는 일차원 O-17 MAS와 이차원 3QMAS NMR을 이용하여, 다성분계 비정질인 Ca-Na 알루미노규산염 $[(CaO)_x(Na_2O)_{1-x}]\;(A1_2O_3)_{0.5}(SiO_2)_6.\;CNAS)$의 자세한 원자단위의 조성에 따른 변화를 보고한다. 비정질 CNAS의 비연결 산소 (non-bridging oxygen, NBO) 중 Ca-NBO는 Na/Ca 비율이 증가함에 따라서 (Ca, Na)-NBO를 형성한다. 이는 비정질 CNAS 내에서 비연결산소와 Ca와 Na 간에 강한 상호작용이 있음을 지시한다. 연결산소인 경우(bridging oxygen, BO, Si-O-Si나 Si-O-Al)의 경우에도 Na/Ca 비율에 따라, 감소의 폭이 비연결 산소보다는 상대적으로 작지만 화학차폐(NMR chemical shift)가 선형적으로 감소한다. 비정질 규산염의 연결산소의 결합각과 결합길이의 분포에 의해 결정되는 위상무질서도(topological disorder)는 Ca 함량이 증가할수록 비선형적으로 증가한다. 이러한 결과들은 비정질 CNAS의 구조가 기존에 알려진 데로 비연결산소만이 Na와 Ca 같은 구조교란양이온(network modifying cation)에 의해 많은 영향을 받는 것이 아니라 연결산소도 이들 양이온에 의하여 영향을 받음을 지시한다 이에 따라 다양한 양이온세기가 비정질의 무질서도에 미치는 영향을 정리하였다.

저밀도 폴리에틸렌의 결정화도에 대한 저온 열처리 효과: 수소 핵자기공명 연구 (Effect of Low-temperature Thermal Treatment on Degree of Crystallinity of a Low Density Polyethylene: $^{1}H$ Nuclear Magnetic Resonance Study)

  • 이창훈;최재곤
    • Elastomers and Composites
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    • 제43권4호
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    • pp.259-263
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    • 2008
  • 저밀도 폴리에틸렌에 대한 장시간 저온 열처리가 저밀도 폴리에틸렌 고분자의 결정화도에 미치는 효과를 고체 수소 핵자기공명을 이용하여 연구하였다. 장시간 열처리는 첫째, 저밀도 폴리에틸렌의 색깔을 엷은 노란색으로 변하게 하였고 둘째, 저밀도폴리에틸렌에서 수소 핵의 스핀-스핀 및 스핀-격자 완화시간을 증가시켰으며, 셋째, 결정화도를 줄어들게 하였다. 먼저, $T_1$의 증가를 저밀도폴리에틸렌의 전체 스핀-격자 완화시간을 결정하는 비정질 영역의 부피 감소에 의한 것이거나 분자간 가교나 수소결합에 의한 특정 분자 운동 성분의 느려짐에 의해 발생하는 것으로 고려하였다. 하지만 결정화도의 감소는 열처리에 의한 비정질 영역의 감소를 의미하므로 전자와는 배치되었다. 따라서 $T_1$의 증가는 후자에 의한 결과임을 알 수 있었다.