• Title/Summary/Keyword: Solid state synthesis

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Synthesis of Electroactive Polythiophene Derivatives and Its Application for Biointerface (I) (전기적 활성을 갖는 폴리티오펜 유도체들의 합성과 생체계면에의 응용 (I))

  • 정선형;배진영;김지흥;정동준
    • Polymer(Korea)
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    • v.26 no.1
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    • pp.28-36
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    • 2002
  • In this study, we synthesized novel thiophene derivatives by the protection of the carboxyl group of 3-thiophene acetic acid with differently substituted benzyl groups. While 3-thiophene acetic acid is not electro-polymerizable, the modified monomers can be easily electro-oxidized to form stable electroactive polymers. The protecting groups can be easily removed in the solid state and the desired reactive carboxyl group can be introduced on the polymer surface. SEM observations show that obtained polymer films show a very good film surface and homogeneous morphology on the Pt electrode. After introduction of macromonomer, FT-IR spectrum shows new absorption bands at 1650 and $1550 cm^{-1}$, which is consistent with the formation of an amide bond. Electroactivity measurements were examined by cyclic voltammogram(CV). These polymers showed the characteristic electrochemical behavior of poly(3-alkylthiophene)s with reversible redox transition in the range of 0.7-0.9 V.

Optimization of $Nd^{3+}$ ion co-doping in $CaAl_2O_4:\;Eu^{2+}$ blue phosphor ($CaAl_2O_4:Eu^{2+}$ 청색(靑色) 형광체(螢光體)의 $Nd^{3+}$ 도핑 최적화(最適化)에 관한 연구(硏究))

  • Bartwal, Kunwar Singh;Ryu, Ho-Jin
    • Resources Recycling
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    • v.16 no.5
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    • pp.46-50
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    • 2007
  • Blue phosphor calcium aluminate, $CaAl_2O_4:Eu^{2+}$ co-doped with $Nd^{3+}$ was prepared by solid state synthesis method. Phosphor materials with 1 mol% $Eu^{2+}$ and varying compositions of $Nd^{3+}$ show high brightness and long persistent luminescence. The synthesized phosphor materials were investigated by powder x-ray diffraction (XRD), SEM, TEM, photoluminescence excitation and emission studies. Broad band UV excited luminescence of the $CaAl_2O_4:Eu^{2+}:Nd^{3+}$ was observed in the blue region (${\lambda}_{max}=440\;nm$) due to transitions from the $4f^65d^1$ to the $4f^7$ configuration of the $Eu^{2+}$ ion. $Nd^{3+}$ ion doping in the phosphor results in long afterglow phosphorescence when the excitation light is cut off.

Synthesis and Photoluminescence Properties of Dy3+- and Eu3+-codoped CaMoO4 Phosphors (Dy3+와 Eu3+ 이온이 동시 도핑된 CaMoO4 형광체의 합성과 발광 특성)

  • Kim, Junhan;Cho, Shinho
    • Journal of Surface Science and Engineering
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    • v.48 no.3
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    • pp.82-86
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    • 2015
  • $Dy^{3+}$- and $Eu^{3+}$-codoped $CaMoO_4$ Phosphors were synthesized by using the solid-state reaction method. The crystal structure, morphology, and optical properties of the resulting phosphor particles were investigated by using the X-ray diffraction, field-emission scanning electron microscopy, and photoluminescence spectroscopy. XRD patterns exhibited that all the synthesized phosphors showed a tetragonal system with a main (112) diffraction peak, irrespective of the content of $Eu^{3+}$ ions. As the content of $Eu^{3+}$ ions increased, the grains showed a tendency to agglomerate. The excitation spectra of the synthesized powders were composed of one strong broad band centered at 305 nm in the range of 220 - 350 nm and several weak peaks in the range of 350 - 500 nm resulting from the 4f transitions of activator ions. Upon ultraviolet excitation at 305 nm, the yellow emission line due to the $^4F_{9/2}{\rightarrow}^6H_{13/2}$ transition of $Dy^{3+}$ ions and the main red emission spectrum resulting from the $^5D_0{\rightarrow}^7F_2$ transition of $Eu^{3+}$ ions were observed. With the increase of the content of $Eu^{3+}$, the intensity of the yellow emission band gradually decreased while that of the red emission increased. These results indicated that the emission intensities of yellow and red emissions could be modulated by changing the content of the $Dy^{3+}$ and $Eu^{3+}$ ions incorporated into the host crystal.

Synthesis and Characterization of BaTiO3 Powder by Solid State Method (고상반응법을 이용한 BaTiO3 합성 및 특성 평가)

  • Kim, Yong Jin;Choi, Moon Hee;Shin, Hyo Soon;Ju, Byeong-Kwon;Chun, Myoung Pyo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.33 no.6
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    • pp.483-489
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    • 2020
  • BaTiO3 powder was synthesized by a solid-state reaction using BaCO3 and TiO2. Different calcination temperatures (800℃, 850℃, 900℃, and 950℃) were set to investigate their effects on the properties of BaTiO3 powder. The synthesized BaTiO3 phase was confirmed to be a single phase by XRD, and the tetragonality (c/a) and crystallite size were calculated. Thereafter, each calcinated BaTiO3 was sintered at five different sintering temperatures (1,100℃, 1,150℃, 1,200℃, 1,250℃, and 1,300℃), and the tetragonality, density, porosity, dielectric constant, and grain size were measured. As the calcination temperature increased, the tetragonality and crystallite size also increased, to 1.008 and 66 nm, respectively, at 950℃. Moreover, most pellets showed increased density, dielectric constant, and tetragonality as the sintering temperature increased up to 1,250℃; the same parameters slightly decreased at 1,300℃. It is noteworthy that the tetragonality of BaTiO3 at 1,250℃ exhibits a very high c/a value of 1.0084. In addition, the grain size and dielectric constant measured near the Curie temperature increased as the sintering temperature increased.

Synthesis and Optical Properties of BaSiO3:RE3+ (RE = Sm, Eu) Phosphors (BaSiO3:RE3+ (RE = Sm, Eu) 형광체의 합성과 광학 특성)

  • Cho, Shinho
    • Korean Journal of Materials Research
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    • v.29 no.6
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    • pp.356-362
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    • 2019
  • $BaSiO_3:RE^{3+}$ (RE = Sm or Eu) phosphor powders with different concentrations of activator ions are synthesized using the solid-state reaction method. The effects of the concentration of activator ions on the structural, photoluminescent, and morphological properties of the barium silicate phosphors are investigated. X-ray diffraction data reveals that the crystal structure of all the phosphors, regardless of the type and the concentration of the activator ions, is an orthorhombic system with a main (111) diffraction peak. The grain particles agglomerate together to form larger clusters with increasing concentrations of activator ions. The emission spectra of the $Sm^{3+}$-doped $BaSiO_3$ phosphors under excitation at 406 nm consist of an intense orange band at 604 nm and three weak bands centered at 567, 651, and 711 nm, respectively. As the concentration of $Sm^{3+}$ increases from 1 to 5 mol%, the intensities of all the emission bands gradually increase, reach maxima at 5 mol% of $Sm^{3+}$ ions, and then decrease significantly with further increases in the $Sm^{3+}$ concentration due to the concentration quenching phenomenon. For the $Eu^{3+}$-doped $BaSiO_3$ phosphors, a strong red emission band at 621 nm and several weak bands are observed. The optimal orange and red light emissions of the $BaSiO_3$ phosphors are obtained when the concentrations of $Sm^{3+}$ and $Eu^{3+}$ ions are 5 mol% and 15 mol%, respectively.

Fabrication and magnetic properties of hexagonal BaFe12O19 ferrite obtained by magnetic-field-assisted hydrothermal process

  • Zhang, Min;Dai, Jianming;Liu, Qiangchun;Li, Qiang;Zi, Zhenfa
    • Current Applied Physics
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    • v.18 no.11
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    • pp.1426-1430
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    • 2018
  • High magnetic field effects on the microstructure and magnetic properties of $BaFe_{12}O_{19}$ hexaferrites synthesized hydrothermal method have been investigated. The obtained results indicate that the lattice constant decreases gradually as the magnetic field strength increases, which may be attributed to the lattice distortion resulted from the high magnetic field. Polycrystalline $BaFe_{12}O_{19}$ samples prepared under magnetic field strength at zero and 5 T are single phase. It is found that application of external magnetic field during synthesis can induce orientated growth of the hexaferrite crystals along the easy magnetic axis. The magnetic properties can be effectively regulated by an application of high magnetic fields. It is observed that the $BaFe_{12}O_{19}$ prepared under a 5 T magnetic field exhibits a higher room-temperature saturation magnetization (66.3 emu/g) than that of the sample (43.6 emu/g) obtained without magnetic field. The results can be explained as the enhanced crystalline, improvement of $Fe^{3+}$ ions occupancy and the oriented growth induced by the external magnetic field. The growing orientation of particles gives rise to increased coercivity due to the enhancement in shape anisotropy. It is expected that an application of magnetic field during the formation of magnetic nanoparticles could be a promising technique to modify magnetic properties with excellent performance.

Research on Afterglow Brightness of Sr4-(x+y+z)Al14O25 : Eux, Dyy, Agz by Solid State Synthesis (고상법으로 합성한 Sr4-(x+y+z)Al14O25 : Eux, Dyy, Agz계 축광성 형광체 장잔광의 연구)

  • Kim, Seung-woo;Kim, Jung-sik
    • Korean Journal of Metals and Materials
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    • v.49 no.4
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    • pp.348-354
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    • 2011
  • Long-lasting brightness $Sr_{4}Al_{14}O_{25}$ : $Eu^{2+}$, $Dy^{3+}$, $Ag^{+}$ phosphor was synthesized by modified solid state reaction and its photoluminescence was investigated. $Sr(NO_3)_{2}$ and $Al(NO_3)_3{\cdot}9H_{2}O$ as starting materials, and $B_{2}O_{3}$ as a flux were mixed with $Eu_{2}O_{3}$ as an activator, $Dy_{2}O_{3}$ as a coactivator, and $AgNO_{3}$ as a charge compensator. The crystalline of target powder showed a single-phase $Sr_{4}Al_{14}O_{25}$ by the XRD characterization and the average particle size was about 20-30 ${\mu}m$ from the FE-SEM observation. $Ag^{+}$ ion doping effects (0-0.06 mol) on $Sr_{4}Al_{14}O_{25}:Eu^{2+},\;Dy^{3+},\;Ag^{+}$ phosphor were measured by photoluminescence spectrometer and luminescence meter. The of photoluminescence intensity of the $Sr_{3.64}Al_{14}O_{25}:Eu_{0.11},\;Dy_{0.22},\;Ag_{0.03}$ phosphor was higher than other compositions and afterglow brightness was 0.186 $cd/m^{2}$.

Direct Microwave Sintering of Poorly Coupled Ceramics in Electrochemical Devices

  • Amiri, Taghi;Etsell, Thomas H.;Sarkar, Partha
    • Journal of Electrochemical Science and Technology
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    • v.13 no.3
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    • pp.390-397
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    • 2022
  • The use of microwaves as the energy source for synthesis and sintering of ceramics offers substantial advantages compared to conventional gas-fired and electric resistance furnaces. Benefits include much shorter processing times and reaching the sintering temperature more quickly, resulting in superior final product quality. Most oxide ceramics poorly interact with microwave irradiation at low temperatures; thus, a more complex setup including a susceptor is needed, which makes the whole process very complicated. This investigation pursued a new approach, which enabled us to use microwave irradiation directly in poorly coupled oxides. In many solid-state electrochemical devices, the support is either metal or can be reduced to metal. Metal powders in the support can act as an internal susceptor and heat the entire cell. Then sufficient interaction of microwave irradiation and ceramic material can occur as the sample temperature increases. This microwave heating and exothermic reaction of oxidation of the support can sinter the ceramic very efficiently without any external susceptor. In this study, yttria stabilized zirconia (YSZ) and a Ni-YSZ cermet support were used as an example. The cermet was used as the support, and a YSZ electrolyte was coated and sintered directly using microwave irradiation without the use of any susceptor. The results were compared to a similar cell prepared using a conventional electric furnace. The leakage test and full cell power measurement results revealed a fully leak-free electrolyte. Scanning electron microscopy and density measurements show that microwave sintered samples have lower open porosity in the electrode support than conventional heat treatment. This technique offers an efficient way to directly use microwave irradiation to sinter thin film ceramics without a susceptor.

Synthesis and luminescent properties of $Sr_2SiO_4:Eu^{2+}$ phosphors ($Sr_2SiO_4:Eu^{2+}$ 형광체의 합성 및 발광특성)

  • Kim, Jong-Min;Park, Yong-Seo;Choi, Hyung-Wook
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.430-431
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    • 2009
  • In this study, europium doped strontium silicate ($Sr_2SiO_4:Eu^{2+}$) phosphor has been synthesized by conventional solid-state method and investigated luminescent characteristic. $SrCO_3$ and $SiO_2$ were mixed together by 2:1 mole ratio. Also $NH_4Cl$ was added as a flux. The mixture were sintered at $800^{\circ}C$, $1000^{\circ}C$ for 3h under the atmosphere (5% $H_2$/95% $N_2$). This phosphor can be applicated to the yellow phosphor for white LED because it has yellow emission band (540nm), which emits efficiently under the 370nm excitaion energy.

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Synthesis of Poly-$N^5$-(3-hydroxypropyl glutamine)/Poly (ethylene glycol)block Copolymer Hydrogel and Its Application to the Artificial Skin (Poly-$N^5$-(3-hydroxypropyl glutamine)/Poly (ethylene glycol)block copolymer hydrogel의 합성과 인공피부에의 응용)

  • 조종수;오상봉
    • Journal of Biomedical Engineering Research
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    • v.12 no.1
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    • pp.57-62
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    • 1991
  • ABA type block copolymers composed of poly($\gamma-benzyl$ L-glutamate) (PBLG) as the A component and poly (ethylene glycol) as the B component were obtained by polymerization of $\gamma-benzyl$ L-gletamate N -carboxyanhydride, initiated by amino groups at both ends of poly(ethylene glycol) . From circular dichroism measurements in ethylene dichloride solution as well as from infrared spectTa measurements in solid state, it was found that the polypep- tide block exists in the a-helical conformation, as in PBLG homopolymer. $Poly-N^5$ (3-hydroxypropyl glutamine) (PHPG)/poly(ethylene glycol)block copolymer hydrogel was obtained by the treatment of PBLG/PBG block copolymer with the mixture of 3-ammine-1-propanol and diamlnooctane. The water content of PHPG/PEG block copolymer hydrogel was about 80wt% when the concentration of crosslinking agent was below 5 mole % per polymer.

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