• Journal of the Korean Ceramic Society
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• v.27 no.8
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• pp.1050-1054
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• 1990

Rutile(TiO2) single crystals were grown by FZ method. Feed rod was sintered in the longitudinal tube-shaped furnace at 135$0^{\circ}C$ and optimum growth condition was growth rate 5-8mm/hr, rotation rate 30-40rpm. When crystal was growing, atomosphere was oxidized condition, and grown single crystal was annealed at 110$0^{\circ}C$. The rutile single crystals were oriented to [001] direction and color change of single crystals were related to atmosphere, and difference of electric conductivity and resistance was due to the fact above.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.16 no.4
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• pp.141-148
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• 2006

Skull melting method can be a good candidate for growing oxide single crystals with high quality and for mass production because of its low production costs and high yield through recycling of crust. In this study, rutile single crystals were frown by the skull melting method and ingot characteristics with the variation of different growth conditions has been investigated. Conditions for high quality rutile ingot growth were used for producing cold-crucible size of ${\Phi}12cm{\times}H14cm$, capacity of 3000 pF tank condenser, work frequency of 2.84 MHz, melt-dwelling time of 9hrs and growing speed of 2 mm/h.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.14 no.6
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• pp.262-266
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• 2004

Rutile single crystals were grown by the skull melting method. Ti metal ring was used for initial RF induction heating. The grown crystals were cut into wafer of 5.5 mm diameter and 1mm thickness. The wafers were annealed in air at $1300^{\circ}C$ up to 15 hours and their transmittance spectra $(\lambda= 200~25000 nm)$ were obtained.

• Journal of the Korean Ceramic Society
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• v.26 no.1
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• pp.1-6
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• 1989

The phenomena that the electrical conductivity of rutile single crystal changes with time were investigated along the a and c crystallographic axes, at 85$0^{\circ}C$ and Po2 in the range of 1~10-18.5atm. The D.C. conductivity decreased with and saturated some value after ca. 100 hours. But the A.C. conductivity showed no time dependence in the whole Po2 range. These experimental results suggest that the time dependence of D.C. conductivity of rutile single crystal is due to space charge polarization effect; the electrode was Pt which is complete electronic conductor, while the sample was TiO2 which is mixed conductor.

• Journal of the Korean Ceramic Society
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• v.28 no.12
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• pp.989-995
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• 1991

By means of the secondary ion mass spectrometer, the tracer diffusion of oxygen in rutile single crystal was measured as function of temperature and oxygen partial pressure. The tracer diffusivity was determined from the depth profile of 18O. The Po2 dependence of D suggests that the dominant defects in TiO2-y are oxygen vacancies (V{{{{ { ‥} atop { o} }}) and interstitial titanium ions (Ti{{{{ {‥‥} atop {i} }}). The doubly ionized oxygen vacancies are prominent at low temperature and Po2. However, the tetravalent interstitial titanium ions predominate at teperature above 120$0^{\circ}C$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.5 no.3
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• pp.240-249
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• 1995

Rutile type of $TiO_{2}$ single crystal was grown by floating zone method in order to obtain the highly transparent and contamination-free single crystal. The linear refractive index of perpendicular and parallel to c-axis was measured as a function o f wavelength from 500 to 1000nm. The optical energy band gap was estimated as 2.99 eV from the absorption spectrum. The theoretical $\chi^{(3)}$} value of $TiO_{2}$ was discussed in comparison with that of $SiO_{2}$ quartz single crystal on the basis of semiempirical model. On the other hand, the second-hyperpolarizability, ${\gamma}({Ti}^{4+})$ was calculated in order to describe the effect of $Ti_{4}$ ion on the third order nonlinear optical properties.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.2 no.1
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• pp.60-69
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• 1992

Fine $TiO_2$ powders were synthesized from ammonium titanium sulphate which produced from $TiCI_4$, and$(NH_4)_2$ SO. solution. Rutile single crystal were grown by the verneuil method with anatase powders and investigated the property of rutile crystal. The optimun growing conditions were as follows $\cdot$The ratio of hydrogen gas and oxygen gas; 3: 1 $\cdot$Growing temperature: $1900^{\circ}C$ $\cdot$The feeding rate of powders: 10g/hr

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.16 no.5
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• pp.181-188
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• 2006

Rutile single crystals grown by skull melting method were cut parallel and perpendicular to growth axis, and both sides of the cut wafers (${\phi}5.5mmx1.0mm$) were then polished to be mirror surfaces. The black wafers were changed into pale yellow color by annealing in air at 1200 and $1300^{\circ}C$ for $3{\sim}15\;and\;10{\sim}50$ hours, respectively. After annealing, structural and optical properties were examined by specific gravity (S.G), SEM-electron backscattered pattern (SEM-EBSP), X-ray diffraction (XRD), FT-IR transmittance spectra, laser Raman spectroscopy (LRS), photoluminescence (PL) and X-ray photoelectron spectroscopy (XPS). These results are analyzed increase of weight in air, decrease of weight in water and specific gravity, shown secondary phase of needle shape, diffusion of oxygen ion and increase of $Ti^{3+}$. From the above results, we suggest that the skull melting method grown rutile single crystals contain defect centers such as $O_v,\;Ti^{3+},\;O_v-Ti^{3+}$ interstitials and $F^+-H^+$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.5 no.3
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• pp.250-260
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• 1995

In general, a sintered rod is used as a feed in the growth of crystals by the floating zone(FZ) method. The sintering condition of the feed rod affected the stability of molten zone because it influenced the interface shape between the feed and the melt during the crystal growth. In this study, rutile and ruby crystals were chosen as samples to analyze the effect of the microstructures of the feed rods. In sintering of the feed rod for the growth of rutile and ruby single crystals, the difference of grain size between the inner and the outer region of the feed rod increased with the sintering temperature and dwelling time. As a result, it altered melting behavior of the feed. The uniform grain size of the sintered rod was necessary for the optimum growing condition of crystals. The effect of pores in the feed rod was not a dominant factor to grow crystals by the FZ method, which was confirmed by growing crystals with nonsinterd rods as feeds.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.3
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• pp.85-88
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• 2001

High oxygen pressure has been applied for a floating zone (FZ) crystal grower in order to grow high quality $TiO_2$(rutile) single crystals suitable for optical application. The $TiO_2$ crystals, grown under 0.3, 0.4, 0.5, and 0.8MPa oxygen pressure respectively, are all transparent and dark blue. The degree of the presence of sub-grain boundary in the crystal differs from the applied oxygen pressure. In particular, $TiO_2$ single crystals grown under0.5 MPa showed sub-grain boundary-free and estimated good for optical devices.