• Journal of the Korean Ceramic Society
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• v.46 no.6
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• pp.615-620
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• 2009

The present research was performed to determine the optimal firing condition and holding time for malayaite crystal, which is responsible for the stable pink-red coloration in glaze at high temperatures, using Cr$Cl_3$ as chromophore for the synthesis of $Cr_2O_3-SnO_2-CaO-SiO_2$ system pigments. The malayaite crystal was influenced by the raw materials used for synthesis, firing temperature, and holding time. Thus there are differences in the crystal phase and in the coloration according to the condition of synthesis. When Cr$Cl_3$ was used as chromophore, the pigment could be synthesized at lower temperatures, because Cr$Cl_3$ melts at $1500{^{\circ}C}$, which is much lower than the temperature at which $Cr_2O_3$ melts (higher than $2435{^{\circ}C}$). And the employed Cr ion showed a change in oxidation state. When a mineralizer was used to improve the employment of malayaite and the Cr ion, and the low temperature was maintained at which the malayaite crystal is produced, the production of malayaite crystal was promoted and the employment of chromophore was also promoted in the oxidation state of Cr (IV). The results of the experiment showed that the optimal firing condition was 18 h of holding time at $800{^{\circ}C}$, using Cr$Cl_3$ as chromophore, followed by 2 h at the raised temperature of $1150{^{\circ}C}$. The change in coloration of the Cr (IV) employed by malayaite showed a very rich color of red. Thus it was possible to effectively synthesize sphene-pink pigments with more red tint at a low temperature.

• Journal of the Korean Ceramic Society
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• v.46 no.6
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• pp.639-642
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• 2009

The research was performed to find out the optimum firing condition for the $SnO_2-TiO_2-V_2O_5$ system yellow pigment. The pigment based on $SnO_2-V_2O_5$ system showed very intense yellow color and it was used widely in ceramics industry. Synthesized pigment, with partial substitutions of $SnO_2\;by\;TiO_2$, was fired at $1300{^{\circ}C}$ soaking 1h and it showed bright yellow color. $SnO_2-TiO_2-V_2O_5$ system was very more intensive changes in yellow color by colorimetric value $b^*$ than $SnO_2-V_2O_5$ system. Synthesized yellow pigments were characterized by X-ray diffraction (XRD), FT-IR, and UV-vis spectroscopy. The best composition for yellow pigment was 93:7:0.5(mole%) for $SnO_2-V_2O_5-TiO_2$. The measurement of CIE $L^*a^*b^*$ of pigment was $L^*(78.82),\;a^*(-4.88)\;and\;b^*$(59.25).

• Journal of the Korean Ceramic Society
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• v.26 no.2
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• pp.187-194
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• 1989

Synthesis of spinel pigment on ZnO-Fe2O3 system. The object of this research is the synthesis of new spinel pigments on the basic of ZnO-Fe2O3 system which was substituted by ZnO-Fe2O3 by MgO-Al2O3. This research was progressed by measuring the X-ray diffraction and the reflectances of the substitued ZnO-Fe2O3 group. Which was obtained by sintering at the temperature of 1,00$0^{\circ}C$, 1,10$0^{\circ}C$, 1,20$0^{\circ}C$ and 1,25$0^{\circ}C$ and them by regrinding. In order to coloring test, here basic compositions of Barium glaze, Zinc glaze, Lime glaze, Lead glaze and Talc glaze used in this experiment are obtained from the ceramic work. Adding synthetic stains in these basic glazes with 3%, mixing and glazing on the specimen. The specimens was fired at 1,28$0^{\circ}C$ in reducing and oxidizing atmosphere in the gas kiln. The results of the research as follow. 1. Many kinds of spinel pigment was produced on ZnO-Fe2O3 system that is to say, not always only spinel. 2. Spinel peak was observed strongly on the ZnO-Fe2O3 system withsubstituting by MgO-Fe2O3 and MgO-Al2O3 group(the ratio of MgO, Al2O3 being increased, observed more strongly). 3. The most effective temperature ranges was 1,20$0^{\circ}C$~1,25$0^{\circ}C$. 4. The color of spinel pigments on this system was observed by "stable YR". 5. It was yellow red in oxidizing and green in reducing atmosphere on the coloring test.ring test.

• Journal of the Korean Ceramic Society
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• v.50 no.3
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• pp.195-200
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• 2013

Here, we report preparation of cyan ceramic nano-pigment for inkjet printing and the Ni substitutional effects on the cyan color. $MgAl_2O_4$ was selected as the crystalline host network for the synthesis of nickel-based cyan ceramic nano-pigments. Various compositions of $Ni_xMg_{1-x}Al_2O_4$ ($0{\leq}x{\leq}1$) powders were prepared using the polymerized complex method. The powder was then preheated at $400^{\circ}C$ for 5 h and finally calcined at $1000^{\circ}C$ for 5 h. XRD patterns of $Ni_xMg_{1-x}Al_2O_4$ showed a single phase of the spinel structure in all the compositions. The particle sizes ranged from 20 to 50 nm in TEM observations. The characteristics of the color tones of $Ni_xMg_{1-x}Al_2O_4$ were analyzed by UV-Visible spectroscopy and CIE $L^*a^*b^*$ measurement. CIE $L^*a^*b^*$ measurement results indicate that the pigment color changes from light cyan to deep cyan due to the decrease of the $a^*$ and $b^*$ values with an increase of an Ni substitutional amount. In addition, the thermal stability and the binding nature of $Ni_xMg_{1-x}Al_2O_4$ are also discussed using TG-DSC and FT-IR results respectively.

• Journal of the Korean Ceramic Society
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• v.44 no.11
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• pp.639-644
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• 2007

Spinel pigments, developing black color in high temperature glazes at oxidation or reduction atmosphere, without CoO because of its high price were synthesized by solid solution method. Ten mixed compositions consisted of NiO, MnO, $Fe_2O_3 and $Mn_2O_3$ were fired at $1250^{\circ}C$ for 1h. The resulting pigments were characterized by using XRD, FT-IR, SEM and UV-vis spectrometer. Structure of the pigments are spinel and particles' shape are spherical or cubic. Glazed tiles containing 5 wt% pigments were fired at $1260^{\circ}C$ and $1240^{\circ}C$ in reduction atmosphere. Color in glazes were analyzed by UV-vis spectrometer. Colors of NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0125 mole% and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole% in lime glaze showed black in oxidation, in reduction NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0125 mole% and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.55{\cdot}Mn_2O_3$ 0.0125 mole% showed black. In case of lime-barium glaze, NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole%, NiO 0.975 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% and NiO 0.925 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% showed black color in oxidation and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole%, NiO 0.925 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% and NiO 0.725 MnO $0.275{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% showed black one in reduction.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.5
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• pp.181-187
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• 2016

In this study, new composition of orange color pigment was developed by replacing formerly used lead and chromium with environment-friendly elements. $TiO_2-SnO-ZnO$ composite was synthesized using the solid state reaction under the reducing atmosphere with the LPG and air mixture gas. The synthesized pigments were characterized by spectrophotometer, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The colorimetric analysis of pigments exhibited color values ranging from yellow to orange-red. Five different crystalline phases were formed after the heat treatment for 4 and 6 hours. The color of pigments was strongly influenced by the crystalline structure of $SnO_2$, having either cubic or tetragonal structure. The oxidation state study of elements revealed that the color of pigment is getting close to rYR with the increase of $Sn^{4+}$ ratio.

• Korean Journal of Materials Research
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• v.24 no.2
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• pp.73-80
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• 2014

Ink-jet printing technology has been widely attractive due to its facility for direct and fine printing on various substrates. Recent studies have focused on expanding the application of ink-jet printing technology from general consumer use and design companies to the prototype production of precision parts and parts manufacturing. The use of ink-jet printing technology in decorated tableware, tiles, and other ceramic products also has many advantages. The printing process is fast and can be adaptable to various kinds of objects because there is no direct contact point between the printer and the substrates to be printed. For application to ceramic product decoration, inks containing highly dispersed inorganic nano-pigments are required. Here we report the synthesis and characterization of blue $CoAl_2O_4$ nanopigment for ink-jet printing. Blue ceramic ink based on the obtained $CoAl_2O_4$ pigment was prepared by dissolving $CoAl_2O_4$ pigment in a mixed solution of ethylene glycol and ethanol with volume ratios of 7:3 and 8:2, respectively, to obtain the appropriate viscosity for ink-jet printing. The ink solution contained 15 wt% of $CoAl_2O_4$ pigment and Cetyltrimethyl ammonium bromide(CTAB) and Sodium dodecyl sulfate(SDS) as dispersive agents. The prepared blue ceramic ink was stably jetted and formed a sphere-shaped droplet from an ink-jet printer.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.274-274
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• 2010

안료의 색상은 출발원료의 조성, 입자크기 및 소결온도에 의한 결정구조 등에 의존한다. 본 연구에서는 Rutile구조를 갖는 세라믹안료인 $TiO_2-WO_3$-NiO의 합성에서 소결온도를 결정하기 위해 소결전 출발원료를 습식법에 의하여 Jar Mill에서 0.7-0.9um로 혼합분쇄한 후 $100^{\circ}C$에서 24시간 건조하였다. 건조후 $1100-1280^{\circ}C$에서 5구간을 선정하여 소결한 시료를 Jar Mill에서 0.8-1um로 분쇄한 후, 다시 $100^{\circ}C$에서 24시간 건조하였다. 이렇게 얻어진 시료를 XRD로 상합성 정도를 조사하고, 색상 및 착색력을 spectrophotometer를 분석하였다. 색상은 1150와 $1250^{\circ}C$에서 가장 좋은 Yellow 색상이 관찰되었으며, XRD에 의한 결정성의 분석결과와 비교적 일치하고 있다. Rutile구조를 갖는 세라믹안료의 색상은 소결시의 결정화도에 따라 민감하게 변화되고 있음을 알 수 있다.

• The Journal of Advanced Prosthodontics
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• v.6 no.6
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• pp.451-455
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• 2014

PURPOSE. The most common failure seen in restorations with a zirconia core is total or layered delamination of the ceramic veneer. In the present study, the shear bond strengths between veneering ceramics and colored zirconia oxide core materials were evaluated. MATERIALS AND METHODS. Zirconia discs ($15{\times}12{\times}1.6mm$) were divided into 11 groups of 12 discs each. Groups were colored according to the Vita Classic scale: A3, B1, C4, D2, and D4. Each group was treated with the recommended shading time for 3 s, or with prolonged shading for 60 s, except for the control group. Samples were veneered with 3 mm thick and 3.5 mm in diameter translucent ceramic and subjected to shear test in a universal testing machine with a crosshead speed of 1 mm/min. One-way analysis of variance (ANOVA) and Tukey's HSD tests were used for comparisons of the groups having the same shading times. A paired t-test was used for groups of the same color (3 s/60 s). RESULTS. Among the 11 groups investigated C4 (3 s) had the highest bond strength with a value of 36.40 MPa, while A3 (3 s) showed the lowest bond strength with a value of 29.47 MPa. CONCLUSION. Coloring procedures can affect zirconia/ceramic bond strength. However, the results also showed that bond strengths of all the investigated groups were clinically acceptable.

• Journal of Powder Materials
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• v.21 no.5
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• pp.377-381
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• 2014

This work describes the coloration, chemical stability of $SiO_2$ and $SnO_2$-coated blue $CoAl_2O_4$ pigment. The $CoAl_2O_4$, raw materials, were synthesized by a co-precipitation method and coated with silica ($SiO_2$) and tin oxide ($SnO_2$) using sol-gel method, respectively. To study phase and coloration of $CoAl_2O_4$, we prepared nano sized $CoAl_2O_4$ pigments which were coated $SiO_2$ and $SnO_2$ using tetraethylorthosilicate, $Na_2SiO_3$ and $Na_2SiO_3$ as a coating material. To determine the stability of the coated samples and their colloidal solutions under acidic and basic conditions, colloidal nanoparticle solutions with various pH values were prepared and monitored over time. Blue $CoAl_2O_4$ solutions were tuned yellow color under all acidic/basic conditions. On the other hand, the chemical stability of $SiO_2$ and $SnO_2$-coated $CoAl_2O_4$ solution were improved when all samples pH values, respectively. Phase stability under acidic/basic condition of the core-shell type $CoAl_2O_4$ powders were characterized by transmission electron microscope, X-ray diffraction, CIE $L^*a^*b^*$ color parameter measurements.