• Journal of the Korean Chemical Society
• /
• v.62 no.2
• /
• pp.118-123
• /
• 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.

• Korean Journal of Materials Research
• /
• v.22 no.12
• /
• pp.711-716
• /
• 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
• /
• v.34 no.3
• /
• pp.731-734
• /
• 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 $Cs_{0.33}WO_3$.

• Journal of the Korean Ceramic Society
• /
• v.38 no.12
• /
• pp.1167-1173
• /
• 2001

The tetragonal tungsten bronze type of Sr$_{x}Ba_{1-x}Nb_{2}O_{6}$(SBN) (0.3$\le$x$\ge$0.7) ceramics was synthesized by the solid state reaction method, and the dielectric properties of SBN ceramics as a function of Sr/Ba ratio were examined. With increasing Sr/Ba ratio in SBN ceramics, the Curie temperature decreased and the maximum dielectric constant at the Curie temperature increased. The relaxor behavior of the SBN ceramics as a function of Sr/Ba ratio was quantitatively evaluated. More relaxor behavior of dielectric characteristics was observed as the ratio of Sr/Ba increased. The experimental results are explained with a viewpoint of crystallography of tungsten bronze structured SBN ceramics.

• The Korean Journal of Ceramics
• /
• v.6 no.4
• /
• pp.380-384
• /
• 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.

• Journal of Powder Materials
• /
• v.26 no.1
• /
• pp.28-33
• /
• 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
• /
• v.6 no.3
• /
• pp.272-275
• /
• 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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2003.07b
• /
• pp.739-743
• /
• 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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2003.08a
• /
• pp.98-102
• /
• 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.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.7 no.3
• /
• pp.384-392
• /
• 1997

Potassium lithium niobate(KLN) single crystal for a nonlinear-optic material, which changes the wavelength of lasers, has a ferroelectric tetragonal tungsten bronze structure at room temperature. It has been very hard to get single crystals of good quality due to the cracks during cooling process. In order to investigate the composition change due to the evaporation of solution during the growth, the thermogravimetric analysis was carried out. In atmospheric condition at $1000^{\circ}C$ which is about $10^{\circ}C$ higher than the crystal growing temperature, the weight change was negligible amount of $1.46{\times}10^{-5}$g/($\textrm{cm}^2$hr). By using both the Pt plate as the nucleation site and the slow cooling method with temperature fluctuation, KLN single crystal of good quality of size 1 cm could be obtained. The phase transition temperature was $490^{\circ}C$, which was higher than that reported by other researchers of the other composition. The optical anisotropy due to the absorption of OH-band exists in the range of IR.