• 한국세라믹학회지
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• 제48권4호
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• pp.303-306
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• 2011

[ $V_2O_5$ ]doped Karrooite pigments were synthesized by the solid state method to get stabilized brown pigment in oxidation and reduction atmosphere. Optimum substitution condition and limited dopant with $V_2O_5$ for Karrooite pigment was investigated. With calcination at $1250^{\circ}C{\sim}1400^{\circ}C$, compositions were designed varying $V_2O_5$ molar ratio by increasing 0.02mole to the formula $Mg_1-xTi_2-xM_{2x}O_5$(x = 0.01~0.09 mole). Synthesized pigments were analyzed by XRD, Raman spectroscopy and UV-vis. When $V_2O_5$ was doped from 0.01 to 0.05 mole, single phase of Karrooite was observed at temperature $1300^{\circ}C$ and soaking time 4h by Raman spectroscopy. However, it was found that excess $VO_2$ peak appeared with 0.07 and 0.09 mole of $V_2O_5$ doped to $MgTi_2O_5$. This result indicated that the maximum limit of solid solution is 0.05 mole $V_2O_5$. Karrooite pigments were applied as a ceramic pigment to achieve brown colors in lime magnesia glaze and lime barium graze at both of oxidation and reduction atmosphere. CIE color coordinates are $L^*$ = 40.34, $a^*$ = 9.94, $b^*$ = 21.40 in lime magnesia glaze.

• 대한화학회지
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• 제4권1호
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• pp.27-37
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• 1957

High-fire stain is influenced by the conditions of glaze, firing atmosphere, etc. On the contrary, low fire stain is not influenced by those conditions but obtainable in arbitrary colors and it is indispensable for pottery decoration. It is difficult for us to study into the color in the sphere of result publication method and expression of color. Looking over the literature on this subject, I have been confronted with much difficulties, accordingly, I made a basic and systematic experiment as to six low-firing stains (blue, green, blue-green, brown black and yellow) and made it proper to be applied in these studies. On pigment, I confirmed the influence of the assistant coloring matter by mixing up the coloring matter and the assistant coloring matter in various proportions. On flux, I measured the melting point by making PbO-$SiO_2$ system and PbO-$B_2O_3-SiO_2$ system and decided the range of usage. Also I checked the coloring by making the pigment on laze with pigment and flux manufactured, and concluded the pigment and flux adaptation to it.

• 한국세라믹학회지
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• 제55권4호
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• pp.368-375
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• 2018

This study deals with the color formation of ceramic pigment in the $TiO_2$-SnO-ZnO system. We designed compounds to control the color formation depending on the composition using the Design of Experiment. The color coordinate values of synthesized pigments, $L^*a^*b^*$ were measured and statistically analyzed color for changing elements depending on its composition. The relationship between the major crystalline phases and chromaticity was examined using XRD, and the oxidation states of each element were analyzed by XPS. The synthesized pigments based on the compound design exhibited various color changes ranging from yellow-orange to green-blue and brown. The statistical analysis on the spectrophotometer results shows that $a^*$ and $b^*$ values decreased with $TiO_2$ content, and increased with SnO content. Yellow-orange color was detected with the main peak of SnO, and the green-blue color developed with the main peak of $Zn_2TiO_4$. The $a^*$ and $b^*$ values increased with increased SnO peak intensity, and decreased with increased $Zn_2TiO_4$ peak intensity. The results revealed that pigment color formation was influenced by changes in the main crystalline phases and crystalline intensity. However, XPS analysis of the oxidation states of each element showed little correlation with the pigment chromaticity result.

• 한국세라믹학회지
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• 제44권10호
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• pp.554-561
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• 2007

Synthesis and characterization of pigments by using $Fe_2O_3,\;CoO,\;Cr_2O_3\;and\;MnO_2$ were undertaken. The resulting pigments were characterized by using XRD, SEM, FT-IR and UV-Vis spectrophotometer. The color of glazed tiles containing 6 wt% pigment changed from dark green to black depending on the compositions of used materials. Pigments were calcined with mixed materials at $1350^{\circ}C$, and the dark green and dark brown color were obtained. Pigments were used to determine possible interactions between a pigment and a glaze.

• 한국세라믹학회지
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• 제12권1호
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• pp.29-36
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• 1975

This study was conducted to research the formation, color development and application for colored glazes of the spinel solid solutions of the green pigment. On specimens prepared by calcining the oxide and basic carbonate mixture at 1250℃ for 1.5 hour, the x-ray analysis, measurement of reflectance and the test of their stabiality as a glaze pigment were carried out. The results are summarized as follows 1) Each sample is composed of single spinel and not of mixture of spinel. 2) Formation of continuous soild solution, except for a few instances, pertaining to Vegard's law was confirmed by means of the x-ray analysis. 3) The more difference between absorption and reflectance lies, the lighter colors are. When the absorption occurs at the high-reflectance, the excitation purity becomes low. On the contrary when the absorption takes place at the low-reflectance, the excitation purity becomes low. On the contrary when the absorption takes place at the low-reflectance, the excitation purity is higher. 4) Colors obtained in the CdO-MgO-Cr2O3-Al2O3 system, as the amounts of Al3+ increased, change from green through brown to pink, and the absorption peak shifts towards violet region. 5) An increase in Co2+ in the CoO-MgO-Cr2O3-Al2O3 system, changes the color from blue green to dark blue. The excitation purity is higher, and the absorption peak shifts toward regions. 6) Colors are green in the NiO-MgO-Cr2O3 and CdO-MgO-Cr2O3 systems in general, but in the ZnO-MgO-Cr2O3 system brillant hue is not obtained. 70 According to the results of the colored glaze test, the spinels turn outto be stable as brilliant glaze pigment in the calcium-magnesia glaze.

• 한국재료학회지
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• 제21권9호
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• pp.515-519
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• 2011

The purpose of this study was to determine the optimal firing condition and composition for $Al_2TiO_5$ crystal, which is suitable for stable coloration in glazes at high temperatures, using $Cr_2O_3$ as chromophore for the synthesis of $Al_2TiO_5$ system pigments. $Al_2TiO_5$ has a high refractive index and good solubility of chromophore in the $Al_2TiO_5$ lattice, making this structure a good candidate for the development of new ceramic pigments. Pigments were synthesized by using $Al_2O_3$ and $TiO_2$ mainly. Various amounts of $Cr_2O_3$ such as 0.01, 0.02, 0.03, 0.04 and 0.05 mole were also added. Each compound was synthesized at $1300^{\circ}C$, $1400^{\circ}C$, and $1500^{\circ}C$ for 2 hours and cooled naturally. The crystal structure, solubility limit, and color of the synthesized pigments were analyzed by XRD, SEM, Raman spectroscopy, UV and UV-vis. The changes in color as the result of applying 6 wt% of the synthesized pigments to lime barium glaze were expressed as CIE-L*a*b* values. A $Cr_2O_3$ 0.03 mole doped $Al_2TiO_5$ brown pigment was successfully synthesize at $1400^{\circ}C$, and the values of CIE-L*a*b* parameters were L* = 44.62, a* = 3.10, and b* = 17.25. In the case of the pigment synthesized at $1500^{\circ}C$, the brown color was obtained at 0.01 mole and 0.02 mole $Cr_2O_3$, and the CIE-L*a*b* values were 55.34, 1.73, 28.64, and 49.39, 0.51, 21.33, respectively. At $1500^{\circ}C$, the maximum limit of solid solution was 0.03 mole $Cr_2O_3$. The glazed sample showed green color, and the values of the CIEL* a*b* parameters were L* = 45.69, a* = -0.98, and b* = 20.38.

• 한국세라믹학회지
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• 제46권4호
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• pp.350-356
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• 2009

Perovskite codoped with chromium and iron have been studied. Samples with $YAl_{0.96}(Cr_{0.04-x}Fe_x)O_3$(x=0.01, 0.02, 0.03, 0.04) were prepared by solid state reaction at $1450^{\circ}C$ for 6 h and were characterized by XRD, FT-IR, Raman spectroscopy, SEM and UV-vis spectrophotometer. The color of the synthesized pigments were from red to dark brown(in bulk). Up to 0.02 mole $Fe_2O_3$ for substituting $Cr_2O_3$ development of color in lime-glaze gives good red color but as increasing amount of $Fe_2O_3$ and decreasing $Cr_2O_3$ proportionally produce from brownish red to brown. Increasing $Fe_2O_3$ amount lead to weaken crystal field relatively due to have smaller ionic radius than $Cr_2O_3$ ionic one. The UV-vis peaks were shifted to lower wavelength.

• 한국세라믹학회지
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• 제13권2호
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• pp.24-30
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• 1976

To observe the influence of tetrahedral and octahedral preference of cations of Ni2+, Ti4+ upon the formation and the color development of the MgO-SnO2 spinel containing Ni2+ and Ti4+ ions, the gradual substitution of Ni2+ ions for Mg2+ ions and of Ti4+ ions for Sn4+ ions of the spinel in NiO-MgO-SnO2-TiO2 system was carried out. On samples prepared by calcining the oxide and basic carbonate mixtures at 130$0^{\circ}C$ for 1.5 hour, the X-ray analysis, measurement of reflectance and the test of their stability as a glaze pigment were also carried out. On samples prepared by calcining the oxide and basic carbonate mixtures at 130$0^{\circ}C$ for 1.5 hour, the X-ray analysis, measurement of reflectance and the test of their stabiality as a glaze pigment were also carried out. The results are summarized as follows. 1) As increasing the amounts of Ni2+ ions in the xNiO.(2-x)MgO.SnO2 system, spinel was not formed easily, and the mixed-spinel was formed in NiO.MgO.SnO2 of x=1 but the spinels was not formed completely in the range of x>1.5 2) The spinels was not more formed in NiO-MgO-TiO2 system than NiO-MgO-SnO2 system. Therefore, Ti4+ ions have strong octahedral preference than Sn4+ ions. The color changed the yellow region little. The mixed-spinel or non-spinel was formed easily NiO.TiO2, MgO.TiO2 of illmenite type as the gradual substitution of Ti4+ ions for Sn4+ ions. 3) The results of glaze test. The color changed from white through graish brown to brown as the gradual substitution of Ni2+ ions for Mg2+ ions in calcium-zinc glaze and calcium glaze, and from white through light yellowish beige to dull beige in tile glaze. Also, the color did not change generally as the gradual substitution of Ti4+ ions for Sn4+ ions in NiO-MgO-SnO2-TiO2 system.

• 한국재료학회지
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• 제23권4호
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• pp.233-239
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• 2013

We collected Seokganju minerals (regions in Gyeryong Mountain, Sangsin-ri, Banpo-myeon, Gongju Chungcheongnam-province), which were used as natural color pigments for grayish-blue during the 15th~16th centuries of the Joseon era, and investigated their crystallographic features to develop a black pigment having a spinel structure. By a Raman analysis, the color of Seokganju under transparent glaze as a pigment for painting was black because hematite ($Fe_2O_3$) in Seokganju was converted to magnetite ($Fe_3O_4$) However, Seokganju into the transparent glaze as a pigment was brown because of hematite ($Fe_2O_3$) and small amounts of maghemite (${\gamma}-Fe_2O_3$) in Seokganju minerals. Only Seokganju mineral is used, it is not suitable for black pigment into the transparent glaze. This study tried to develop a spinel crystal black pigment stabilized by Seokganju with CoO, $Cr_2O_3$, NiO, and $MnO_2$ at $1280^{\circ}C$. A Raman spectroscopy analysis was performed to verify the presence of Mn The results showed that it existed as spinel, and two crystal phases $CoFe_2O_4$ and $MnFe_2O_4$ were mixed. $CoFe_2O_4$ spinel has a dark grayish black color and $MnFe_2O_4$ spinel has a greenish black color, and these two appeared as black. The color of a specimen calcined by adding 6 wt% of pigment mixed with 5 wt% of $MnO_2$ added to lime glaze was analyzed with a UV spectrophotometer. When applying the color pigment, it appeared black stabilized with $L^*$24.23, $a^*$ 0.12, $b^*$ -2.29 at $1260^{\circ}C$ oxidative calcination, With $1240^{\circ}C$ reduction firing, it is appeared black stabilized with low brightness of $L^*$ 23.13, $a^*$ -1.12, $b^*$ 0.54.

• 한국분말재료학회지
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• 제20권3호
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• pp.210-214
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• 2013

This manuscript reports on compared color evolution about phase transformation of ${\alpha}-FeOOH@SiO_2$ and ${\beta}-FeOOH@SiO_2$ pigments. Prepared ${\alpha}$-FeOOH and ${\beta}$-FeOOH were coated with silica for enhancing thermal properties and coloration of both samples. To study phase and color of ${\alpha}$-FeOOH and ${\beta}$-FeOOH, we prepared nano sized iron oxide hydroxide pigments which were coated with $SiO_2$ using tetraethylorthosilicate and cetyltrimethyl-ammonium bromide as a surface modifier. The silica-coated both samples were calcined at high temperatures (300, 700 and $1000^{\circ}C$) and characterized by scanning electron microscopy, CIE $L^*a^*b^*$ color parameter measurements, transmission electron microscopy and UV-vis spectroscopy. The yellow ${\alpha}$-FeOOH and ${\beta}$-FeOOH was transformed to ${\alpha}-Fe_2O_3$ with red, brown at 300, $700^{\circ}C$, respectively.