• 제목/요약/키워드: Solid-state synthesis

검색결과 355건 처리시간 0.034초

Y3Al5O12:Eu3+ 적색 형광체의 제조와 발광특성 (Luminescent Characteristics and Synthesis of Y3Al5O12:Eu3+ Red Phosphors)

  • 유일
    • 한국재료학회지
    • /
    • 제32권10호
    • /
    • pp.425-428
    • /
    • 2022
  • In this study, Y3Al5O12:Eu3+ red phosphors were synthesized at different temperatures using a solid state reaction method. The crystal structures, surface and optical properties of the Y3Al5O12:Eu3+ red phosphors were investigated using X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), and photoluminescence (PL) analyses. From XRD results, the crystal structure of the Y3Al5O12:Eu3+ red phosphors was determined to be cubic. The maximum emission spectra were observed for the Y3Al5O12:Eu3+ red phosphor prepared by annealing for 4h at 1,700 ℃. The 565~590 nm photoluminescent spectra of the Y3Al5O12:Eu3+ red phosphors is associated with the 5D07F2 magnetic dipole transition of the Eu3+ ions. The intensity of the photoluminescent spectra in the red phosphors is more dominant for the magnetic dipole transition than the electric dipole transition with increasing annealing temperature. The International Commission on Illumination (CIE) coordinates of Y3Al5O12:Eu3+ red phosphors prepared by 1,700 ℃ annealing temperature are X = 0.5994, Y = 0.3647.

Synthesis and Comparative Analysis of Crystallite Size and Lattice Strain of Pb2Ba1.7Sr0.3Ca2Cu3O10+δ Superconductor

  • Hasan, Maher Abd Ali;Jasim, Kareem Ali;Miran, Hussein Ali Jan
    • 한국재료학회지
    • /
    • 제32권2호
    • /
    • pp.66-71
    • /
    • 2022
  • In this article, Pb2Ba1.7Sr0.3Ca2Cu3O10+δ superconductor material was synthesized using conventional solid-state reaction method. X-ray diffraction (XRD) analysis demonstrated one dominant phase 2223 and some impurities in the product powder. The strongest peaks in the XRD pattern were successfully indexed assuming a pseudo-tetragonal cell with lattice constants of a = 3.732, b = 3.733 and c = 14.75 Å for a Pb-Based compound. The crystallite size and lattice strain between the layers of the studied compound were estimated using several methods, namely the Scherrer, Williamson-Hall (W.H), size-strain plot (SSP) and Halder Wagner (H.W) approach. The values of crystallite size, calculated by Scherrer, W.H, SSP and H.W methods, were 89.4540774, 86.658638, 87.7555823 and 85.470086 Å, respectively. Moreover, the lattice strain values obtained by W.H, SSP and H.W methods were 0.0063240, 0.006325 and 0.006, respectively. It was noted that all crystallite size results are consistent; however, the best method is the size-strain plot because it gave a value of R2 approaching one. Furthermore, degree of crystallites was calculated and found to be 59.003321%. Resistivity analysis suggests zero-resistance, which is typical of superconducting materials at critical temperature. Four-probe technique was utilized to measure the critical temperature at onset Tc(onset), zero resistivity Tc(off set), and transition (width ΔT), corresponding to temperatures of 128 K, 116 K, and 12 K, respectively.

Synthesis and Analysis of the Impact of Partial Mercury Replacement with Lead on the Structural and Electrical Properties of the Hg1-xPbxBa2Ca2Cu3O8+δ Superconductor

  • Kareem Ali Jasim;Chaiar Abdeen Zaynel Saleh;Alyaa Hamid Ali Jassim
    • 한국재료학회지
    • /
    • 제34권1호
    • /
    • pp.21-26
    • /
    • 2024
  • In this investigation, samples of the chemical (Hg1-xPbxBa2Ca1.8Mg0.2Cu3O8+δ) were prepared utilizing a solid-state reaction technique with a range of lead concentrations (x = 0.0, 0.05, 0.10, and 0.20). Specimens were pressed at 8 tons per square centimeter and then prepared at 1,138 K in the furnace. The crystalline structure and surface topography of all samples were examined using X-ray diffraction (XRD) and atomic force microscopy (AFM). X-ray diffraction results showed that all of the prepared samples had a tetragonal crystal structure. Also, the results showed that when lead was partially replaced with mercury, an increase in the lead value impacted the phase ratio, and lattice parameter values. The AFM results likewise showed excellent crystalline consistency and remarkable homogeneity during processing. The electrical resistivity was calculated as a function of temperature, and the results showed that all samples had a contagious behavior, as the resistivity decreased with decreasing temperature. The critical temperature was calculated and found to change, from 102, 96, 107, and 119 K, when increasing the lead values in the samples from 0.0 to 0.05, 0.10, and 0.20, respectively.

(Ba0.5Sr0.5)0.99Co0.2Fe0.8O3-δ(BSCF)의 합성 및 BSCF/GDC(Buffer)/ScSZ의 전기화학적 특성 (Synthesis of (Ba0.5Sr0.5)0.99Co0.2Fe0.8O3-δ (BSCF) and the Electrochemical Performance of the BSCF/GDC(Buffer)/ScSZ)

  • 임용호;황해진;문지웅;박선민;최병현;이미재
    • 한국세라믹학회지
    • /
    • 제43권6호
    • /
    • pp.369-375
    • /
    • 2006
  • [ $(Ba_{0.5}Sr_{0.5})_{0.99}Co_{x}Fe_{1-x}O_{3-{\delta}}$ ] [x=0.8, 0.2](BSCF) powders were synthesized by a Glycine-Nitrate Process (GNP) and the electrochemical performance of the BSCF cathode on a scandia stabilized zirconia, $[(Sc_{2}O_3)_{0.11}(ZrO_2)_{0.89}]-1Al_{2}O_3$ was investigated. In order to prevent unfavorable solid-state reactions between the cathode and zirconia electrolyte, a GDC ($Gd_{0.1}Ce_{0.9}O_{2-{delta}}$) buffer layer was applied on ScSZ. The BSCF (x = 0.8) cathode formed on GDC(Buffer)/ScSZ(Disk) showed poor electrochemical property, because the BSCF cathode layer peeled off after the heat-treatment. On the other hand, there were no delamination or peel off between the BSCF and GDC buffer layer, and the BSCF (x = 0.2) cathode exhibited fairly good electrochemical performances. It was considered that the observed phenomenon was associated with the thermal expansion mismatch between the cathode and buffer layer. The ohmic resistance of the double layer cathode was slightly lower than that of the single layer BSCF cathode due to the incorporation of platinum particle into the BSCF second layer.

카바졸과 페노시아진을 이용한 염료감응형 태양전지의 염료 합성과 광적특성 (Synthesis and Photovoltaic Properties of Dendritic Photosensitizers containing Carbazole and Phenothiazine for Dye-sensitized Solar Cells)

  • 김명석;정대영;김재홍
    • 한국신재생에너지학회:학술대회논문집
    • /
    • 한국신재생에너지학회 2010년도 춘계학술대회 초록집
    • /
    • pp.89.1-89.1
    • /
    • 2010
  • Since Gratzel and co-workers developed a new type of solar cell based on the nanocrystalline $TiO_2$ electrode, dye-sensitized solar cells (DSSCs) have attracted considerable attention on account of their high solar energy-to-conversion efficiencies (11%), their easy manufacturing process with low cost production compared to conventional p-n junction solar cells. The mechanism of DSSC is based on the injection of electrons from the photoexcited dye into the conduction band of nanocrystalline $TiO_2$. The oxidized dye is reduced by the hole injection process from either the hole counter or electrolyte. Thus, the electronic structures, such as HOMO, LUMO, and HOMO-LUMO gap, of dye molecule in DSSC are deeply related to the electron transfer by photoexcitation and redox potential. To date, high performance and good stability of DSSC based on Ru-dyes as a photosensitizer had been widely addressed in the literatures. DSSC with Ru-bipyridyl complexes (N3 and N719), and the black ruthenium dye have achieved power conversion efficiencies up to 11.2% and 10.4%, respectively. However, the Ru-dyes are facing the problem of manufacturing costs and environmental issues. In order to obtain even cheaper photosensitizers for DSSC, metal-free organic photosensitizers are strongly desired. Metal-free organic dyes offer superior molar extinction coefficients, low cost, and a diversity of molecular structures, compared to conventional Ru-dyes. Recently, novel photosensitizers such as coumarin, merocyanine, cyanine, indoline, hemicyanine, triphenylamine, dialkylaniline, bis(dimethylfluorenyl)-aminophenyl, phenothiazine, tetrahydroquinoline, and carbazole based dyes have achieved solar-to-electrical power conversion efficiencies up to 5-9%. On the other hand, organic dye molecules have large ${\pi}$-conjugated planner structures which would bring out strong molecular stacking in their solid-state and poor solubility in their media. It was well known that the molecular stacking of organic dyes could reduce the electron transfer pathway in opto-electronic devices, significantly. In this paper, we have studied on synthesis and characterization of dendritic organic dyes with different number of electron acceptor/anchoring moieties in the end of dendrimer. The photovoltaic performances and the incident photon-to-current (IPCE) of these dyes were measured to evaluate the effects of the dendritic strucuture on the open-circuit voltage and the short-circuit current.

  • PDF

기계화학공정을 이용한 Perovskite 구조의 (Pb, La)$TiO_3$ 나노 분말 합성 및 특성 (Synthesis and characterization of perovskite nano-sized (Pb, La)$TiO_3$ powder using mechano chemical process)

  • 임보라미;양재교;이동석;노태형;서정혜;이연승;김희택;좌용호
    • 한국결정성장학회지
    • /
    • 제18권5호
    • /
    • pp.200-204
    • /
    • 2008
  • 기계화학공정(MCP; Mechano Chemical Process)은 원료 분말이 기계적인 에너지로 인해 상 형성이 활성화되기 때문에 기존의 볼밀링을 이용한 고상반응에서 필수적인 높은 온도에서의 하소 공정이 필요하지 않다. 본 연구에서는 고 에너지 MCP 방법을 이용하여 perovskite 구조를 가지는 PLT 나노 분말을 제조하였다. 특히, 일반적으로 출발물질로 염을 이용하는 것과 달리 산화물을 원료 분말로 사용하여 어떠한 열처리 공정 없이 PLT 나노 분말을 합성하였다. 또한 건식으로 밀링을 하여 분말 건조 공정이 필요 없어서 공정이 간단하다. MCP 밀링은 시간 별로 12시간까지 진행하였으며, 제조된 분말의 상 분석과 결정면 분석 결과 3시간 이후에는 perovskite 구조의 순수한 PLT 상을 형성하였다. 또한 마이크로 크기의 원료 분말이 밀링 3시간이 지나자 약 20 nm 크기의 균일한 나노 입자가 생성되었다.

발화합성용액의 pH가 Y1Ba2Cu3O7-x 초전도상 생성 속도에 미치는 영향 (Effect of the pH of Pyrophoric Synthetic Solution on the Formation Kinetics of Y1Ba2Cu3O7-x Superconducting Phase)

  • 박정식;김영순;양석우;김춘영;신형식
    • 공업화학
    • /
    • 제9권2호
    • /
    • pp.165-171
    • /
    • 1998
  • $Y_2O_3$(99.9%)와 $BaCO_3$(99.9%) 및 CuO(99.9%)를 사용하여 $Y_1Ba_2Cu_3O_{7-x}$(123) 분말을 발화합성법에 의해 제조하였다. 발화전 용액을 여러 가지 pH로 변화시켜 제조하였으며, 이 분말을 성형하여 열처리 온도와 시간 변화에 따른 상형성과 반응특성을 조사하였다. 시료의 조성과 조직의 특성은 ICP와 SEM을 이용하여 측정하였고, Y-Ba-Cu-O계의 상형성과 전화율을 결정하기 위해 X선 회절분석을 하였다. 발화합성법을 이용하여 pH 7(${\pm}0.3$)에서 제조된 123 분말이 순도와 균일성 및 반응특성에서 가장 좋은 결과를 보였다. pH 7(${\pm}0.3$)에서 제조된 분말을 이용한 123 상생성에 따른 활성화에너지(${\Delta}E_a$)는 191kJ/mol으로서 고상반응법의 230kJ/mol에 약 13% 정도 더 낮았다.

  • PDF

TiCl4를 출발원료로한 구형 Li4Ti5O12 분말합성 및 리튬이차 전지특성 (Electrochemical Properties of Lithium Secondary Battery and the Synthesis of Spherical Li4Ti5O12 Powder by Using TiCl4 As a Starting Material)

  • 최병현;지미정;권용진;김은경;남산
    • 한국재료학회지
    • /
    • 제20권12호
    • /
    • pp.669-675
    • /
    • 2010
  • One of the greatest challenges for our society is providing powerful electrochemical energy conversion and storage devices. Rechargeable lithium-ion batteries and fuel cells are among the most promising candidates in terms of energy and power density. As the starting material, $TiCl_4{\cdot}YCl_3$ solution and dispersing agent (HCP) were mixed and synthesized using ammonia as the precipitation agent, in order to prepare the nano size Y doped spherical $TiO_2$ precursor. Then, the $Li_4Ti_5O_{12}$ was synthesized using solid state reaction method through the stoichiometric mixture of Y doped spherical $TiO_2$ precursor and LiOH. The Ti mole increased the concentration of the spherical particle size due to the addition of HPC with a similar particle size distribution in a well in which $Li_4Ti_5O_{12}$ spherical particles could be obtained. The optimal synthesis conditions and the molar ratio of the Ti 0.05 mol reaction at $50^{\circ}C$ for 30 minutes and at $850^{\circ}C$ for 6 hours heat treatment time were optimized. $Li_4Ti_5O_{12}$ was prepared by the above conditions as a working electrode after generating the Coin cell; then, electrochemical properties were evaluated when the voltage range of 1.5V was flat, the initial capacity was 141 mAh/g, and cycle retention rate was 86%; also, redox reactions between 1.5 and 1.7V, which arose from the insertion and deintercalation of 0.005 mole of Y doping is not a case of doping because the C-rate characteristics were significantly better.

Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • 대한화학회지
    • /
    • 제55권6호
    • /
    • pp.919-925
    • /
    • 2011
  • A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Vicinal Oxime 리간드의 새로운 구리(II) 착물에 대한 합성, 특성 및 ESR 연구 (Synthesis, Characterization and ESR Studies of New Copper(II) Complexes of Vicinal Oxime Ligands)

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • 대한화학회지
    • /
    • 제55권4호
    • /
    • pp.603-611
    • /
    • 2011
  • Ethoxylacetyl oxime 리간드 [HL, (1) 및 $H_2L^1$, (3)]와 아세트산 구리(II) 일수화물을 반응시켜 팔면체 및 사각평면착물을 각각 얻었다. 이들 착물을 원소분석, IR 및 UV-Vis 스펙트럼, 자기수자율, 전기전도도 및 ESR 스펙트럼으로 조사하였다. DMF에서 이들 착물의 몰전기전도도 측정한 결과 비이온성을 보였다. 실온 및 77 K에서 [$(L)_2Cu(H_2O)_2$], (2) 착물의 ESR 스펙트럼은 배위결합성을 갖는 축대칭($d_{x2-y2}$)의 특성을 보이며, 또한 전형적인 쌍극자 상호작용에 의해 큰 띠나비를 갖는다. 그러나 착물 [$(L^1)Cu$], (4)는 고체상태에서 큰 띠넓임으로 인해 초미세 갈라짐이 관찰되지 않았는데, 이는 구리(II) 결합자리들 사이의 스핀-교환 상호작용에 의한 것으로 확인되었다. 실온에서 도포된 구리(II) 착물의 스펙트럼은 배위된 질소원자로 인해 극초미세 갈라짐을 보였다. 또한 이 물질은 공유 결합성을 갖는 축형태($d_{x2-y2}$)의 특성을 보이고, 구리(II) 이온의 환경은 기본적으로 사각-평면 배열을 갖는다. 77 K의 얼어있는 메탄올에서 [$(L_1)Cu$], (4)의 스펙트럼은 이합체 화합물의 삼중항 상태의 특성을 보이며, 두 구리(II) 이온 중심 사이의 거리를 계산한 결과 4.8 이다.