• 분석과학
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• 제10권1호
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• pp.18-30
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• 1997

Si / Al비가 130 정도인 Na, TPA-ZSM-5를 저온 상압법으로 합성하였으며, 이들의 결정화 과정을 XRD, XRF, FT-IR, NMR 및 SEM을 이용하여 고찰하였다. 결정의 형성과정은 autoclave법과는 다소 다르게 나타났으나 최종 생성물의 분광학적 특성은 전형적인 ZSM-5 영역에서 나타났다. 또한 반응 도중 생성된 국부결함은 소성에 의해 제거됨을 알 수 있었으며, 저온상압하에서도 반응시간을 48시간 이내로 단축할 수 있음을 알 수 있었다.

• 대한화학회지
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• 제40권10호
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• pp.656-662
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• 1996

저온상압법에 의해 Si/Al의 비가 100정도되는 ZSM-5를 합성하였으며 시간 경과에 따른 결정화과정을 $^{27}Al$ 및 $^{29}Si$ MAS NMR spectea 및 FT-IR로 고찰하였다. 저온상압 하에서 합성한 결과 초기 반응물질 및 성분비에 따라 화학적 이동은 기종의 연구와는 다른 경향을 보였으나 반응이 진행됨에 따라 최종 생성물의 화학적 이동은 전형적이 ZSM-5 영역에서 나타나고 있음을 확인하였다. 그리고 국부결함은 소성에 의해 제거되었으며 최종생성물의 XRD 및 SEM의 결과에서도 합성된 물질이 ZSM-5임을 확인하였다.

• 한국재료학회지
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• 제30권7호
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• pp.338-342
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• 2020

Tin oxide (SnO₂) nanocrystals are synthesized by a thermal evaporation method using a mixture of SnO₂ and Mg powders. The synthesis process is performed in air at atmospheric pressure, which makes the process very simple. Nanocrystals with a belt shape start to form at 900 ℃ lower than the melting point of SnO₂. As the synthesis temperature increases to 1,100 ℃, the quantity of nanocrystals increases. The size of the nanocrystals did not change with increasing temperature. When SnO₂ powder without Mg powder is used as the source material, no nanocrystals are synthesized even at 1,100 ℃, indicating that Mg plays an important role in the formation of the SnO₂ nanocrystals at temperatures as low as 900 ℃. X-ray diffraction analysis shows that the SnO₂ nanocrystals have a rutile crystal structure. The belt-shaped SnO₂ nanocrystals have a width of 300~800 nm, a thickness of 50 nm, and a length of several tens of micrometers. A strong blue emission peak centered at 410 nm is observed in the cathodoluminescence spectra of the belt-shaped SnO₂ nanocrystals.

• Bulletin of the Korean Chemical Society
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• 제30권12호
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• pp.2921-2926
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• 2009

Cu-BTC[$Cu_3(BTC)_2(H_2O)_3$, BTC = 1,3,5-benzenetricarboxylate], one of the most well-known metal-organic framework materials (MOF), has been synthesized under atmospheric pressure and room temperature by using ultrasound. The Cu-BTC can be obtained in 1 min in the presence of DMF (N,N-dimethylformamide), suggesting the possibility of continuous production of Cu-BTC. Moreover, the surface area and pore volume show that the concentration of DMF is important for the synthesis of Cu-BTC having high porosity. The morphology and phase also depend on the concentration of DMF : Cu-BTC cannot be obtained at room temperature in the absence of DMF and aggregated Cu-BTC (with low surface area) is produced in the presence of high concentration of DMF. It seems that the deprotonation of benzenetricarboxylic acid by base (such as DMF) is inevitable for the room temperature syntheses.

• Bulletin of the Korean Chemical Society
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• 제21권7호
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• pp.679-684
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• 2000

The Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 compounds, both with Ruddlesden-Popper structures, have been synthesized by the ceramic method at $1150^{\circ}C$ under atmospheric pressure. The crystallographic structure of the compounds was assigned to the tetr agonal system with space group 14/mmm by X-ray diffraction(XRD) Rietveld refinement. The reduced lattice volume and lattice parameters increased as the Ta with 5d substitutes for the Nb with 4d in the compounds. The Co/Nb(Ta)O bond length has been determined by X-ray absorption spectroscopic(EXAFS/XANES) analysis and the XRD refinement. The CoO6,octahedra were tetragonally distorted by elongation of Co-O bond along the c-axis. The magnetic measurement shows the compounds Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 have paramagnetic properties and the Co ions with intermediate spin sates between high and low spins in D4h symmetry. All the compounds showed semiconducting behavior whose electrical conductivity increased with temperature up to 1000 K. The electrical conductiviy increased and the activation energy for the conduction decreased as the number of perovskite layers increased in the compounds with chemical formula An+1BnO3n+1.

• 폴리머
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• 제39권2호
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• pp.225-234
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• 2015

In this study, we proposed to synthesize thermally stable, soluble and conjugated Schiff base polymer (SbP). For this reason, a specific molecule namely 4,4'-thiodiphenol which has sulfur and oxygen bridge in its structure was used to synthesize bi-functional monomers. Bi-functional amino and carbonyl monomers namely 4,4'-[thio-bis(4,1-phenyleneoxy)] dianiline (DIA) and 4,4'-[thiobis(4,1-phenyleneoxy)]dibenzaldehyde (DIB) were prepared from the elimination reaction of 4,4'-thiodiphenol with 4-iodonitrobenzene and 4-iodobenzaldehyde, respectively. The structures of products were confirmed by elemental analysis, FTIR, $^1H$ NMR and $^{13}C$ NMR techniques. The molecular weight distribution parameters of SbP were determined by size exclusion chromatography (SEC). The synthesized SbP was characterized by solubility tests, TG-DTA and DSC. Also, conductivity values of SbP and SbP-iodine complex were determined from their solid conductivity measurements. The conductivity measurements of doped and undoped SbP were carried out by Keithley 2400 electrometer at room temperature and atmospheric pressure, which were calculated via four-point probe technique. When iodine was used as a doping agent, the conductivity of SbP was observed to be increased. Optical band gap ($E_g$) of SbP was also calculated by using UV-Vis spectroscopy. It should be stressed that SbP was a semiconductor which had a potential in electronic and optoelectronic applications, with fairly low band gap. SbP was found to be thermally stable up to $300^{\circ}C$. The char of SbP was observed 29.86% at $1000^{\circ}C$.

• Bulletin of the Korean Chemical Society
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• 제17권9호
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• pp.794-798
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• 1996

Solid solutions of the nonstoichiometric Dy1-xSrxCoO3-y system with the compositions of x=0.00, 0.25, 0.50, 0.75, and 1.00 have been synthesized by the solid state reaction at 1000 ℃ under atmospheric air pressure. The crystallographic structures of the solid solutions are analyzed by the powder X-ray diffraction patterns at room temperature. The analyses assign the compositions of x=0.00 and 0.25 to the orthorhombic system with space group of Pbnm/D2h16, the compositions of x=0.50 and 0.75 to the tetragonal system like a typical SrCoO2.86, and the composition of x=l.00 or SrCoO2.50 to the brownmillerite type system with space group of I**a. The reduced lattice volumes increase with x value due to the larger radius of Sr2+ ion than that of Dy3+ ion. The mole ratio of Co4+ ion to total Co ion with mixed valence state between Co3+ and Co4+ ions at B sites or τ value has been determined by an iodometric titration. All the samples except for the DyCoO3 compound show the mixed valnce state and thus the composition of x=0.50 has the maximum τ value in the system. The oxygen vacancies increasing with x value are randomly distributed over the crystal lattice except for the composition of x=l.00 which have the ordering of the oxygen vacancies. The nonstoichiometric chemical formulas of the Dy1-xSrxCo3+1-τCo4+τO3-(x-τ)/2 system are formulated from the x, τ, and y values. The electrical conductivity in the temperature range of 100 to 900 K increases with τ value linearly because of positive holes of the Co4+ ions in π* band as a conducting carrier. The activation energy of the x=0.50 as Ea=0.17 eV is minimum among other compouds. Broad and high order transition due to the overlap between σ* and π* bands broadened by the thermal activation is observed near 1000 K and shows a low temperature-semiconducting behavior. Magnetic properties following the Currie-Weiss law show the low to high spin transition in the cobaltate perovskite. Especially, the composition of x=0.75 presents weak ferromagnetic behavior due to the Co3+-O2--Co4+ indirect superexchange interaction.