• 제목/요약/키워드: X-ray회절법

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Temperature-Programmed Reduction of Copper Oxide Supported on ${\gamma}-Al_2O_3$ and $SiO_2$ (${\gamma}-Al_2O_3$$SiO_2$에 입혀진 산화 구리의 승온 환원)

  • Hwa-Gyung Lee;Chong-Soo Han;Min-Soo Cho;Kae-Soo Lee;Hakze Chon
    • Journal of the Korean Chemical Society
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    • v.30 no.5
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    • pp.415-422
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    • 1986
  • The metal-support interaction of copper oxide supported on ${\gamma}$-alumina and silica was studied by X-ray diffraction (XRD) and temperature-programmed reduction(TPR). It was found that XRD pattern of CuO can not be observed up to 5.0wt % copper content for CuO/${\gamma}-Al_2O_3$ while CuO/$SiO_2$ sample shows the CuO pattern even at 2.5wt% copper content. $H_2-$TPR of CuO/${\gamma}-Al_2O_3$ system shows four major peaks at 145${\circ}C$, 185${\circ}C$, 210${\circ}C$, and 250${\circ}C$. In the case of CuO/$SiO_2$, a large peak at 250${\circ}C$ was appeared accompanying a small peak at 425${\circ}C$. Comparing the TPR peaks with that of copper aluminate which was prepared from the calcination of CuO/${\gamma}-Al_2O_3$ at 1000${\circ}C$, the peaks at around 145${\circ}C$, 200${\circ}C$ (185${\circ}C$ and 210${\circ}C$), and 250${\circ}C$ were corresponded to $Cu^+$ ion in CuO interacting ${\gamma}-Al_2O_3$, $Cu^+$ ions in defect sites of ${\gamma}-Al_2O_3$ and $Cu^{2+}$ ion in the bulk CuO layer, respectively. From the results, it was concluded that there is considerable metal-support interaction in CuO on ${\gamma}-Al_2O_3$ and the interaction results in a stabilization of $Cu^+$ ion in the system.

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Synthesis, Sytructure, and Magnetic Properties of One-Dimensional Thiophoshates, $Al_2NiP_2S_6$ (A=Rb, Cs) (1차원 구조를 갖는 Thiophoshates, $Al_2NiP_2S_6$ (A=Rb, Cs)의 합성, 구조 및 자기적 성질)

  • Dong, Yong Kwan;Lee, Kun Soo;Yun, Ho Seop;Hur, Nam Hwi
    • Journal of the Korean Chemical Society
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    • v.45 no.3
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    • pp.242-246
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    • 2001
  • The quaternary thiophosphates, $A_2NiP_2S_6$ (A=Rb, Cs), have been synthesized with halide fluxes and structurally characterized by single-crystal X-ray diffraction technique. These compounds crystallize in the space group $C_{2h}^5-P2_1/n$ of the monoclinic system with two formula units in a cell of dimensions a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, and $V=546.0(3)\AA^3$ for Rb2NiP2S6 and a=5.957(4), b=12.696(7), $c=7.679(4)\AA$, $b=93.60(5)^{\circ}$, and $V=579.7(5)\AA^3$ for $Cs_2NiP_2S_6.$ These compounds are isostructural. The structure of $Cs_2NiP_2S_6$ is made up of one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chains along the a axis and these chains are isolated by $Cs^+$ ions. The Ni atom is octahedrally coordinated by six S atoms. These Ni$S_6$ octahedral units are linked by sharing three m-S atoms of the $[P_2S_6^{4-}]$ anions to form the infinite one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chain. For $Cs_2NiP_2S_6$, the magnetic susceptibility reveals an antiferromagnetic exchange interaction below 8K,which corresponds to the Neel temperature ($T_N$). Above $T_N$, this compound obeys Curie-Weiss law. The magnetic moment, C, and ${\theta}forCs_2NiP_2S_6$ are 2.77 B.M., 0.9593 K, and -19.02 K, respectively. The effective magnetic moment obtained from the magnetic data is agreed with the spin-only value of $Ni^{2+}d^8$(2.83 B.M.) system.

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A comparative study of electroplating and electroless plating for diameter increase of orthodontic wire (교정용 선재의 직경 증가를 위한 전기도금법과 무전해도금법의 비교연구)

  • Kim, Jae-Nam;Cho, Jin-Hyoung;Sung, Young-Eun;Lee, Ki-Heon;Hwang, Hyeon-Shik
    • The korean journal of orthodontics
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    • v.36 no.2 s.115
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    • pp.145-152
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    • 2006
  • The purpose of this study was to evaluate electroless plating as a method of increasing the diameter of an orthodontic wire in comparison with eletroplating. After pretreatment plating of the 0.016 inch stainless steel orthodontic wire, electroless plating was performed at $90^{\circ}C$ until the diameter of the wire was increased to 0.018 inch. During the process of electroless plating, the diameter of the wire was measured every 5 minutes to examine the increasing ratio of the wire's diameter per time unit. And to examine the uniformity, the diameter at 3 points on the electroless-plated orthodontic wire was measured. An X-ray diffraction test for analyzing the nature of the plated metal and a 3-point bending test for analyzing the physical property were performed. The electroless-plated wire group showed a increased tendency for stiffness, yield strength, and ultimate strength than the electroplated wire group. And there was a statistically significant difference between the two groups for stiffness and ultimate strength. In the electroless-plated wire group, the increasing ratio of the diameter was $0.00461{\pm}0.00003mm/5min$ (0.00092 mm/min). In the electroplated wire group, it was $0.00821{\pm}0.00015mm/min$. The results of the uniformity test showed a tendency for uniformity in both the plating methods. The results of this study suggest that electroless plating of the wire is closer to the ready-made wire than electroplating wire in terms of the physical property. However, the length of plating time needs further consideration for the clinical application of electroless plating.

Physical Properties of Cd2GeSe4 and Cd2GeSe4:Co2+ Thin Films Grown by Thermal Evaporation (진공증착법에 의해 제작된 Cd2GeSe4와 Cd2GeSe4:Co2+ 박막의 물리적 특성)

  • Lee, Jeoung-Ju;Sung, Byeong-Hoon;Lee, Jong-Duk;Park, Chang-Young;Kim, Kun-Ho
    • Journal of the Korean Vacuum Society
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    • v.18 no.6
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    • pp.459-467
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    • 2009
  • $Cd_2GeSe_4$ and $Cd_2GeSe_4:Co^{2+}$ films were prepared on indium-tin-oxide(ITO)-coated glass substrates by using thermal evaporation. The crystallization was achieved by annealing the as-deposited films in flowing nitrogen. X-ray diffraction spectra showed that the $Cd_2GeSe_4$ and the $Cd_2GeSe_4:Co^{2+}$ films were preferentially grown along the (113) orientation. The crystal structure was rhomohedral(hexagonal) with lattice constants of $a=7.405\;{\AA}$ and $c=36.240\;{\AA}$ for $Cd_2GeSe_4$ and $a=7.43\;{\AA}$ and $c=36.81\;{\AA}$ for $Cd_2GeSe_4:Co^{2+}$ films. From the scanning electron microscope images, the $Cd_2GeSe_4$ and $Cd_2GeSe_4:Co^{2+}$ films were plated, and the grain size increased with increasing annealing temperature. The optical energy band gap, measured at room temperature, of the as-deposited $Cd_2GeSe_4$ films was 1.70 eV and increased to about 1.74 eV and of the as-deposited $Cd_2GeSe_4:Co^{2+}$ films was 1.79 eV and decreased to about 1.74 eV upon annealing in flowing nitrogen at temperatures from $200^{\circ}C$ to $500^{\circ}C$. The dynamical behavior of the charge carriers in the $Cd_2GeSe_4$ and $Cd_2GeSe_4:Co^{2+}$ films were investigated by using the photoinduced discharge characteristics technique.

Three Crystal Structures of Dehydrated Partially $Co^{2+}-Exchanged$ Zeolite A Treated with Potassium Vapor (부분적으로 코발트 이온으로 치환한 제올라이트 A를 진공 탈수한 후 칼륨 증기로 반응시킨 3개의 결정구조)

  • Jeong Mi Suk;Jang Se Bok
    • Korean Journal of Crystallography
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    • v.15 no.2
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    • pp.59-68
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    • 2004
  • Three crystal structures of dehydrated partially $Co^{2+}-exchanged$ zeolite A treated with 0.6 Torr of K at $300^{\circ}C$ (for 12 hrs, 6 hrs, and 2 hrs) vapor have been determined by single-crystal X-ray diffraction techniques in the cubic space group Pm3m at 21(1)$^{\circ}C(a=12.181(1)\;{\AA},\;a=12.184(1)\;{\AA},\;and\;a=12.215(1)\;{\AA})\;respectively)$. Their structures were refined to the final error indices, R(weight) of 0.090 with 10 reflections, 0.091 with 82 reflections, and 0.090 with 80 reflections, respectively, for which $1>\sigma(I)$. In each structure, all four $Co^{2+}$ and four $Na^+$ ions to be reduced by K atoms. The cobalt and sodium atoms produced are no longer found in the zeolite. K species are found at five different crystallographic sites: three $K^+$ ions lie at the planes of 8-rings, filling that position, ca. 11.5 K^+$ ions lie on threefold axes, ca. 4.0 in the large cavity and ca. 4.0 in the sodalite cavity, and ca. 0.5 $K^+$ ion is found near a 4-ring. ca. three $K^0$ atoms are found deep into the large cavity on threefold axes. In these structures, crystallographic results show that cationic tetrahedral $K_4$ (and/or triangular $K_3$) clusters have formed in the sodalites of zeolite A. The $K_4$ and/or $K_3$ clusters coordinate trigonally to three oxygens of a six-oxygen ring. The partially reduced ions of these clusters interact primarily with oxygen atoms of the zeolite structure rather than with each other. ca. 14.5K species are found per unit cell, more than the twelve $K^+$ ions needed to balance the anionic charge of zeolite framework, indicating that sorption of $K^0$ has occurred. The three $K^0$ atoms in the large cavity are closely associated with three out of four $K^+$ ions in the large cavity to form $K_7^{4+}$ clusters. The $K_7^{4+}$ cluster not interacts primarily with framework oxygens.

Crystallographic Study on the Selectivity and Distribution of Sr2+ Ions Within Zeolite A In the Presence of Competing Na+ Ions in Aqueous Exchange Solution (Na+ 경쟁이온이 존재하는 수용액에서 Zeolite A 내 Sr2+ 이온의 선택성 및 분포에 관한 결정학적 연구)

  • kim, Hu Sik;Park, Jong Sam;Lim, Woo Taik
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.1
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    • pp.41-50
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    • 2022
  • To study the properties of Sr2+ exchange into zeolite A with increasing the molar concentration of Na+ in given exchange solution, four single crystals of fully dehydrated Sr2+- and Na+- exchanged zeolite A were prepared by the bath method using mixed ion-exchange solutions. The Sr(NO3)2:NaNO3 molar rations of the ion exchange solution were 1:1(crystal 1), 1:100(crystal 2), 1:250(crystal 3), and 1:500 (crystal 4), respectively, with a total concentration of 0.05 M. The single-crystals were then vacuum dehydration at 623 K and 1×10-4 Pa for 2 days. Their single-crystal structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group Pm3-m, at 100(1) K, and were then refined to the final error indices of R1/wR2=0.047/0.146, 0.048/0.142, 0.036/0.128, and 0.040/0.156 for crystals 1, 2, 3, and 4, respectively. In crystals 1 and 2, the 6 Sr2+ ions are found at three different crystallographic sites. In crystal 3, 1 Sr2+ and 10 Na+ ions are found in large cavity and sodalite unit. In crystal 4, only 12 Na+ ions occupy three equipoints. The degree of Sr2+ ion-exchange decreased sharply from 100 to 16.7 to 0% as the initial Na+ concentration increase and the Sr2+ concentration decrease. In addition, the unit cell constant of the zeolite framework decreased with this lower level of Sr2+ exchange.

Properties of Photoluminescence and Growth of CdIn2Te4 Single Crystal by Bridgeman method (Bridgeman법에 의한 CdIn2Te4 단결정 성장과 광발광 특성)

  • Moon, Jong-Dae
    • Journal of Sensor Science and Technology
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    • v.12 no.6
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    • pp.273-281
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    • 2003
  • A stoichiometric mixture for $CdIn_2Te_4$ single crystal was prepared from horizontal electric furnace. The $CdIn_2Te_4$ single crystal was grown in the three-stage vertical electric furnace by using Bridgeman method. The quality of the grown crystal has been investigated by the x-ray diffraction and the photoluminescence measurements. The (001) growth plane of oriented $CdIn_2Te_4$ single crystal was confirmed from back-reflection Laue patterns. The carrier density and mobility of $CdIn_2Te_4$ single crystal measured with Hall effect by van der Pauw method are $8.61{\times}10^{16}\;cm^{-3}$ and $242\;cm^2/V{\cdot}s$ at 293 K, respectively. The temperature dependence of the energy band gap of the $CdIn_2Te_4$ single crystal obtained from the absorption spectra was well described by the Varshni's relation, $E_g(T)=1.4750\;eV-(7.69{\times}10^{-3}\;eV)T^2/(T+2147)$. After the as-grown $CdIn_2Te_4$ single crystal was annealed in Cd-, In-, and Te-atmospheres, the origin of point defects of $CdIn_2Te_4$ single crystal has been investigated by the photoluminescence(PL) at 10 K. The native defects of $V_{Te}$, $Cd_{int}$, and $V_{Cd}$, $Te_{int}$ obtained by PL measurements were classified as a donors or acceptors type. And we concluded that the heat-treatment in the Cd-atmosphere converted $CdIn_2Te_4$ single crystal to an optical n-type. Also, we confirmed that In in $CdIn_2Te_4$ did not form the native defects because In in $CdIn_2Te_4$ single crystal existed in the form of stable bonds.

Characterization of InAs Quantum Dots in InGaAsP Quantum Well Grown by MOCVD for 1.55 ${\mu}m$

  • Choe, Jang-Hui;Han, Won-Seok;Song, Jeong-Ho;Lee, Dong-Han
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.134-135
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    • 2011
  • 양자점은 전자와 양공을 3차원으로 속박 시키므로 기존의 bulk나 양자우물보다 양자점을 이용한 레이저 다이오드의 경우 낮은 문턱 전류, 높은 미분이득 및 온도 안전성의 장점이 있을 거라 기대되고 있다. 그러나, 양자점은 낮은 areal coverage 때문에 높은 속박효율을 얻지 못하고 있다. 이러한 양자점의 문제점을 해결하기 위해 양자점을 양자우물 안에 성장시켜 운반자들의 포획을 향상시키는 방법들이 연구되고 있다. 양자우물 안에 양자점을 넣으면 양자우물이 운반자들의 포획을 증가 시키고, 열적 방출도 억제하여 온도 안정성이 향상 되는 것으로 알려져 있다. 광통신 대역의 1.3 ${\mu}m$ 경우, GaAs계를 이용하여 InAs 양자점을 strained InGaAs 박막을 우물층으로 한 dot-in-a-well 구조의 연구는 몇몇 보고된 바 있다. 그러나 InP계를 사용하는 1.55 ${\mu}m$ 대역에서 dot-in-a-well구조의 연구는 아직 미미하다. 본 연구에서는 유기 금속 화학 증착법(metal organic chemical vapor deposition)을 이용하여 InP 기판 위에 InAs 양자점을 자발성장법으로 성장하였으며 dot-in-a-well 구조에서 우물층으로 1.35 ${\mu}m$ 파장의 $In_{0.69}Ga_{0.31}As_{0.67}P_{0.33}$ (1.35Q)를, 장벽층으로는 1.1 ${\mu}m$ 파장의 $In_{0.85}Ga_{0.15}As_{0.32}P_{0.68}$(1.1Q)를 사용하였다. 양자우물층과 장벽층은 모두 InP 기판과 격자가 일치하는 조건으로 성장하였다. III족 원료로는 trimethylindium (TMI)와 trimethylgalium (TMGa)을 사용하였으며 V족 원료 가스로는 $PH_3$ 100%, $AsH_3$ 100%를, carrier gas로는 $H_2$를 사용하였다. InP buffer층의 성장 온도는 640$^{\circ}C$이며 양자점 성장 온도는 520$^{\circ}C$이다. 양자점 형성은 원자력간 현미경(Atomic force microscopy)를 이용하여 확인하였으며, 박막의 결정성은 쌍결정 회절분석(Double crystal x-ray deffractometry)를 이용하여 확인하였다. 확인된 성장 조건을 이용하여 양자점 시료를 성장하였으며 광여기분광법(Photoluminescence)을 이용하여 광특성을 분석하였다. Fig. 1은 dot in a barrier 와 dot-in-a-well 시료의 성장구조이다. Fig. 1(a)는 일반적인 dot-in-a-barrier 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장한 후 양자점을 성장하였다. 그 후 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 1(b)는 dot-in-a-well 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장 후 1.35Q 우물층을 4 nm 성장하였다. 그 위에 InAs 양자점을 성장하였다. 그 후에 1.35Q 우물층을 4 nm 성장하고 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 2는 dot-in-a-barrier 시료와 dot-in-a-well 시료의 상온 PL data이다. Dot-in-a-barrier 시료의 PL 파장은 1544 nm이며 반치폭은 79.70 meV이다. Dot-in-a-well 시료의 파장은 1546 nm이며 반치폭은 70.80 meV이다. 두 시료의 PL 파장 변화는 없으며, 반치폭은 dot-in-a-well 시료가 8.9 meV 감소하였다. Dot-in-a-well 시료의 PL peak 강도는 57% 증가하였으며 적분강도(integration intensity)는 45%가 증가하였다. PL 데이터에서 높은 에너지의 반치폭 변화는 없으며 낮은 에너지의 반치폭은 8 meV 감소하였다. 적분강도 증가에서 dot-in-a-well 구조가 dot-in-a-barrier 구조보다 전자-양공의 재결합이 증가한다는 것을 알 수 있으며, 반치폭 변화로부터 특히 높은 에너지를 갖는 작은 양자점에서의 재결합이 증가 된 것을 알 수 있다. 이는 양자우물이 장벽보다 전자-양공의 구속력을 증가시키기 때문에 양자점에 전자와 양공의 공급을 증가시키기 때문이다. 따라서 낮은 에너지를 가지는 양자점을 모두 채우고 높은 에너지를 가지는 양자점까지 채우게 되므로, 높은 에너지를 가지는 양자점에서의 전자-양공 재결합이 증가되었기 때문이다. 뿐만 아니라 파장 변화 없이 PL peak 강도와 적분강도가 증가하고 낮은 에너지 쪽의 반치폭이 감소한 것으로부터 에너지가 낮은 양자점보다는 에너지가 높은 양자점에서의 전자-양공 재결합율이 급증하였음을 알 수 있다. 우리는 이와 같은 연구에서 InP계를 이용해 1.55 ${\mu}m$에서도 dot in a well구조를 성장 하여 더 좋은 특성을 낼 수 있으며 앞으로 많은 연구가 필요할 것이라 생각한다.

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Growth of Fe3O4 Particles and Their Magnetic Properties (Fe3O4 분말제조와 자기적 특성)

  • Kwon, Woo-Hyun;Lee, Seung-Wha;Chae, Kwang-Pyo;Lee, Jae-Gwang;Sur, Jung-Chul
    • Journal of the Korean Magnetics Society
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    • v.19 no.5
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    • pp.180-185
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    • 2009
  • Fe$_3$O$_4$ particles, prepared by a sol-gel method, were examined for their structural characteristic, particle shapes and sizes, and their magnetic properties. Two different chemical compositions (using a mol rate Fe$^{2+}$/Fe$^{3+}$ = 1/2 and only Fe$^{2+}$) and 2-methoxyethanol were used for making proper solutions. And the solutions were refluxed and dry in a dry oven and the samples were fired at 200$\sim$600$^{\circ}C$ in the N$_2$ atmosphere. The formation of single-phased spinel ferrite powders was identified with the X-ray diffraction measurement as they were fired at above 250$^{\circ}C$. The result of scanning electron microscopy measurement showed the increase of annealing temperature yielded the particle size increased. The magnetic transition was observed using the Mossbaur spectroscopy measurement. As the ferrite, prepared with the chemical composition (Fe$^{2+}$/Fe$^{3+}$ = 1/2), was fired at 250$^{\circ}C$, 78% of the ferrite had a ferrimagnetic property and 22% of the ferrite was non-magnetic. In case of preparing the sample with only Fe$^{2+}$ and annealed at 200$^{\circ}C$, it had a single phased spinel structure but its particle size was too small to be ferrimagnetic. The annealing temperature above 250$^{\circ}C$ made powders a spinel structure regardless of the preparation method. They had a typical soft magnetic property and their saturation magnetization and coercivity became larger as the annealing temperature increased.

Catalytic Combustion of Methane over $AMnAl_{11}O_{19}$(A=La, Sr, Ba) and $CeO_2/LaAMnAl_{11}O_{19}$ ($AMnAl_{11}O_{19}$(A=La, Sr, Ba) 및 $CeO_2/LaAMnAl_{11}O_{19}$를 이용한 메탄의 촉매 연소)

  • Kim, Seongmin;Lee, Joon Yeob;Cho, In-Ho;Lee, Dae-Won;Lee, Kwan-Young
    • Korean Chemical Engineering Research
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    • v.49 no.5
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    • pp.633-638
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    • 2011
  • Mn substituted La, Sr or Ba-hexaaluminate were prepared by $(NH_4)_2CO_3$ co-precipitate method and calcined at $1,200^{\circ}C$ for 5 h. Catalysts were characterized by X-ray diffraction and $N_2$ physisorption and scanning electron microscope (SEM). Compared to $SrMnAl_{11}O_{19}$ and $BaMnAl_{11}O_{19}$, $LaMnAl_{11}O_{19}$ in which La located at mirror plane showed better crystallinity and high surface area, 13 $m^2/g$. $LaMnAl_{11}O_{19}$ revealed well developed plate-like structure which is characteristic structure of hexaaluminate. The catalytic activity of methane combustion increased in the following order: $LaMnAl_{11}O_{19}$ > $SrMnAl_{11}O_{19}$ > $BaMnAl_{11}O_{19}$ and was dependent on surface area of catalysts. 60 wt% $CeO_2/LaMnAl_{11}O_{19}$ calcined at $700^{\circ}C$ showed enhanced methane activity and methane was oxidized completely at low temperature ($700^{\circ}C$). It was confirmed that addition of ceria seems to be effective for the low and middle temperature combustion of methane. But, after calcination at high temperature of $1,200^{\circ}C$, it lost the promoting effect of ceria due to increase of ceria particle size and it had a limit to applying to the high temperature catalytic combustion.