• Title/Summary/Keyword: 단일상 합성법

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Crystallographic and Mossbauer Studies of Magnetic Garnet $Y_{3-x}Bi_xFe_5O_{12}$ by a Sol-Gel Method (Sol-gel 합성에 의한 자성 garnet $Y_{3-x}Bi_xFe_5O_{12}$의 결정학적 및 Mossbauer 분광학 연구)

  • 엄영란;김철성;이재광
    • Journal of the Korean Magnetics Society
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    • v.8 no.4
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    • pp.203-209
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    • 1998
  • Crystallographic and magnetic properties of single phase garnet $Y_{3-x}Bi_xFe_5O_{12}$ (x=0.0, 0.25, 0.5, 0.75, 1.0) were studied by using x-ray diffraction, Mossbauer spectroscopy and vibrating sample magnetometer (VSM). Ultra-fine polycrystalline cubic samples have been prepared by sol-gel method. The lattice constant increase linearly with increasing an amount of Bi. Annealing temperature was larger than 800 $^{\circ}C$ for the growth of a single-phase garnet powder. The second phase of garnet, $(BiFeO_3)$, was at 1000 $^{\circ}C$ for x=0.75, and 950 $^{\circ}C$ for x=1.00. From Mossbauer spectroscopy and VSM measurements, the magnetization and the coercivity were decreased and the Curie temperature $Y_{3-x}Bi_xFe_5O_{12}$(x=0.0, 0.25, 0.5, 0.75, 1.0) was slightly increased as increasing the Bi content.

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Magnetic Properties of Fe4N Nanoparticles and Magnetic Fe17Sm2Nx Powders (Fe4N 나노분말과 Fe17Sm2Nx 자성분말의 자기적 특성)

  • Oh, Young-Woo;Lee, Jung-Goo;Park, Sang-Jun
    • Journal of the Korean Magnetics Society
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    • v.22 no.3
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    • pp.79-84
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    • 2012
  • Nano-magnetic materials such as iron-nitrides have been actively studied as an alternative to the application of high density, high performance needs for next generation information storage and also alternative to the rare earth and neodymium magnet. $Fe_4N$ is the basic materials for magnetic storage media and is one of the important magnetic materials in focus because of its higher magnetic recording density and chemical stability. Single phase ${\gamma}^{\prime}-Fe_4N$ nanoparticles have been prepared by a PAD (Plasma Arc Discharge) method and nitriding in a $NH_3-H_2$ mixed gases at temperature, $400^{\circ}C$ for 4 hrs. Also $Fe_{17}Sm_2N_x$ powders were synthesized by nitriding after reduction/diffusion of $Fe_{17}Sm_2$ to compare the magnetic properties with nano-sized $Fe_4N$ particles. The saturation magnetization of $Fe_4N$ and $Fe_{17}Sm_2N_x$ were 149 and 117 emu/g, respectively, but the coercive force was considerably smaller than that of bulk or acicular $Fe_4N$.

Effects of Metal Ion Mole Ratio and Calcination Temperatures on Magnetic Properties and Microstructure of Ba2Co2Fe12O22 Powders Synthesized by Solid State Reaction (고상반응법으로 제조된 Ba2Co2Fe12O22분말의 자기적 성질과 미세구조에 미치는 금속이온몰비와 열처리 온도의 영향)

  • Cho, Kwang-Muk;Nam, In-Tak
    • Journal of the Korean Magnetics Society
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    • v.19 no.6
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    • pp.216-221
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    • 2009
  • Y-type barium ferrite $Ba_2Co_2Fe_{12}O_{22}$ was synthesized by a solid state reaction method. Effects of metal ion mole ratio and calcination temperatures on magnetic properties and microstructures of the synthesized powders were investigated. Phase analysis and microstructure observation were performed with a XRD (X-ray diffractometer) and a FESEM (field effect scanning electron microscope), respectively. Magnetic properties of the powders were measured with a VSM (vibrating sample magnetometer). Single phase Y-type was synthesized when metal ion mole fraction $Fe^{3+}:\;Ba^{2+}:\;Co^{2+}$ was 6 : 1 : 1 and calcination temperature was $1050\;{^{\circ}C}$. High saturation magnetization value of 39.1 emu/g was obtained when metal ion mole fraction $Fe^{3+}:\;Ba^{2+}:\;Co^{2+}$ was 8 : 1 : 1 and calcination temperature was $1200\;{^{\circ}C}$.

Study on Phase Relation and Synthesis of Pyrochlore in the System of Ca-Ce-Zr-Ti-O (Ca-Ce-Zr-Ti-O System에서의 파이로클로어 합성 및 상관계에 대한 연구)

  • Chae Soo-Chun;Bae In-Kook;Jang Young-Nam;Yudintsev S.V.
    • Economic and Environmental Geology
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    • v.37 no.6 s.169
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    • pp.603-612
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    • 2004
  • Pyrochlore is known as one of the most promising materials for the immobilization of radionuclide in high level waste. This study included the synthesis, phase relation and characteristics of $pyrochlore(CaCeZr_xTi_{2-x}O_{7,\;x=0.2\~2.0)$ in the system of Ca-Ce-Zr-Ti-O. Using the CPS(Cold pressing and sintering) method, the mixtures of $CaCO3_,\;CeO_2,\;ZrO_2\;and\;TiO_2$ oxides were pressed, and sintered at $1100\~1600^{\circ}C$ for 20 hours. The optimal synthetic conditions at various compositions were differed from 1300 to $1600^{\circ}C$ Even in the optimal temperatures, pyrochlore or fluorite coexisted with minor amount of perovskite, $CeO_2\;or\;Ce_{0.75}Zr_{0.25}O_2$. It was confirmed that pyrochlore and fluorite structures were stable at $x\leq0.6\;and\;x\geq1.0$, respectively. Especially, the compositions of pyrochlore or fluorite showed non-stoichiometric compositions in that contents of Ca and Ti were more deficient and those of Zr and Ce were more excess than batch compositions with the increase of x value. These characteristics stemmed from the behavior of elements occupied at eight- and six-coordinated site, and then caused the coexistence of perovskite, $CeO_2\;or\;Ce_{0.75}Zr_{0.25}O_2$ along with pyrochlore or fluorite.

다양한 활성제 이온이 치환 고용된 MgNb2O6 형광체의 특성

  • Kim, Ji-Seon;Jo, Sin-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.167-167
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    • 2013
  • 최근에 산화물 형광체는 황화물 형광체에 비해 높은 화학적 안정성을 나타내기 때문에 백색 발광 다이오드, 전계방출 디스플레이와 플라즈마 디스플레이 패널에 그 응용성을 넓히고 있다. 마그네슘 니오베이트(magnesium niobate, MgNb2O6)는 우수한 유전 특성(상대 유전상수=18.4)을 나타내기 때문에 마이크로파 유전체로 응용 가능하며, 단일상 릴랙서 페라브스카이트(relaxor perovskite) Pb(Mg1/3Nb2/3)O3을 합성하기 위한 전구체 (precursor)로 널리 사용되고 있으며, 나이오븀산염 이온에서 다양한 색상을 방출하는 활성제 이온으로 효율적인 에너지 전달이 일어남으로써 Sm3+, Dy3+, Eu3+와 같은 희토류 이온의 좋은 모체 격자로 개발할 수 있다. 본 연구에서는 마그네슘 니오베이트 MgNb2O6 모체 결정에 다양한 활성제 이온, 즉 Eu3+, Sm3+, Dy3+, Tb3+를 선택적으로 주입하여 발광 효율이 높은 천연색 형광체를 합성하고자 한다. 특히, 모체 결정에 주입되는 활성제 이온 주위의 국소적인 환경이 반전 대칭에서 변형되는 척도를 조사하여 활성제의 주 발광 파장의 세기가 최대가 되는 최적의 조건을 결정하고자 한다. Mg1-1.5xNb2O6:REx3+ 형광체 분말 시료는 초기 물질 MgO, Nb2O5와 희토류 이온을 화학 반응식에 맞게 정밀 저울로 측량하여 플라스틱 용기에 ZrO2 볼과 함께 넣고, 소정의 에탄올을 채운 뒤 밀봉하고서, 300 rpm의 속도로 20시간 볼밀 (ball-mill) 작업을 수행하였다. 그 후, 체(sieve)로 ZrO2 볼을 걸러낸 다음에 혼합된 용액을 각 비커에 담아서 $40^{\circ}C$의 건조기에서 24시간 건조하였고, 건조된 시료를 막자 사발에 넣고 잘게 갈고 80 ${\mu}m$의 체로 걸러낸 후에, 알루미나 도가니에 활성제 이온별로 각각 담아, 전기로에 장입하여 매분당 $5^{\circ}C$의 비율로 온도를 상승시켜 $350^{\circ}C$에서 5시간 동안 하소 공정을 실시한 후에, 온도를 계속 일정한 율로 증가시켜 $1,200^{\circ}C$에서 5시간 동안 소성하여 합성하였다. 합성된 형광체 분말의 결정 구조는 $Cu-K{\alpha}$ 복사선(파장: 1.5406)을 사용하여 X-선회절장치로 측정하였으며, 형광체의 표면 형상은 전계형 주사전자현미경으로 관측하였다. 흡광와 발광스펙트럼은 제논 램프를 광원으로 갖는 형광 광도계를 사용하여 측정하였다. 모체 결정에 활성제 이온 Eu3+, Sm3+, Dy3+, Tb3+가 도핑된 형광체 분말은 각각 적색, 주황색, 황색, 녹색 발광이 관측되었다. 각 발광 스펙트럼과 결정 입자의 크기와 형상 사이의 상호 관계를 조사하였다. 실험 결과로부터, 각 형광체의 발광 파장은 활성제 이온의 종류 와 서로 밀접하게 관련되어 있으며, 형광체 시료 합성시 활성제 이온의 농도를 선택적으로 조절함으로써 발광의 세기를 제어할 수 있음을 확인하였다.

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Enhancing Production Rate of Emulsion via Parallelization of Flow-Focusing Generators (유동-집속 생성기의 병렬화를 통한 에멀젼 생산속도 향상)

  • Jeong, Heon-Ho
    • Korean Chemical Engineering Research
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    • v.56 no.5
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    • pp.761-766
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    • 2018
  • Droplet-based microfluidic device has led to transformational new approaches in various applications including materials synthesis and high-throughput screening. However, efforts are required to enhance the production rate to industrial scale because of low production rate in a single droplet generator. In here, we present a method for enhancing production rate of monodisperse droplets via parallelization of flow-focusing generators. For this, we fabricated a three-dimensional monolithic elastomer device (3D MED) that has the 3D channel structures in a single layer, using a double-sided imprinting method. We demonstrated that the production rate of monodisperse droplet is increased by controlling the flow rate of continuous and dispersed phases in 3D MED with 8 droplet generators. Thus, we anticipate that this microfluidic system will be used in wide area including microparticle synthesis and screening system via encapsulation of various materials and cells in monodisperse droplets.

Syntheses, Dielectric Properties and Ordering Structures of $Pb(Fe _{1/2}Ta_{1/2})O_3$ ($Pb(Fe _{1/2}Ta_{1/2})O_3$의 합성, 유전특성 및 질서배열구조)

  • 우병철;김병국;김병호
    • Korean Journal of Crystallography
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    • v.13 no.3_4
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    • pp.165-171
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    • 2002
  • Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$, ceramics were successfully synthesized from the powders prepared by solid state reaction (sintering temperature: $1100^{\circ}C$, density: $9.3g/cm^3$, average grain size: $5.1{\pm}1.2mm$, space group: Pm3m). Their dielectric properties measured at $-150{\sim}50^{\circ}C$ showed the maximum relative dielectric constant of 31000 at $-41^{\circ}C$. 1 kHz, and typical relaxor ferroelectrics characteristics such as diffuse phase transition and dielectric relaxation phenomena. However, the diffuseness of phase transition decreased and the dielectric properties became more normal ferroelectrics as the time of annealing at $1000^{\circ}C$ increased. By using Raman spectroscopy, it was revealed that the $Fe^{3+}$ and $Ta^{5+}$ ions in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, are stoichiometrically 1 : 1 ordered within the short-range that can not be probed even by transmission electron microscopy, and this stoichiometric 1 : 1 ordering is enhanced by the annealing. The relaxor ferroelectric characteristics in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, could be correlated with the stoichiometric 1 : 1 short-range ordering of B-site cations, and the decrease of relaxor ferroelectric characteristics in the annealed $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the enhanced stoichiometric 1 : 1 short-range ordering of B-site cations.

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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Mineral Products and Characteristics of Phase Transformation after Hydrothermal Treatment according to the Synthetic Method and Cation Combination during Birnessite Synthesis (버네사이트 합성 시 합성 방법 및 양이온 조건에 따른 생성 광물 및 열수처리 후 상전이 특성)

  • Min, Soyoung;Kim, Yeongkyoo
    • Economic and Environmental Geology
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    • v.52 no.6
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    • pp.509-517
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    • 2019
  • The birnessite (7Å manganate, δ-MnO2) which is a manganese oxide and comprises manganese nodules, is a major manganese mineral on the earth surface and a precursor in the synthesis of todorokite. In this study birnessite was synthesized by three different methods: Feng et al. (2004) and Luo et al. (1998) based on redox reaction and Ma et al. (1999) based on reduction reaction. 12 birnessite samples were synthesized by different combinations of Na+ and K+ cations based on the base (OH-) and permanganate (MnO4-) reagents in the synthesis. The mineral compositions of synthesized birnessite were identified by XRD, and the two cation ratio in the mineral was measured by ICP. The products obtained after hydrothermal treatment of Mg-buserite, by the precursor of birnessite, was examined by XRD, and then phase transition to todorokite and their characteristics were compared. Our results show that the byproducts and the characteristics of phase transition by each synthetic method have different trends. Hausmannite (γ-Mn3O4) and feitknechtite (β-MnOOH) were formed by both methods in the redox reaction mechanism. By Feng et al. (2004)'s method, manganite (γ-MnOOH) phase only appeared when cation was predominantly Na+. Two birnessite samples synthesized by redox reaction mechanism showed phase transition to todorokite (10Å manganate, OMS-1) when both NaOH and KMnO4 were used together. However, single-phase birnessite was formed by Ma et al. (1999)'s method, and phase transition was confirmed only for the sample when the cation was only composed of Na+.

Comparison of Oligosaccharyltransferase Assay Methods Using a Fluorescent Peptide (형광펩타이드를 이용한 Oligosaccharyltransferase Assay 방법 연구)

  • Kim, Seong-Hun
    • Korean Journal of Microbiology
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    • v.46 no.1
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    • pp.96-103
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    • 2010
  • Oligosaccharyltransferase (OTase) catalyzes the transfer of a lipid-linked oligosaccharide (LLO) to the nascent polypeptide. Most eukaryotes have an OTase composed of a multisubunit protein complex. However, the kinetoplastid Leishmania major and the bacterium Campylobacter jejuni have only a single subunit for OTase activity, Stt3p and PglB, respectively. In this study, a new in vitro assay for OTase was developed by using a fluorescent peptide containing N-glycosylation sequon, Asn-Xaa-Thr/Ser, where Xaa can be any amino acid residue except Pro. L. major Stt3p and C. jejuni PglB as a model OTase enzyme demonstrated the formation of glycopeptides from a fluorescent peptide through OTase activities. For separation and measurement of the glycopeptides produced by the OTases, Tricine-SDS-PAGE, a lectin column and fluorospectrophotometer, and HPLC were applied. Comparison of these assay methods for analyzing a fluorescent glycopeptide showed HPLC analysis is the best method for separation of glycopeptides and nonglycosylated peptides as well as for quantify the peptides than other methods.