• Title/Summary/Keyword: solid-phase synthesis

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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
    • Korean Journal of Materials Research
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    • v.32 no.2
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    • pp.66-71
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    • 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 Application of Bluish-Green BaSi2O2N2:Eu2+ Phosphor for White LEDs (백색 LED용 청록색 BaSi2O2N2:Eu2+ 형광체의 합성 및 응용)

  • Jee, Soon-Duk;Choi, Kang-Sik;Choi, Kyoung-Jae;Kim, Chang-Hae
    • Korean Journal of Materials Research
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    • v.21 no.5
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    • pp.250-254
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    • 2011
  • We have synthesized bluish-green, highly-efficient $BaSi_2O_2N_2:Eu^{2+}$ and $(Ba,Sr)Si_2O_2N_2:Eu^{2+}$ phosphors through a conventional solid state reaction method using metal carbonate, $Si_3N_4$, and $Eu_2O_3$ as raw materials. The X-ray diffraction (XRD) pattern of these phosphors revealed that a $BaSi_2O_2N_2$ single phase was obtained. The excitation and emission spectra showed typical broadband excitation and emission resulting from the 5d to 4f transition of $Eu^{2+}$. These phosphors absorb blue light at around 450 nm and emit bluish-green luminescence, with a peak wavelength at around 495 nm. From the results of an experiment involving Eu concentration quenching, the relative PL intensity was reduced dramatically for Eu = 0.033. A small substitution of Sr in place of Ba increased the relative emission intensity of the phosphor. We prepared several white LEDs through a combination of $BaSi_2O_2N_2:Eu^{2+}$, YAG:$Ce^{3+}$, and silicone resin with a blue InGaN-based LED. In the case of only the YAG:$Ce^{3+}$-converted LED, the color rendering index was 73.4 and the efficiency was 127 lm/W. In contrast, in the YAG:$Ce^{3+}$ and $BaSi_2O_2N_2:Eu^{2+}$-converted LED, two distinct emission bands from InGaN (450 nm) and the two phosphors (475-750 nm) are observed, and combine to give a spectrum that appears white to the naked eye. The range of the color rendering index and the efficiency were 79.7-81.2 and 117-128 lm/W, respectively. The increased values of the color rendering index indicate that the two phosphor-converted LEDs have improved bluish-green emission compared to the YAG:Ce-converted LED. As such, the $BaSi_2O_2N_2:Eu^{2+}$ phosphor is applicable to white high-rendered LEDs for solid state lighting.

Fabrication of Gd1.5Ba2Cu3O7-y Bulk Superconductors from the Powder Synthesized by a Solid-State Reaction Method (고상반응법으로 합성한 분말로부터 Gd1.5Ba2Cu3O7-y 벌크 초전도체의 제조)

  • Kim, Yong Ju;Park, Seung Yeon;You, Byung Youn;Park, Soon-Dong;Kim, Chan-Joong
    • Korean Journal of Materials Research
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    • v.23 no.6
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    • pp.309-315
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    • 2013
  • $GdBa_2Cu_3O_{7-y}$(Gd123) powders were synthesized by the solid-state reaction method using $Gd_2O_3$ (99.9% purity), $BaCO_3$ (99.75%) and CuO (99.9%) powders. The synthesized Gd123 powder and the Gd123 powder with $Gd_2O_3$ addition ($Gd_{1.5}Ba_2Cu_3O_{7-y}$(Gd1.5)) were used as raw powders for the fabrication of Gd123 bulk superconductors. The Gd123 and Gd1.5 bulk superconductors were fabricated by sintering or a top-seeded melt growth (TSMG) process. The superconducting transition temperature ($T_{c,onset}$) of the sintered Gd123 was 93 K and the transition width was as large as 20 K. The $T_{c,onset}$ of the TSMG processed Gd123 was 82 K and the transition width was also as large as 12 K. The critical current density ($J_c$) at 77 K and 0 T of the sintered Gd123 and TSMG processed Gd123 were as low as a few hundreds A/$cm^2$. The addition of 0.25 mole $Gd_2O_3$ and 1 wt.% $CeO_2$ to Gd123 enhanced the $T_c$, $J_c$ and magnetic flux density (H) of the TSMG processed Gd123 sample owing to the formation of the superconducting phase with high flux pinning capability. The $T_c$ of the TSMG processed Gd1.5 was 92 K and the transition width was 1 K. The $J_cs$ at 77 K (0 T and 2 T) were $3.2{\times}10^4\;A/cm^2$ and $2.5{\times}10^4\;A/cm^2$, respectively. The H at 77 K of the TSMG-processed Gd1.5 was 1.96 kG, which is 54% of the applied magnetic field (3.45 kG).

The study of oligopepetide synthesis and biological activity (올리고 펩타이드 유도체의 합성과 생리활성에 관한 연구)

  • Kim, Bo-Mi
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.12
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    • pp.62-70
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    • 2018
  • In this study, we synthesized Oligo Peptide (Lys-Val-Ala-Arg-Pro: KVARP) and peptide derivatives using Solid Phase Peptide Synthesis(SPPS). KVARP was commonly known to improve whitening of skin. We measured bio-activity of the synthesized compounds. The whitening effect was measured in tyrosinase inhibition and the result showed to be highly effective with 93% inhibition rate at $5000{\mu}g/m{\ell}$ of Geranic-KVARP, on the other hand the IC50 value was $68{\mu}g/m{\ell}$. The wrinkle-reducing effect was measured by elastase inhibition at a concentration of 63% at $400{\mu}g/m{\ell}$ of Salicylic-KVARP, and the IC50 value was $253{\mu}g/m{\ell}$. In the DPPH assay, Caffeic-KVARP showed more than 95% antioxidant activity at $400{\mu}g/m{\ell}$ with high concentration and IC50 value was $31{\mu}g/m{\ell}$. The anti-inflammatory effect of Nitric Oxide inhibition was 67% at $400{\mu}g/m{\ell}$ of Lipoic-KVARP. Therefore, the four types of KVARP derivative that were synthesized from various experiments has shown that it could have potential to be used to develop new medicines, cosmetics as well as in various industries.

Automated Synthesis of [$^{18}F$]Fallypride for Routine Clinical Use (자동합성장치를 이용한 [$^{18}F$]Fallypride의 합성)

  • Park, Jun-Hyung;Moon, Byung-Seok;Lee, Hong-Jin;Lee, Hyo-Jun;Lee, In-Won;Lee, Byung-Chul;Kim, Sang-Eun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.14 no.2
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    • pp.104-109
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    • 2010
  • Purpose: $[^{18}F]$Fallypride plays an effective radiotracer for the study of dopamine $D_2/D_3$ receptor occupancy, neuropsychiatric disorders and aging in humans. This tracer has the potential for clinical use, but automated labeling efficiency showed low radiochemical yields about 5~20% with relatively long labelling time of fluorine-18. In present study, we describe an improved automatic synthesis of [$^{18}F$]Fallypride using different base concentration for routine clinical use. Materials and Methods: Fully automated synthetic process of [$^{18}F$]Fallypride was perform using the TracerLab $FX_{FN}$ synthesizer under various labeling conditions and tosyl-fallypride was used as a precursor. [$^{18}F$]Fluoride was extracted with various concentration of $K_{2.2.2.}/K_2CO_3$ from $^{18}O$-enriched water trapped on the ion exchange cartridge. After azeotropic drying, the labeling reaction proceeded in $CH_3CN$ at $100^{\circ}C$ for 10 or 30 min. The reaction mixture was purified by reverse phase HPLC and collected organic solution was exchanged by tc-18 Sep-Pak for the clinically available solution. Results: The optimal labeling condition of [$^{18}F$]Fallypride in the automatic production was that 2 mg of tosyl-fallypride in acetonitrile (1 mL) was incubated at $100^{\circ}C$ for 10 min with $K_{2.2.2.}/K_2CO_3$ (11/0.8 mg). [$^{18}F$]Fallypride was obtained with high radiochemical yield about $66{\pm}1.4%$ (decay-corrected, n=28) within $51{\pm}1.2$ min including HPLC purification and solid-phase purification for the final formulation. Conclusion: [$^{18}F$]Fallypride was prepared with a significantly improved radiochemical yield with high specific activity and shorten synthetic time. In addition, this automated procedure provides the high reproducibility with no synthesis failures (n=28).

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Change of Electrochemical Characteristics Due to the Fe Doping in Lithium Manganese Oxide Electrode

  • Ju Jeh Beck;Kang Tae Young;Cho Sung Jin;Sohn Tae Won
    • Journal of the Korean Electrochemical Society
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    • v.7 no.3
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    • pp.131-137
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    • 2004
  • Sol-gel method which provides better electrochemical and physiochemical properties compared to the solid-state method was used to synthesize the material of $LiFe_yMn_{2-y}O_4$. Fe was substituted to increase the structural stability so that the effects of the substitution amount and sintering temperature were analyzed. XRD was used for the structural analysis of produced material, which in turn, showed the same cubic spinel structure as $LiMn_2O_4$ despite the substitution of $Fe^{3+}$. During the synthesis of $LiFe_yMn_{2-y}O_4$, as the sintering temperature and the doping amount of Fe(y=0.05, 0.1, 0.2)were increased, grain growth proceeded which in turn, showed a high crystalline and a large grain size, certain morphology with narrow specific surface area and large pore volume distribution was observed. In order to examine the ability for the practical use of the battery, charge-discharge tests were undertaken. When the substitution amount of $Fe^{3+}\;into\;LiMn_2O_4$ increased, the initial discharge capacity showed a tendency to decrease within the region of $3.0\~4.2V$ but when charge-discharge processes were repeated, other capacity maintenance properties turned out to be outstanding. In addition, when the sintering temperature was $800\~850^{\circ}C$, the initial capacity was small but showed very stable cycle performance. According to EVS(electrochemical voltage spectroscopy) test, $LiFe_yMn_{2-y}O_4(y=0,\;0.05,\;0.1,\;0.2)$ showed two plateau region and the typical peaks of manganese spinel structure when the substitution amount of $Fe^{3+}$ increased, the peak value at about 4.15V during the charge-discharge process showed a tendency to decrease. From the previous results, the local distortion due to the biphase within the region near 4.15V during the lithium extraction gave a phase transition to a more suitable single phase. When the transition was derived, the discharge capacity decreased. However the cycle performance showed an outstanding result.

Development of Matrix for the Immobilization of High Level Radioactive Waste : Study on the Synthesis of Ce-pyrochlore (고준위 핵페기물의 고정화를 위한 메트릭스 개발 : Ce파이로클로어 합성 연구)

  • ;;;Yudintsev, S. V²
    • Economic and Environmental Geology
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    • v.35 no.2
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    • pp.97-102
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    • 2002
  • Ce-pyrochlore (CaCe $Ti_2 $O_7)was synthesized to study its properties and phase relations in CaO-Ce $O_2$-Ti $O_2$ system because Ce-pyrochlore was known as a promising material for the immobilization of radioactive actinide. The samples were prepared from the high purity starling materials under the pressure of 200~400 kg/$\textrm{cm}^2$ at room temperature, and annealed at 1000~ 150$0^{\circ}C$. The Synthesized samples were analysed and indentified with XRD and SEM/EDS methods. The optimal formation condition of Ce-pyrochlore was at 130$0^{\circ}C$ under $O_2$ atmosphere and the chemical composition of it wasCa$Ca_{1-x}Ti_{2-y}O_{7-x-2y}$(x=0.03-0.05, y=0.02~0.04) At temperature between 130$0^{\circ}C$ 140$0^{\circ}C$, Ce-pyrochlore underwent rapidly the incongruent decomposition to perovskite. Ce-perovskite, a partial solid solution between perovskite and loparite (C $e_{0.66}$Ti $O_3$), was observed as a major phase above 140$0^{\circ}C$.>.

Synthesis of ferromagnetic Sm-Fe-N powders subjected to mechanochemical reaction (Mechanochemical Reaction에 의한 Sm-Fe-N계 자성분말의 합성)

  • 이충효;최종건;김판채
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.10 no.4
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    • pp.292-296
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    • 2000
  • Mechenochemical reaction by planetary type ball mill is applied to prepare $Sm_2$$Fe_{17}$$N_{x}$ permanent magnet powders. Starting from pure samarium and iron powders, the formation process of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ phase by ball milling and a subsequent solid state reaction were studied. At as-milled stage powders were found to consist of amorphous Sm-Fe and $\alpha$-Fe phases in all composition of $Sm_2$$Fe_{100-x}$(x = 11, 13, 15). The dependence of starting composition of elemental powder on the formation of Sm-Fe intermetallic compound was investigated by heat treatment of as-milled powders. When Sm concentration was 15 at%, heat-treated powder consists of mostly $Sm_2$$Fe_{17}$$N_{x}$single phase. For synthesizing of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ compound, additional nitriding treatment was carried out under $N_2$gas atmosphere at $450^{\circ}C$. The increase in the coercivity and remanence was parallel to the nitrogen content which increased drastically at first and then gradually as the nitriding time was extended. The ball-milled Sm-Fe-N powders were expected to be prospective materials for synthesizing of permanent magnet with high performance.

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Synthesis and Electrochemical Properties of (La0.6Sr0.4)(Co0.2Fe0.8)O3 cathode for SOFC on pH Control Using Modified Oxalate Method (Modified Oxalate Method 의해 합성한 SOFC용(La0.6Sr0.4)(Co0.2Fe0.8)O3 Cathode의 pH 변화에 따른 특성)

  • Lee, Mi-Jai;Choi, Byung-Hyun;Kim, Sei-Ki;Park, Sang-Sun;Lee, Kyung-Hee
    • Journal of the Korean Electrochemical Society
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    • v.10 no.4
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    • pp.288-294
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    • 2007
  • The LSCF cathode far Solid Oxide Fuel Cell was investigated to develop high performance unit cell at intermediate temperature by modified oxalate method with different electrolytes and different pH. The LSCF powders employed La, Sr, Co and Fe oxides, oxalic acid, ethanol and $NH_4OH$ solution were synthesized with pH controlled as 2, 6, 7, 8, 9 and 10 at $80^{\circ}C$ Single crystalline phase was obtained from pH $2{\sim}9$. on the other hand, $La_2O_3$ appeared from pH 10. Very fine powder with particle size of 50 nm was obtained at calcination temperature of $800^{\circ}C$ for 4 hours. LSCF cathode synthesized at pH 7 showed the highest electric conductivity in the temperature range of $600^{\circ}C$ to $900^{\circ}C$ its value was 950 S/cm at $900^{\circ}C$ Under same synthesis conditions, polarization resistance of each LSCF cathode was changed with different calcination temperatures. As-prepared powder presented 2.52, 1.54 and $2.58\;{\Omega}$ at $600^{\circ}C$ with ScSZ, 8Y-YSZ and GDC as its electrolyte respectively after calcination at $800^{\circ}C$ for 4 hours.

Synthesis of Garnet in the Ca-Ce-Gd-Zr-Fe-O System (Ca-Gd-Ce-Zr-Fe-O계에서의 석류석 합성 연구)

  • Chae Soo-Chun;Jang Young-Nam;Bae In-Kook;Yudintsev S.V.
    • Economic and Environmental Geology
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    • v.38 no.2 s.171
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    • pp.187-196
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    • 2005
  • Structural sites which cations can occupy in garnet structure are centers of the tetrahedron, octahedron, and distorted cube sharing edges with the tetrahedron and octahedron. Among them, the size of cation occuping at tetrahedral site (the center of tetrahedron) is closely related with the size of a unit cell of garnet. Accordingly, garnet containing iron with relative large ionic radii in tetrahedral site can be considered as a promising matrix for the immobilization of the elements with large ionic radii, such as actinides in radioactive wastes. We synthesized several garnets with the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$, and studied their properties and phase relations under various conditions. Mixed samples were fabricated in a pellet form under a pressure of $200{\~}400{\cal}kg/{\cal}cm^2$ and were sintered in the temperature range of $1100\~1400^{\circ}C$ in air and under oxygen atmospheres. Phase identification and chemical analysis of synthesized samples were conducted by XRD and SEM/EDS. In results, garnet was obtained as the main phase at $1300^{\circ}C$, an optimum condition in this system, even though some minor phases like perovskite and unknown phase were included. The compositions of garnet and perovskite synthesized from the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$ were ranged $[Ca_{l.2-1.8}Gd_{0.9-1.4}Ce_{0.3-0.5}]^{VIII}[Zr_{0.8-1.3}Fe_{0.7-1.2}]^{VI}[Fe_{2.9-3.1}]^{IV}O_{12}$ and $Ca_{0.1-0.5}Gd_{0.0-0.8}Ce_{0.1-0.5}\;Zr_{0.0-0.2}Fe_{0.9-1.1}O_3$, respectively. Ca content was exceeded and Ce content was depleted in the 8-coordinated site, comparing to the initial batch composition. This phenomena was closely related to the content of Zr and Fe in the 6-coordinated site.