• Bulletin of the Korean Chemical Society
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• v.20 no.3
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• pp.355-361
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• 1999

To improve the volatility and stability of lead complexes, the principle of stabilization by saturating the metal coordination sphere by intramolecular coordination through a β-diketonates with an ethereal group has was tested. Several new lead complexes with alkoxyalkyl-substituted β-diketonates, Pb(R1C(O)CHC(O)(CH2)3OR2)2(Rl=t-Bu, Me, OMe, i-Pr, R2=Me, Et), or carboxylate, Pb(OC(O)(CH2)3OEt)2, were prepared by the reaction between Pb(OAc)2 and corresponding alkoxyalkyl-substituted β-diketonates, and they were found to have a viscous liquid phase. The nature of the head (β-diketonate or carboxylate) or tails and substituents of β-diketonates appeared not to be important for the formation of the liquid phase. It is worth mentioning that Pb(OAc)2, which has limited use due to its low solubility, was successfully adopted as a starting material for the preparation of new lead complexes. Easy hydrolysis, reaction with HCl, and 13C NMR spectra indicated that tail portions were not coordinated to the metal as a copper derivative, Cu(t-BuC(O)CHC(O)(CH2)3OMe)2. All these complexes were not volatile enough for the MOCVD experiments, but a methyl derivative, Pb(MeC(O)CHC(O)(CH2)3OEt)2, showed some sublimation. The methoxy derivative, Pb(MeOC(O)CHC(O)(CH2)3OEt)2, was thermally unstable due to possible equilibrium between species coordinating with a keto oxygen atom and an ethereal atom of a methoxy group, which was confirmed by IR and 13C NMR spectra.

• Journal of the Korean Ceramic Society
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• v.32 no.3
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• pp.305-312
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• 1995

Thin films of Pb(Mg, Zn)1/3Nb2/3O3 were fabricated by spin coating the Pb-Mg-Zn-Nb-O complex alkoxide sols on(111) Pt-coated MgO (100) planes. It was observed that the content of H2O and the rheological characteristics of sol greatly influenced the orientation of perovskite grains after thin-film formation. A strong preferential orientation of (100)-type planes of the perovskite grains was obtained for the sol aged for 15 days with the molar ratio of H2O to total metal alkoxides=2. As small angle X-ray scattering experiment in the Porod region was performed to correlate the observed preferential orientation with the network structure of precursors at various stage of aging. It was shown that the degree of branching of the Pb-Mg-Zn-Nb-O precursor chain had a direct effect on the preferred oreintation, and weakly branched precursor systems led to highly oriented grains after thin-film formation.

• Current Photovoltaic Research
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• v.6 no.1
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• pp.12-16
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• 2018

The interest in perovskite solar cells has been skyrocketed owing to their rapid progress in efficiency in recent years. Here, we report the effect of non-stoichiometry in the methylammonium lead trihalide ($MAPbI_3$) precursors used in a solution process with different MAI : $PbI_2$ ratios of 1 : 0.96, 1 : 1.10, 1 : 1.15, and 1:1.20. With an increase in the $PbI_2$ content, the $PbI_2$ secondary phase was found to form at grain boundary region of perovskite thin films, as evidenced by X-ray diffraction (XRD) and scanning electron microscopy (SEM). In terms of device performance, open-circuit voltage in particular is significantly improved with increasing the molar ratio of $PbI_2$, which is possibly ascribed to the reduction in recombination sites at grain boundary of perovskite and hence the prolonged life time of light-generated carriers according to the reported. As a result, the $PbI_2-excess$ devices exhibited a higher power conversion efficiency compared to the MAI-excess ones.

• Bulletin of the Korean Chemical Society
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• v.30 no.5
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• pp.1135-1138
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• 2009

Hollow Sn and Pb nanoparticles have been prepared by a rapid injection of an aqueous solution of $SnCl_2$- poly(vinylpyrrolidone) (PVP, surfactant) and $Pb(OAc)_2${\cdot}$3H_2O-PVP$ into an aqueous solution of sodium borohydride (reducing agent) in simple, one-pot reaction at room temperature under an argon atmosphere, respectively. The two hollow nanoparticles have been fully characterized by TEM, HRTEM, SAED, XRD, and EDX analyses. Upon exposure to air, the black Pb hollow nanoparticles are gradually transformed into a mixture of Pb, litharge (tetragonal PbO), massicot (orthorhombic PbO), and $Pb_5O_8$. The order and speed of mixing of the reactants between the metal precursor-PVP and the reductant solutions and stoichiometry of all the reactants are crucial factors for the formation of the two hollow nanocrystals. The Sn and Pb hollow nanoparticles were produced only when 1:(1.5-2) and 1:3 ratios of the Sn and Pb precursors to $NaBH_4$ were employed with a rapid injection, respectively.

• Journal of the Korean Ceramic Society
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• v.28 no.11
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• pp.892-896
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• 1991

The cyrstallization behavior of lead titanate powders prepared by sol-gel and coprecipitation techniques was investigated. The lead titanate precursors were derived from a mixed solution of lead nitrate and titanium tetrachloride at 4$0^{\circ}C$ to 43$^{\circ}C$ and pH of 9.00 to 9.75. The X-ray diffraction patterns of the dried gel and coprecipitated powders showed it to be amorphous. DTA runs of the powders indicated crystallization to occur at 475~48$0^{\circ}C$. However, the amorphous powders were partially crystallized at 400~45$0^{\circ}C$ with sufficient annealing time. The room temperature Raman spectra from heat-treated powders changed continuously from amorphous to crystalline state with increasing heat-treating temperature. By annealing coprecipitated powders, a dramatic change in the Raman spectra due to the structural relaxation as the annealing temperatures increased, was clearly visible. i.e., coprecipitated, gel, and crystalline structure, in turn.

• Progress in Superconductivity
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• v.4 no.2
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• pp.157-161
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• 2003

We have performed the electrochemical method to fabricate high temperature superconducting (TlPbBi) -(SrBa)-Ca-Cu-O films. The precursors of the superconducting sample were codeposited at a periodic pulsed-potential cycle (1 second at -4V and 1 second at -1V) on a silver substrate. The variation of structure, microstructure and element were analysed by ICP and SEM techniques. The specimens were consisted predominantly of the Tl-1212 phase and have a transition temperature of 80～87 K in low magnetic field. It was showed that each grain has the stoichiometric ratio of $T1_{0.7}$Pb_$Bi_{0.3}$ $_Sr{0.1}$ $Ba_{2.4}$ $Ca_{0.2}$ $Cu_{1.2}$ $2.5/O_{x}$ by EDX analysis.sis.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.04a
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• pp.17-20
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• 2002

The effects of relatively low lead content (0.2~0.3) on the 2223 phase formation and transport property of Bi-2223/Ag tapes have been investigated. The results show that lead contents have great impact on the phase assemblage of precursors, subsequently, on the phase formation and transport property of silver sheathed BSCCO-2223 tapes. Powders containing Pb=0.25 and Pb=0.3 resulted in the nearly identical $J_c$ values in fully processed tapes, but leaded to significant difference on the phase formation process. For the case of Pb=0.2, both low conversion fraction of 2212 to 2223 and low $J_c$ value were obtained in final reacted tape, which was probably due to lack of enough liquid phase to facilitate the phase transformation.

• Bulletin of the Korean Chemical Society
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• v.33 no.7
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• pp.2305-2308
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• 2012

Perovskite structured barium titanate particles ($BaTiO_3$) platelets were synthesized by molten salt synthesis and topochemical microcrystal conversion. As the precursors of $BaTiO_3$, plate-like $BaBi_4Ti_4O_{15}$ particles were first synthesized by the reaction of $Bi_4Ti_3O_{12}$, $BaCO_3$, and $TiO_2$ at $1080^{\circ}C$ for 3 h in $BaCl_2$-KCl molten salt. After the topochemical reactions, layer-structured $BaBi_4Ti_4O_{15}$ particles transformed to the perovskite $BaTiO_3$ platelets. $BaTiO_3$ particles with thickness of approximately $0.5{\mu}m$ and a length of $10-15{\mu}m$ retained the morphology feature of the $BaBi_4Ti_4O_{15}$ precursor. For <001> $Pb(Mg_{1/3}Nb_{2/3})O_3-32.5PbTiO_3$ (PMNT)-5 wt % PbO piezoelectric ceramics textured with 5 vol % of $BaTiO_3$ templates, the Lotgering factor reached 0.82, and $d_{33}$ was 870 pC/N.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.6 no.6
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• pp.457-460
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• 2005

Nano-sized titanium oxide and zirconium oxide powders were synthesized by hydrolysis of titanium isopropoxide $[Ti(OC_3H7)_4]$ and zirconium tetrachloride ($ZrC1_4$) via a sol-gel technique. Lead titanate powders were prepared by mixing $TiO_2$ precursors with PbO slurry made with dilute $NH_4OH$. Lead zirconate titanate powders were, then, synthesized by mixing $PbTiO_3$ with $ZrO_2$ powders. The goal of this research was to obtain the $PbZrTiO_3(PZT)$ powders and sintering these powders at low temperature. The $PbTiO_3$ and PZT powders after firing were analyzed by X-ray diffraction(XRD) and transmission electron microscopy(TEM) was utilized to observe the shape and size of the synthesized nano-particles. In the XRD pattern, the well-crystallized PZT phase could be obtained in consequence of firing at $900^{\circ}C$. SEM micrographs also showed that grains of PZT were relatively well grown with the size of the range of $2{\~}4{\mu}m$. The densified perovskite structure of $PbZrTiO_3$ could be obtained by sintering at temperature as low as $900^{\circ}C$. Characterization of the samples showed improved piezoelectric properties.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.05a
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• pp.69-72
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• 2003

Bi-2223 superconducting wires were fabricated by stacking, drawing process with different precursor powders and different heat-treatment histories. The precursor powders were 2 kinds of Pb content. And a part of the tapes were experienced pre-annealing process which caused tetragonal structure of Bi-2212 phase to orthorhombic structure of it was during drawing process. We confirmed the transformation of Bi-2212 phase from tetragonal structure to orthorhombic structure and reduction of second phases. XRD and DC magnetization analysis were performed in order to investigate the fraction of Bi-2223 phase in Bi-2223/Ag HTS tape. We could achieve best Ic of 70 A class at the Bi-2223/Ag tape using low Pb content of precursor powder and experienced pre-annealing process. DC magnetization analysis was useful to investigate the fraction of Bi-2223 phase in the Bi-2223/Ag tape.