• Title/Summary/Keyword: Zirconyl

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The Environmental Control of $Er^{3+}$ ions in $R-SiO_2/ZrO_2$ Sol-Gel Matrix ($R-SiO_2/ZrO_2$ 졸-겔 재료내 $Er^{3+}$이온의 결합 환경 제어)

  • 김주현;권정오;석상일;안복엽
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.224-224
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    • 2003
  • 광통신을 위한 구성 요소는 빛을 발생시키는 발광소자, 빛을 검출하는 수광소자 그리고 광신호를 처리하는 광신호처리 소자로 구성된다. 이때 각 소자간 광전송과 광소자에 의한 광 신호 처리 과정에서 광전송 손실이 심각하게 일어나 광정보를 상실하게 되므로 각 요소별로 광신호 증폭이 반드시 필요하다. 뿐만 아니라 완전 광화에 의한 초고속/대용량 광통신망의 구축에는 저가이며, 광집적화가 가능한 광도파로형 광증폭기가 요구되고 있다. 짧은 거리에 높은 증폭 효율을 얻기 위한 광도파로형 광증폭기를 구현하기 위해서는 광통신 파장대인 1.55$\mu\textrm{m}$ 대역의 증폭이 가능한 Er 이온을 고농도로 도핑 할 필요가 있다. 그러나 Er 이온을 단순히 고농도로 첨가하면 Er-Er 간 뭉침 현상에 의해 더 이상의 증폭이 어렵게 된다. 본 연구에서는 이러한 문제를 해결하면서 스핀 코팅이 가능하여 저가 공정이 가능한 유/무기 졸-겔 재료 내에 Er 이온을 제어된 방법으로 첨가하고 그 결합 환경을 FT-IR 및 $^{17}$ O-NMR로 분석하였다. 유/무기 졸겔 재료 제조를 위하여 먼저 MPTS(MethAcryoxyPropylTrimethoxySilane)를 부분 가수분해한 후 ZrOCl$_2$.8$_2$O (Zirconyl Chloride Octahydrate) 와 ErCl$_3$. 6$H_2O$ (Erbium(III) Chloride Hexahydrate)를 순차적으로 결합시키고, Zr/MPTS 및 Zr/Er의 첨가비에 따른 발광 특성을 PL(photoluminescence) 스팩트럼으로 분석하여 Er 이온의 주위 결합 환경이 PL에 미치는 영향을 조사하였다. 또한 Si 기판에 코팅한 Er이 도핑된 유/무기 하이브리드 졸-겔 코팅막의 굴절율 등 광도파로 재료로서의 특성도 프리즘 커플러 등을 이용하여 조사하였다.

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Encapsulation and optical properties of Er3+ ions for planar optical amplifiers via sol-gel process (졸-겔법을 이용한 광증폭기의 Er 이온 캡슐화 및 광학적 특성)

  • Kim, Joo-Hyeun;Seok, Sang-Il;Ahn, Bok-Yeop
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.11a
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    • pp.135-135
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    • 2003
  • The fast evolution in the fold of optical communication systems demands powerful optical information treatment. These functions can be performed by integrated optical systems. A key component of such systems is erbium doped waveguide amplifier(EDWA). The intra 4f radiative transition of Er at 1.5 $\mu\textrm{m}$ is particularly interesting because this wavelength is standard in optical telecommunications. The fabrication of waveguide amplifier for integrated optics using sol-gel process has received an increasing attention. Potential advantage of lower cost by less capital equipment and easy processing makes this process an attractive alternatives to conventional technologies like flame hydrolysis deposition, ion exchange and chemical vapor deposition, etc. In addition, sol-gel process has been found to be extremely suitable for the control of composition and refractive index related directly with optical properties. The main drawback of such an amplifier with respect to the EDWA is the need for a much higher Er3+ concentration to compensate for the smaller interaction length. However, the high doping of Er might be resulted in the non-radiative relaxation by clustering of Er ions End co-operative upconversion. In order to solve this problem, we investigate the possibility of avoiding short Er-Er distances by encapsulation of Er3+ ions in hosts such as organic-inorganic hybrid materials. For inorganic-organic hybrid sols, methacryloxypropyltrimethoxysilane (MPTS), zirconyl chloride octahydrate and erbium(III) chloride hexahydrate were used as starting materials, followed by conventional sol-gel process. It was observed by TEM that nano sols having core/shell toplology were formed, depending on the mole ratio of Zr/Er. The surface roughness for the coatings on Si substrate was investigated by AFM as a function of Zr/Er ratio. The local environment and vibrational Properties of Er3+ ions were studied using Near-IR, FT-IR, and UV/Vis spectroscopy. Nano hybrid coatings derived from polymer and Er doped encapsulation Eave the good luminescence at 1.55$\mu\textrm{m}$.

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Hydrothermal Synthesis and Mechanical Characterization of 3mol%Y2O3-ZrO2 by Urea Contents (우레아 첨가량 변화에 따라 수열합성법으로 제조 된 3mol%Y2O3-ZrO2 분말의 합성 및 기계적 특성 평가)

  • Lee, Hak-Joo;Go, Myung-Won;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.425-431
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    • 2011
  • The industrial manufacturing of YSZ products can be summarized as a three step process: a) hydrolysis of zirconyl chloride and mixing of other solutions, b) precipitation, and c) calcination. The addition of ammonia or OH- is essential in the precipitation process. However, a strong agglomeration was observed in the results of an ammonia or OH- addition. Thus, it is necessary to disperse the powders smoothly in order to improve the mechanical strength of YSZ. In this study, YSZ was synthesized using the urea stabilizer and hydrothermal method. YSZ powders were synthesized using a hydrothermal method with Teflon Vessels at $180^{\circ}C$ for 24 h. The mole ratio of urea to Zr was 0, 0.5, 1, and 2. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens ($33\;mm{\times}8\;mm{\times}1{\pm}0.5\;mm$) for three-point bend tests were used in the mechanical properties evaluation. The crystalline of YSZ powders observed a tetragonal phase in the sample with a ratio of Zr:urea = 1:2 addition and a hydrothermal reaction time of 24 h. The average primary particle size of YSZ was measured to be 9 nm to 11 nm. The agglomerated particle size was measured from 15 nm to 30 nm. The three-point bending strength of the YSZ samples was 142.47 MPa, which is the highest value obtained for the Zr:urea = 1:2 ratio addition YSZ sample.

Synthesis, Spectroscopic, and Biological Studies of Chromium(III), Manganese(II), Iron(III), Cobalt(II), Nickel(II), Copper(II), Ruthenium(III), and Zirconyl(II) Complexes of N1,N2-Bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)propyl)phthalamide (N1,N2-bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)propyl)phthalamide의 크롬(III), 망간(II), 철(III), 코발트(II), 니켈(II), 구리(II), 루테늄(III) 및 산화 지르코늄(II) 착물에 대한 합성과 분광학 및 생물학적 연구)

  • Al-Hakimi, Ahmed N.;Shakdofa, Mohamad M.E.;El-Seidy, Ahemd M.A.;El-Tabl, Abdou S.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.418-429
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    • 2011
  • Novel chromium(III), manganese(II), iron(III), cobalt(II), nickel(II), copper(II), ruthenium(III), and zirconyl(II) complexes of $N^1,N^2$-bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)propyl)phthalamide ($H_4L$, 1) have been synthesized and characterized by elemental, physical, and spectral analyses. The spectral data showed that the ligand behaves as either neutral tridentate ligand as in complexes 2-5 with the general formula $[H_4LMX_2(H_2O)]{\cdot}nH_2O$ (M=Cu(II), Ni(II), Co(II), X = Cl or $NO_3$), neutral hexadentate ligand as in complexes 10-12 with the general formula $[H_4LM_2Cl_6]{\cdot}nH_2O$ (M=Fe(III), Cr(III) or Ru(III)), or dibasic hexadentate ligand as in complexes 6-9 with the general formula $[H_2LM_2Cl_2(H_2O)_4]{\cdot}nH_2O$ (M = Cu(II), Ni(II), Co(II) or Mn(II), and 13 with general formula $[H_4L(ZrO)_2Cl_2]{\cdot}8H_2O$. Molar conductance in DMF solution indicated the non-ionic nature of the complexes. The ESR spectra of solid copper(II) complexes 2, 5, and 6 showed $g_{\parallel}$ >g> $g_e$, indicating distorted octahedral structure and the presence of the unpaired electron in the $N^1,N^2$ orbital with significant covalent bond character. For the dimeric copper(II) complex $[H_2LCu_2Cl_2(H_2O)_4]{\cdot}3H_2O$ (6), the distance between the two copper centers was calculated using field zero splitting parameter for the parallel component that was estimated from the ESR spectrum. The antibacterial and antifungal activities of the compounds showed that, some of metal complexes exhibited a greater inhibitory effect than standard drug as tetracycline (bacteria) and Amphotricene B (fungi).

The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-propanol (이소프로판올의 탈수반응에서 지르코니아 촉매의 결정상에 따른 영향)

  • Sim, Hye-In;Park, Jung-Hyun;Cho, Jun Hee;Ahn, Ji-Hye;Choi, Min-Seok;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.208-213
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    • 2013
  • Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

Synthesis and Characterization of Homobinuclear Complexes of UO2(VI), ZrO(IV) and Th(IV) ions with 3-Benzylidine/Furfurylidine/(Pyridyl/Thienyl-2'-methylene) imino-5-p-sulphonamido phenyl azo-2-thiohydantoins (3-Benzylidine/Furfurylidine/(Pyridyl/Thienyl-2'-methylene) imino-5-p-sulphonamido phenyl azo-2-thiohydantoins와 UO2(VI), ZrO(IV) 및 Th(IV) 이온의 동종이핵 착물에 대한 합성 및 특성)

  • Dash, D.C.;Mahapatra, A.;Naik, P.;Mohapatra, R.K.;Naik, S.K.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.412-417
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    • 2011
  • A series of homobinuclear complexes of the type [$M_2L(NO_3)_n(H_2O)_m$] where M=$UO_2$(VI), ZrO(IV), Th(IV); L=3-benzylidine-imino-5-p-sulphonamido phenyl azo-2-thiohyatoin(bispt), 3-furfurylidine-imino-5-p-sulphonamido phenyl azo-2-thiohydantoin(fispt),3-pyridyl-2'-methylene-imino-5-p-sulphonamido phenyl azo-2-thiohydantoin(pmispt) and 3-thienyl-2'-methylene-imino-5-p-sulphoanamido phenyl azo-2-thiohydantoin(tmispt); n=8 for Th(IV) and 4 for others, m=4 for bispt and 3 for others have been synthesized and characterized on the basis of elemental analysis, thermal analysis, molar conductance, magnetic moment and spectroscopic data (IR, electronic and $^1H$-NMR). In the light of this information, the ligands can be visualized as tetradentate co-ordinating through azomethine nitrogen, carbonyl oxygen to one metal centre where as azo nitrogen and thioimido nitrogen to the other metal centre yielding homo binuclear complexes of the above composition. The fungi toxicity of the ligands & their zirconyl complexes against some fungal pathogen has been studied.

Fabrication of high purified zirconium dioxide (ZrO2) and stabilized zirconia (TZP: tetragonal zirconia polycrystal) powders (고순도 산화지르코늄(ZrO2) 및 안정화 지르코니아 (TZP: tetragonal zirconia polycrystal) 분말제조)

  • 최의석
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.55-85
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    • 1996
  • 지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.

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