• 대한화학회지
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• 제62권2호
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• pp.118-123
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• 2018

The hexagonal tungsten bronze $Cs_xWO_3$ nanoparticle was synthesized by a chemical coprecipitation method of ammonium tungstate and $Cs_2CO_3$ in acidic condition. This synthetic method for cesium tungsten bronze is reported for the first time as far as we know. The synthesized $Cs_xWO_3$ as precipitated showed a weak crystallinity of hexagonal unit cell with a crystallite size of about 4 nm without annealing. When the synthesized $Cs_xWO_3$ was annealed in $N_2$ atmosphere, the crystallinity and crystallite size systematically increased maintaining the typical hexagonal tungsten bronze structure as the annealing temperature increased. The analyzed Cs content in the bronze was about 0.3 vs W, which is very close to the theoretical maximum value, 1/3 in cesium tungsten bronze. According to XPS analysis, the reduced tungsten ions existed as both the forms of $W^{5+}$ and $W^{4+}$ and the contents systematically increased as the annealing temperature increased up to $800^{\circ}C$. The $Cs_xWO_3$ thin films on PET substrate were also prepared by a wet-coating method using the ball-milled solution of the annealed $Cs_xWO_3$ nanoparticles at various temperatures. The near-infrared shielding property of these thin films increased systematically as the annealing temperature increased up to $800^{\circ}C$ as expected with the increased contents of reduced tungsten ions.

• 한국재료학회지
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• 제22권12호
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• pp.711-716
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• 2012

Tungsten bronze structure $Sr_{1-x}Ba_xNb_2O_6$ (SBN) single crystals were grown primarily using the Czochralski method, in which several difficulties were encountered: striation formation and diameter control. Striation formation occurred mainly because of crystal rotation in an asymmetric thermal field and unsteady melt convection driven by thermal buoyancy forces. To optimize the growth conditions, bulk SBN crystals were grown in a furnace with resistance heating elements. The zone of $O_2$ atmosphere for crystal growth is 9.0 cm and the difference of temperature between the melt and the top is $70^{\circ}C$. According to the growth conditions of the rotation rate, grown SBN became either polycrystalline or composed of single crystals. In the case of as-grown $Sr_{1-x}Ba_xNb_2O_6$ (x = 0.4; 60SBN) single crystals, the color of the crystals was transparent yellowish and the growth axis was the c-axis. The facets of the crystals were of various shapes. The length and diameter of the single crystals was 50~70 mm and 5~10 mm, respectively. Tungsten bronze SBN growth is affected by the temperature profile and the atmosphere of the growing zone. The thermal expansion coefficients on heating and on cooling of the grown SBN single crystals were not matched. These coefficients were thought to influence the phase transition phenomena of SBN.

• Bulletin of the Korean Chemical Society
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• 제34권3호
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• pp.731-734
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• 2013

Reduced tungsten bronze nanoparticles of ternary and quaternary compounds were prepared by adding sodium and cesium to crystal structures of tungsten trioxides ($Na_xCs_{0.33-x}WO_3$, x = 0, 0.11) while maintaining the overall alkali metal fraction at 0.33, in an attempt to control near infrared (NIR) shielding property in the particular wavelength range of 780 to 1200 nm. The structure and composition analysis of the quaternary compound, $Na_{0.11}Cs_{0.22}WO_3$, revealed that 93.1% of the hexagonal phase was formed, suggesting that both alkali metals were mainly inserted in hexagonal channel. The NIR shielding property for $Na_{0.11}Cs_{0.22}WO_3$ was remarkable, as this material demonstrated efficient transmittance of visible light up to 780 nm and enhancement in NIR shielding because of the blue-shifted absorption maximum in comparison to $Cs_{0.33}WO_3$.

• 한국세라믹학회지
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• 제38권12호
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• pp.1167-1173
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• 2001

텅스텐브론즈 구조를 가지는 Sr$_{x}Ba_{1-x}Nb_{2}O_{6}$(SBN) (0.3$\le$x$\ge$0.7) 세라믹스를 고상반응법으로 합성하고 Sr/Ba의 비에 따른 유전특성을 조사하였다. SBN 세라믹스는 Sr/Ba의 비가 증가함에 따라 상전이 온도는 낮아지고 상전이 온도에서의 최대 유전율은 증가하였다. 또한 SBN 세라믹스는 Sr 함량에 따른 relaxor 거동을 정량화하여 평가하였는데, Sr/Ba의 비가 증가할수록 유전율은 더욱 완만해지는 것을 관찰할 수 있었다. 이러한 실험 결과를 텅스텐브론지 구조를 가진 SBN 세라믹스의 결정구조 관점에서 해석하였다.

• The Korean Journal of Ceramics
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• 제6권4호
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• pp.380-384
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• 2000

Crystal structure of $Ba_5-5X$Y$_10/3$Nb$_10$O$_30$ was tried to determine by Rietveld analysis using powder X-ray diffraction data. This compound has tetragonal tungsten bronze (TTB) structure with general formula, (Al)$_2$(A2)$_4$(B1)$_2$(B2)$_8$(O1)$_8$(O2)$_8$(O3)$_4$(O4)$_2$(O5)$_4$(O6)$_4$. However, it was difficult to determine the distribution of Ba and Y in Al and A2 sites by the analysis only. Combination of Rietveld analysis and site potentials calculation as well as lattice energy calculations helped to determine the distribution. As the result, it was clarified that $Ba^2+$ cations occupy A2 (pentagonal tunnel site) and $Y^3+$ cations occupy Al (cubic site). The distribution of cations at each site coincides with the distribution estimated by the difference of ionic radii. This supports the formation condition of TTB which was proposed in our previous report. $Ba_5-5X$Y$_10X/3$Nb$_10$O$_30$ shows ferroelectric characteristics. In this compound, remanent polarization decreases slightly with the composition X. On the other hand, the result of crystal structure determination reveals that atomic positions along c-axis for A1, A2, B1 and B2 cations are also decreased with the composition X. This would suggest that the dependence of remanent polarization on composition X is derived by the dependence of atomic coordinates on composition X.

• 한국분말재료학회지
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• 제26권1호
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• pp.28-33
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• 2019

The gas sensor is essential to monitoring dangerous gases in our environment. Metal oxide (MO) gas sensors are primarily utilized for flammable, toxic and organic gases and $O_3$ because of their high sensitivity, high response and high stability. Tungsten oxides ($WO_3$) have versatile applications, particularly for gas sensor applications because of the wide bandgap and stability of $WO_3$. Nanosize $WO_3$ are synthesized using the hydrothermal method. As-prepared $WO_3$ nanopowders are in the form of nanorods and nanorulers. The crystal structure is hexagonal tungsten bronze ($MxWO_3$, x =< 0.33), characterized as a tunnel structure that accommodates alkali ions and the phase stabilizer. A gas detection test reveals that $WO_3$ can detect acetone, butanol, ethanol, and gasoline. This is the first study to report this capability of $WO_3$.

• The Korean Journal of Ceramics
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• 제6권3호
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• pp.272-275
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• 2000

Starting from the stoichiometric composition of $K_2$CO$_3$: Li$_2$CO$_3$: Nb$_2$O$_5$=3 : 2 : 5 with the mole ratio, $K_3$LiNb$_6$O$_17$ 17/ single crystals were grown using the Czochralski method. Although the starting melt composition corresponds to the $K_3$Li$_2$Nb$_5$O$_15$ crystals, the chemical composition of the as grown crystals appears to be $K_2.95$Li$_1.33$Nb$_6.17$O$_17$ or $K_2.60$Li$_1.17$Nb$_{5.44}$ 5.44/O$_{15}$ which relatively contain fewer Li ions than $K_3$Li$_2$Nb$_5$O$_15$ crystals. We investigated the influence of the deficiency of the Li ions in the tetragonal tungsten bronze structure through the measurements of DE loop, temperature dependent dielectric constant, differential thermal analysis and temperature dependent X-ray diffraction pattern.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2003년도 하계학술대회 논문집 Vol.4 No.2
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• pp.739-743
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• 2003

[ $Ba_2NaNb_5O_{15}$ ], hereafter BNN, thin films are attractive candidates for nonvolatile memory and electro-optic devices. In the present work, thin films that have different contents of Ba, Nb and Na have been prepared by H-MOD technique on silicon and Pt substrates. XRD and SEM were used to investigate the phase evolution behavior and the microstructure of the films. It was found that the films of about 500nm thick were crack-free and uniform in microstructure. Nb content strongly influenced the phase formation of the films, where unwanted phases were always formed at the stoichiometric BNN composition. However, the unwanted phases decreased with the increase of excess Nb content, and the single phase (tetragonal tungsten bronze structure) BNN thin film was obtained when the niobium content reached some point. From this study, the sub-solidus phase diagram below $850^{\circ}C$ for $BaO-Na_2O-Nb_2O_5$ ternary system is proposed.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2003년도 제5회 영호남 학술대회 논문집
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• pp.98-102
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• 2003

$Ba_2NaNb_5O_{15}$, hereafter BNN, thin films are attractive candidates for nonvolatile memory and electro-optic devices. In the present work, thin films that have different contents of Ba, Na and Nb have been prepared by H-MOD technique on silicon and Pt substrates. XRD and SEM were used to investigate the phase evolution behavior and the microstructure of the films. It was found that the films of about 450nm thick were crack-free and uniform in microstructure. Nb content strongly influenced the phase formation of the films, where low temperature phase was always formed at the stoichiometric BNN composition. However, the amount of low temperature phase decreased with the increase of excess Nb content, and the single phase (orthorhombic tungsten bronze structure) BNN thin film was obtained at the temperature as low as $750^{\circ}C$ for samples with excess niobium. From this study, the sub-solidus phase diagram below $850^{\circ}C$ for $BaO-Na_2O-Nb_2O_5$ ternary system is proposed.

• 한국결정성장학회지
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• 제7권3호
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• pp.384-392
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• 1997

레이저의 파장을 변환시키는 비선형광학 재료인 potassium lithium niobate(KLN) 단결정은 상온에서 정방형 tungsten-bronze 구조를 갖는 강유전체이다. 결정성장이 매우 어렵고 성장된 결정을 냉각하는 과정에 생기는 균열에 의해 고품질의 단결정을 얻기가 쉽지 않았다. 결정성장 도중에 생기는 용액의 증발에 의한 조성의 변화를 알아보고자 열중량 분석을 행하였는데 결정성장 온도보다 약 1$0^{\circ}C$ 정도 높은 $1000^{\circ}C$에서 휘발은 $1.46{\times}10^{-5}$g/ ($\textrm{cm}^2$hr)로 미량이었다. 백금판을 핵생성의 자리로 사용하고 온도에 요동을 주며 서냉을 하여 결정을 성장시키는 방법을 사용하여 좋은 품질의 비교적 대형인 1 cm 정도의 KLN 단결정을 성장시킬 수 있었다. 상전이 온도는 $490^{\circ}C$로 앞서 보고된 것보다 고온이었다. OH- 밴드에 의한 광학적 이방성이 IR 영역에서 존재하였다.