• Title/Summary/Keyword: X-선 구조분석

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Spin-Flop of α-Fe2O3 Nano Particles (α-Fe2O3 나노 입자에서 Spin-Flop에 관한 연구)

  • Sur, Jung-Chul;Park, Chul-Jin;Choi, Jung-Wan;Gee, S.H.;Hong, Y.K.
    • Journal of the Korean Magnetics Society
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    • v.14 no.5
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    • pp.169-173
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    • 2004
  • We have synthesized monodispersed $\alpha$-F $e_2$ $O_3$ nano particles to investigate the spin change during the Morin transition temperature( $T_{M}$). The particle size was founded to have a very uniform distribution of 80 nm by x-ray diffraction and size dispersion analyzer. The Mossbauer spectra between the 4.2 K and the room temperature show that $T_{M}$ was shifted and the spin states of Fe ion were changed with the particle size. The Morin transition temperature of bulk usually quoted in literature is 265 K but, it decreases with the size and no transition was found at the critical size down to 4.2K. The spin direction of 80 nm sized particles are normal to the hexagonal c-axis above the $T_{M}$ and are tilted about 28~29$^{\circ}$ below $T_{M}$, which is the [110] direction of rombohedral structure.

Preparation and Performance Evaluation of Zinc Phosphate-Coated Mica Anticorrrosive Pigment (운모상에 인산아연이 도포된 방청안료의 제조 및 성능평가)

  • Lee, Yu Jin;Park, Seong Soo;Hong, Seong Soo;Lee, Seung Ho;Kim, Dae Sung;Lee, Gun Dae
    • Clean Technology
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    • v.19 no.3
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    • pp.257-263
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    • 2013
  • The zinc phosphate-coated mica (ZP/mica) pigments were prepared using phosphoric acid, zinc nitrate and mica as starting materials, and used as anticorrosive pigments. The scanning electron microscopy (SEM) and x-ray diffraction (XRD) techniques were used to observe the morphology and crystal structure of prepared pigments. The prepared pigments were incorporated into an epoxy binder to prepare coating and the corrosion inhibition performance of the pigments was evaluated using electrochemical impedance spectroscopy (EIS). It was found that the anticorrosive performance of the ZP/mica pigment prepared at $70^{\circ}C$ was the better than that prepared at $20^{\circ}C$. The formation of ZnO, in addition to $Zn_3(PO_4)_2{\cdot}2H_2O$, was observed on ZP/mica pigment prepared at $70^{\circ}C$. The excellent anticorrosive performance of ZP/mica pigment could be ascribed to the synergistic effect with electrochemical anticorrosive mechanism from zinc compounds on mica and barrier anticorrosive mechanism from lamellar mica.

Preparation and Characterization of Plasticized Poly(vinyl chloride)-g-Poly(oxyethylene methacrylate) Graft Copolymer Electrolyte Membranes (가소화된 Poly(vinyl chloride)-g-Poly(oxyethylene methacrylate) 가지형 고분자 전해질막 제조 및 분석)

  • Seo, Jin-Ah;Koh, Jong-Kwan;Koh, Joo-Hwan;Kim, Jong-Hak
    • Membrane Journal
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    • v.21 no.3
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    • pp.222-228
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    • 2011
  • Poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) graft copolymer was synthesized via atom transfer radical polymerization (ATRP) and used as an electrolyte for electrochromic device. Plasticized polymer electrolytes were prepared by the introduction of propylene carbonate (PC)/ethylene carbonate (EC) mixture as a plasticizer. The effect of salt was systematically investigated using lithium tetrafluoroborate ($LiBF_4$), lithium perchlorate ($LiClO_4$), lithium iodide (LiI) and lithium bistrifluoromethanesulfonimide (LiTFSI). Wide angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) measurements showed that the structure and glass transition temperature ($T_g$) of polymer electrolytes were changed due to the coordinative interactions between the ether oxygens of POEM and the lithium salts, as supported by FT-IR spectroscopy. Transmission electron microscopy (TEM) showed that the microphase-separated structure of PVC-g-POEM was not greatly disrupted by the introduction of PC/EC and lithium salt. The plasticized polymer electrolyte was applied to the electrochromic device employing poly(3-hexylthiophene) (P3HT) conducting polymer.

Mechanical Properties and Reaction Products of Activated Slag System Depending on Gypsum Presence and Calcium Carbonate Addition (석고 존재 및 탄산칼슘 첨가에 따른 활성 슬래그의 역학적 성능 및 반응생성물)

  • Jeong, Yeonung;Lim, Gwi Hwan;Park, Su Hyeon;Kim, Joo Hyung;Kim, Tae-Sang
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.24 no.4
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    • pp.55-63
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    • 2020
  • This study investigates the mechanical properties and reaction products of activated slag pastes depending on gypsum presence and calcium carbonate addition in terms of compressive strength tests and synchrotron X-ray diffraction. The chemicals of CaO and NaOH are used as activators with different two dosages. The reaction of CaO-activated slag without gypsum just accelerated by addition of calcium carbonate at early ages, but no improvement was observed at later ages. On the other hand, the mechanical properties of CaO-activated slag pastes with gypsum were improved with calcium carbonate, enhancing the stability of ettringite. The variation of mechanical properties of NaOH-activated slag pastes was negligible depending on calcium carbonate addition in case of no gypsum. The addition of calcium carbonate into NaOH-activated slag pastes with gypsum deteriorated its mechanical properties due to the ion competition between CO32- ions and SO32- ions, decreasing crystallinity of reaction products.

Surface Modification of Ba0.6Sr0.4TiO3 by Trimethylsilyl Chloride as a Silylation Agent (Trimethylsilyl Chloride를 Silylation Agent로 사용한 Ba0.6Sr0.4TiO3 나노입자의 표면개질 연구)

  • Lee, Chan;Han, Wooje;Park, Hyung-Ho
    • Journal of the Microelectronics and Packaging Society
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    • v.26 no.4
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    • pp.127-132
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    • 2019
  • In this study, barium strontium titanate (BSTO) with high dielectric perovskite structure was synthesized by liquid-solid solution synthesis and the surface was modified using trimethylsilyl chloride (TMCS) as a silylation agent. Silylation surface modification is a method of reacting -OH ligand on the surface of BSTO nanoparticles with Cl in TMCS to generate HCl and replacing the ligand on the surface of nanoparticles with -Si, -CH3. Silylation was optimized by varying the concentration of TMCS, and the structure of the silicon network was confirmed by Fourier-transform infrared spectroscopy. In addition, the crystallinity of BSTO nanoparticles was confirmed by X-ray diffractometer and the size of the nanoparticles was calculated using Scherrer equation. The field emission scanning electron microscopic image observed the change of the surface-modified BSTO particle size, and the contact angle measurement confirmed the hydrophobic property of the contact angle of 120.9° in the optimized nanoparticles. Finally, the surface-modified BSTO dispersion experiment in de-ionized water confirmed the hydrophobic degree of the nanoparticles.

Rheological Properties and Foaming Behaviors of Modified PP/Nano-filler Composites (개질 폴리프로필렌/나노필러 복합체의 유변학적 특성 및 발포거동)

  • Yoon, Kyung Hwa;Lee, Jong Won;Kim, Youn Cheol
    • Polymer(Korea)
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    • v.37 no.4
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    • pp.494-499
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    • 2013
  • Modified polypropylene (m-PP) was fabricated by furfuryl sulphide (FS) as branching agent and m-PP/nano-filler composites were prepared with silicate and multi-walled carbon nanotube (MWCNT), using a twin screw extruder. The chemical structures and thermal properties of the m-PP were investigated by FTIR and DSC. The chemical structure of the m-PP was confirmed by the existence of =C-H stretching peak of the branching agent at 3100 $cm^{-1}$. There was no district change in melting temperature in case of m-PP, but a certain increase in crystallization temperature was notified and the increase was in the range of $10-20^{\circ}C$. The rheological properties, filler dispersion and foaming behaviors of the m-PP/nano-filler composites were investigated by dynamic rheometer, X-ray diffractometer (XRD) and scanning/transmission electron microscope (SEM/TEM). m-PP/nano-filler composites showed a high complex viscosity at a low frequency, an increase in melt elasticity, and a high shear thinning effect. Compared to pure PP, m-PP and m-PP/nano-filler composites were sufficient to enhance the foaming behavior.

The Role of Acid in the Synthesis of Red-Emitting Carbon Dots (장파장 형광 탄소 양자점 제조에 있어서 산의 역할에 대한 연구)

  • Yun, Sohee;Lee, Jinhee;Choi, Jin-sil
    • Applied Chemistry for Engineering
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    • v.33 no.3
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    • pp.309-314
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    • 2022
  • Carbon dots (CDs) are few nanometer-sized carbon-based nanoparticles and emerging candidate materials in various fields such as biosensors and bioimaging due to their excellent optical properties and high biocompatibility. However, most CDs, emitting blue light, have limited their application in biomedical fields due to the low penetration of short-wavelength lights into the biological system. Therefore, there has been enormous need to develop long-wavelength emitting CDs. In this study, red-emitting CDs were successfully synthesized through the hydrothermal reaction of p-phenylenediamine with hydrochloric acid. In addition, the effect of the amount of hydrochloric acid on the formation of carbon dots, resulting in the variation of the chemical structures of CDs, were investigated, which was confirmed with the intensive structural analyses using infrared and X-ray photoelectron spectroscopy. It was found that the chemical structure of CDs governed their optical properties and quantum yield. Therefore, this study provides an insight into the role of acid in forming red-emitting CDs as the optimal probe for biomedical application.

반극성 (11-22)n형 GaN의 실리콘 도핑농도 증가에 따른 결함감소와 이에 따른 반극성(11-22) GaN계 LED소자의 특성향상에 대한 연구

  • Lee, Jae-Hwan;Han, Sang-Hyeon;Song, Gi-Ryong;Lee, Seong-Nam
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.308.2-308.2
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    • 2014
  • 최근 III-N계 물질 기반의 광 반도체 중 m-면 사파이어 기판을 사용하여 반극성 (11-22) GaN박막을 성장하는 광반도체의 발광효율을 높이려는 연구가 많이 진행되고 있다. 하지만, 반극성 (11-22) GaN와 m-면 사파이어 기판과의 큰 격자상수 차이와 결정학적 이방성의 차이에 의해 많은 결정 결함이 발생하게 된다. 이러한 결정결함들은 반극성 LED소자내에서 누설전류 및 비발광 재결합, 순방향전압 등의 소자특성을 저하시키는 큰 요인이 되기 때문에 고효율 발광소자를 제작함에 있어 어려움을 야기시킨다. 이러한, 반극성 LED 소자의 효율 향상을 위해 결함 분석에 대한 연구를 주를 이루고 있는 상황으로, n-GaN층에 Si도핑에 관한 연구가 진행되고 있다. 이미 극성과 비극성에서는 n-GaN층에 Si이 도핑이 증가될수록 결정질이 향상되고, 양자우물의 계면의 질도 향상 되었다는 보고가 있다. 본 연구에서는 반극성 (11-22) GaN 기반의 발광소자를 제작함에 있어 n-GaN 층의 도핑 농도 변화를 통한 반극성 GaN 박막의 결정성 및 전기적 특성 변화에 따른 LED소자의 전계 발광 특성에 대한 연구를 진행하였다. 금속유기화학증착법을 이용하여 m-면 사파이어 기판에 $2.0{\mu}m$두께의 반극성 (11-22) GaN 박막을 저온 GaN완충층이 존재하지 않는 고온 1단계 성장법을 기반으로 성장하였다.[3] 이후, $2.0{\mu}m$ 반극성 (11-22) GaN 박막 위에 $3.5{\mu}m$ 두께의 n-GaN 층을 성장시켰다. 이때, n-형 도펀트로 SiH4 가스를 4.9, 9.8, 19.6, 39.2 sccm으로 변화하여 성장하였다. 이 4가지 반극성 (11-22) n-GaN 템플릿을 이용하여 동일 구조의 InGaN/GaN 다중양자우물구조와 p-GaN을 성장하여 LED 구조를 제작하였다. X-선 ${\omega}$-rocking curve를 분석한 결과, 이러한 특성은 반극성 (11-22) n-GaN층의 Si 도핑농도 증가에 따라서 각 (0002), (11-20), (10-10) 면에서 결정 결함이 감소하고, 반극성 (11-22) n형 GaN템플릿을 이용하여 성장된 반극성 GaN계 LED소자는 20mA인가 시 도핑 농도 증가에 따라 9.2 V에서 5.8 V로 전압이 감소하였으며 역방향 전류에서도 누설전류가 감소함이 확인되었다. 또한, 전계 발광세기도 증가하였는데, 이는 반극성 n형 GaN박막의 실리콘 도핑농도 증가에 따라 하부 GaN층의 결정성이 향상과 더불어 광학적 특성이 향상되고, n형 GaN층의 전자 농도 및 이동도의 동시 증가에 따라 전기적 특성이 향상 됨에 따라 LED소자의 전계 발광 특성이 향상된 것으로 판단된다.

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Synthesis and Characterization of Al-containing Titanium Silicalite-1 Catalysts (알루미늄 함유 티타늄 실리카라이트-1 촉매의 합성 및 특성 연구)

  • Ko, Yong Sig;Hong, Suk Bong;Kim, Geon Joong;Ahn, Wha Seung
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.639-647
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    • 1998
  • Al-containing titanium silicalite-1 ([Al]-TS-1) catalyst was prepared hydrothermally, and the effects of synthesis parameters such as silica/alumina sources, $SiO_2/TiO_2$ ratio, and aging treatment were investigated. The structure, crystal size, and shape were examined by XRD and SEM, and the extent of titanium incorporation into the zeolite framework was examined using UV-vis DRS spectroscopy. For [Al]-TS-1 catalyst preparation, aging of ca. 24h was essential, and the faster crystallization rates were achieved with Cab-O-Sil than with Ludox or TEOS as a silica source. In addition, the higher crystallinity and faster crystallization rate were obtained using sodium aluminate as an aluminum source. 2-butanol oxidation using $H_2O_2$ as an oxidant was carried out to confirm the redox property of the [Al]-TS-1. Acid sites catalyzed toluene alkylation study indicated that lattice titanium species in [Al]-TS-1 weakened the acid strength, and the para-ethyltoluene selectivity was enhanced as a results.

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Effects of Calcinations Temperature on the Electrochemical Properties of Li[Ni0.6Co0.2Mn0.2]O2 Lithium-ion Cathode Materials (리튬 이차전지용 양극활물질 Li[Ni0.6Co0.2Mn0.2]O2의 소성 온도가 전기화학적 특성에 미치는 영향)

  • Yoo, Gi-Won;Jeon, Hyo-Jin;Son, Jong-Tae
    • Journal of the Korean Electrochemical Society
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    • v.16 no.2
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    • pp.59-64
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    • 2013
  • Using $Na_2CO_3$ and $MeSO_4$ (Me = Ni, Co and Mn) as starting materials, the precursor of $[Ni_{0.6}Co_{0.2}Mn_{0.2}]CO_3$ has been synthesized by carbonate co-precipitation. The precursor was mixed with $Li_2CO_3$, and calcined at 750, 850, and$950^{\circ}C$ in air. Effect of calcinations temperature on characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ cathode materials was investigated. The structure and characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ were determined by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and electrochemical measurements. The X-ray diffraction (XRD) results show that the intensity ratio of $I_{(003)}/I_{(104)}$ increased and the R-factor ratio decreased with the increase of calcinations temperature. And Scanning electron microscopy (SEM) result show that the primary particle size increased. Especially, the $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ calcined at $950^{\circ}C$ for 24 H shows excellent electrochemical performances with reversible specific capacity of $165.3mAhg^{-1}$ [cut-off voltage 2.5~4.3 V, 0.1 C($17mAhg^{-1}$)] and good capacity retention of 95.4% after 50th charge/discharge cycles[cut-off voltage 2.5~4.3 V, 1 C($170mAhg^{-1}$)].