• Journal of dental hygiene science
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• v.15 no.5
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• pp.577-584
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• 2015

The purpose of this study was to evaluate the effect of metal chloride infiltration treatment on color and strength changes of the yttria-stabilized tetragonal zirconia polycrystals (Y-TZP). Fifty disc specimens were prepared with a Y-TZP powder (ZPEX; Tosoh, Japan). Thirty different metal chloride solutions containing 0.03~0.08 wt% chromium and 0.03~0.07 wt% terbium ions were prepared. Presintered Y-TZP specimens were soaked in metal chloride coloring liquids for 3 minutes and sintered in air at $1,450^{\circ}C$ for 2 hours. The color of the specimens was measured with spectrophotometer and color difference (${\Delta}E^*$) was obtained based on the CIE $L^*$, $a^*$, $b^*$ color coordinate values. To evaluate the effect of metal chloride infiltration strength changes, the biaxial flexural test was performed at crosshead speed 0.5 mm/min. Colors of the sintered Y-TZP showed the colors of Vita shade guide A1, A2 and A3 with the infiltration of chromium and terbium chloride solutions. Density of the sintered Y-TZP increased by the infiltration of chromium and terbium chloride solutions. Bi-axial flexural strength of the sintered Y-TZP did not show statistically significant differences by the infiltration of chromium and terbium chloride solutions (p>0.05). Chromium and terbium chloride did not affect the crystal phase of zirconia, and all specimens showed tetragonal phase. Accordingly, this study suggests that chromium and terbium chlorides can make colored zirconia while adding in a liquid form. The color of colored zirconia differ from that of vita shade guide but it can use all ceramic restoration as substructure in dental clinic.

• Journal of Dental Rehabilitation and Applied Science
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• v.37 no.3
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• pp.111-122
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• 2021

Purpose: The purpose of this in vitro study was to investigate the flexural strength and translucency of three layers in 5Y-ZP and to assess the effect of additional firings on these properties. Materials and Methods: Sintered zirconia blocks were sectioned according to three layers : incisal, transition, and body. Disc-shaped specimens were fabricated from each layer. The diameter of specimens was 15.0 mm and each thickness of specimens for biaxial flexural strength test and translucency was 1.2 mm and 1.0 mm. The specimens were classified into subgroups according to the number of firing (0, 1, and 3 times; n = 10/subgroup) and the additional firings were performed under 900℃ using a furnace. Biaxial flexural strength and translucency was measured using universal testing machine and uv-vis spectrophotometer. X-ray diffraction (XRD) analysis was used for measurement of the phase identification. One-way ANOVA, Tukey HSD test were performed (α = 0.05). Results: There was no significant difference in flexural strength between the three layers (P > 0.05), while there was significant difference in translucency between different layers (P < 0.05). The flexural strength of incisal and transition layer was decreased by the single additional firing, and the three additional firings significantly decreased the flexural strength of three layers. The translucency of layer was decreased by additional firings except the body layer. The XRD patterns of all groups were similar. Conclusion: Three layers of 5Y-ZP were different only in translucency. Additional firings affected the flexural strength and translucency differently depending on the layers but crystalline phases were not changed.

• Journal of the Korean Ceramic Society
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• v.42 no.2 s.273
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• pp.140-144
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• 2005

The microstructures and mechanical properties of Tetragonal Zirconia Polycrystals (TZP) sintered bodies, which made by pressureless and spark plasma sintering techniques, were investigated using XRD, SEM, and TEM techniques. In the spark plasma sintered samples, the TZP grains were equiaxed type including many sub-grain boundaries regardless of sintering conditions. The biaxial strength of TZP having an average of 80 nm grains in diameter was high in value with 1025 MPa, but fracture toughness showed a low value due to the absence of a fracture toughening mechanism such as transformation toughening. In the Pressureless Sintered (PLSed) samples, the grain size of TZP was strongly dependent on the sintering temperature; i.e., it gradually increased as the sintering temperature increased. The value of fracture toughness increased as the grain size increased by the stress-induced phase transformation and Borne crack deflection.

• Journal of the Korean Ceramic Society
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• v.43 no.2 s.285
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• pp.98-105
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• 2006

YBCO film was synthesized by using a new approach to the TFA-MOD method. In the fabrication process, $Y_2Ba_1Cu_1O_x\;and\;Ba_3Cu_5O_8$ powders were used as precursors (the so called '211 process'), instead of Y-, Ba-, and Cu-based acetates, and dissolved in trifluoroacetic acid followed by calcining and firing heat treatment. Consequently, we successfully fabricated YBCO film and evaluated the phase formation, texture evolution, and critical properties as a function of the calcining and firing temperature and humidity, in order to explore its possible application in coated conductor fabrication. The films were calcined at $430-460^{\circ}C$ and then fired at $750-800^{\circ}C\;in\;a\;0-20\%$ humidified $Ar-O_2$ atmosphere. We observed that $BaF_2$ phase was effectively reduced and that a sharp and strong biaxial texture formed under humidified atmosphere leading to increased critical properties. In addition, we found that the microstructure varied significantly with the firing temperature: the grain grew further, the film became denser, and the degree of texture and phase purity varied as the firing temperature increased. For the film fired at $775^{\circ}C$ after calcining at $460^{\circ}C$, the critical current was obtained to be 39 A/cm-width (corresponding critical current density is $2.0\;MA/cm^2$ which was probably attributed to such factors as the enhanced phase purity and out-of-plane texture, the moderate film density and grain size, and crack-free surface.

• Journal of the Korean Ceramic Society
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• v.40 no.8
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• pp.751-757
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• 2003

Rapid densification of a SiC-30 wt% TiC powder with additive 10 wt% A1$_2$O$_3$-Y$_2$O$_3$-CaO was conducted by Spark Plasma Sintering(SPS). The fully-densified materials can be obtain through the SPS process with very fast heating rate and short holding time. In the present work, the heating rate and applied pressure were kept to be $100^{\circ}C$/min and 40 MPa, while sintering temperature varied from $1600^{\circ}C$ to $1800^{\circ}C$ for 10 min. The full densification of SiC-30 wt% TiC composites with the addition of $Al_2$O$_3$, $Y_2$O$_3$ and CaO was achieved at the temperature above $1700^{\circ}C$ by spark plasma sintering. The XRD found that 3C-SiC and TiC were maintained the entire SPS process temperature, without phase transformation of SiC and formation of YAG phase to $1800^{\circ}C$. The microstructures of the rapidly densified SiC-30 wt% TiC composites consisted of smaller equiaxed SiC grains and larger TiC grains. The biaxial strength of 635.2 MPa and fracture toughness of 6.12 MPaㆍ$m^{1/2}$ were found for the specimen prepared at $1750^{\circ}C$.

• Progress in Superconductivity
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• v.8 no.1
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• pp.65-70
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• 2006

We fabricated $YBa_2Cu_33O_{7-x}$(YBCO) films on(00l) $LaAlO_3$ substrates prepared by metal organic deposition(MOD) method using trifluoroacetate(TFA) solution and evaluated the effects of the humidity on the microstructure, phase purity, and critical properties. The films calcined at $430^{\circ}C$ were fired at $775^{\circ}C$ at 0%, 4.2%, 12.1%, and 20.0% humidified As gas mixed with 0.1% $O_2$. We observed that the amount of $BaF_2$ phase was effectively reduced and that a sharp and strong biaxial texture formed under a humidified atmosphere, leading to increased critical properties. For the films fired at 0% humidity, the $T_c\;and\;I_c$ were undetectably small. When the humidity was increased to 4.2%, the corresponding $T_c$(onset) and $I_c$ were increased to 90.5 K and 8 A/cm-width, respectively. For the films at the humidity range of 12.1-20.0%, the $I_c$ was found to be 35 A/cm-width. According to the results of the XRD, pole-figure, and SEM, these improved critical properties are probably attributed to the formation of a purer YBCO phase, larger grain size, and stronger c-axis orientation.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.16 no.4
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• pp.133-140
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• 2006

The growth characteristics and properties of large size $SrAlF_5$ single crystals are described and compared with those of $BaMgF_4$. Transmission spectra in the vacuum ultraviolet wavelength region indicate a high transparency of $SrAlF_5$ (about 90% without considering surface reflection loses) down to 150 nm, on contrast to the optical loses observed for $BaMgF_4$. The ferroelectric character of $SrAlF_5$ is evidenced by the reversal of the spontaneous polarization in a hysteresis loop. The higher potential of $SrAlF_5$ in comparison with $BaMgF_4$ for the realization of all-solid-state lasers in the ultraviolet wavelength region by the quasi-phase matching (QPM) technique is pointed out. $SrAlF_5$, besides a higher grade of transparency, shows a nonlinear effective coefficient similar to that of quartz and uniaxial nature, on contrast to the one order smaller nonlinear coefficient and biaxial character of $BaMgF_4$. The refractive index of $SrAlF_5$ from the ultraviolet to the near-infrared wavelength region is measured by the minimum deviation method. The Sellmeier and Cauchy coefficients are obtained from the fits to the curves of the ordinary and extraordinary refractive indices, and the grating period for the first order QPM is estimated as a function of the wavelength. The poling periodicity for 193 nm SHG from 386 nm is $4{\mu}m$.

• Progress in Superconductivity
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• v.7 no.2
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• pp.140-144
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• 2006

We fabricated the YBCO films on single crystal $LaAlO_3$ substrates via a metal organic deposition (MOD) process. In the process, $Y_2Ba_1Cu_1O_x$ and $Ba_3Cu_5O_8$ powders were dissolved in trifluoroacetic acid (TFA) followed by calcining and firing heat treatments. To evaluate the effects of the firing temperature on YBCO phase formation and critical properties, the films were fired at $750^{\circ}C,\;775^{\circ}C\;and\;800^{\circ}C$ after calcining at $430^{\cric}C$. Microstructure observation indicated that a crack-free surface formed and a strong biaxial texture was developed. The FWHM of out-of-plane texture was measured to be in the range of $4.3^{\cric}-7.0^{\circ}$ for all the films. When the YBCO film was fired at $775^{\cric}C$, it had the highest critical properties: 88.5 K of critical temperature and 16 A/cm-width of critical current ($1MA/cm^2$ as critical current density). On the other hand, those properties were degraded as firing at $750^{\circ}C\;and\;800^{\circ}C$. It is considered that the improved critical values are partly owing to dense and homogeneous microstructure, strong texture, and high oxygen content.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.19 no.5
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• pp.467-476
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• 2006

We fabricated the YBCO films on LAO substrate using the TFA-MOD method and evaluated the effects of heat treatment temperature and film thickness on the microstructure, degree of texture, and critical properties. The calcining and firing were peformed at the temperature range of $370^{\circ}C-460^{\circ}C\;and\;750^{\circ}C-800^{\circ}C$, respectively. For the films fired at $775^{\circ}C$ after calcining at $400^{\circ}C-430^{\circ}C$showed highest critical temperature (Tc-onset) of 89.5 K and critical current (Ic) of 40A/cm-width which corresponds to critical current density (Jc) of $1.8MA/cm^2$. The highest critical properties are probably attributed to the formation of purer YBCO phase, stronger biaxial texture, and higher oxygen content, according to the XRD, pole-figure, SEM, Raman analysis. From the multi-coated films, the Ic increased from 39 to 169 A/cm-width as the coating repeated to four times, while the corresponding Jc was measured from once to be in the range of $0.8-1.2MA/cm^2$. Both Ic and Jc degraded as the coating repeated further, indicating that the optimum thickness is in the range of $1.0{\mu}m-1.7{\mu}m$.

• Journal of the korean academy of Pediatric Dentistry
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• v.34 no.1
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• pp.1-12
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• 2007

The purpose of this study was to evaluate the effect that various concentration and application time of hydrogen peroxide had on tooth whitening and physical properties. The hydroxyapatite (HA) discs of $12mm({\Phi}){\times}1.2mm(t)$ in dimensions were made by compression $(100kg/cm^2)$ and sintering (at $1350^{\circ}C$ for 2 hours) All specimens were polished sequentially with '240 through '2000 emery paper and one side of each specimen was polished finally with $0.3{\mu}m$ alumina paste. The discs were placed in sterile whole stimulated saliva overnight at $37^{\circ}C$ in order to form an in vitro pellicle layer. Then the discs were rinsed with distilled water and soaked into staining broth at $37^{\circ}C$ for 7 days. These stained specimens were bleached with hydrogen peroxide according to the change of concentration $(3{\sim}30%)$ and application time ($3{\sim}10$ days). The specimens were analyzed with a spectrophotometer, X-ray diffractometer (XRD), scanning electron microscope (SEM), surface roughness tester, microhardness tester and biaxial flexural strength. The results of present study can be summarized as follows : 1. The bleaching effect was increased with the increased concentration and the extended application time of hydrogen peroxide. 2. The surface roughness was significantly increased from the specimen bleached with 15% hydrogen peroxide for 10 days and with 30% for 7 and 10 days respectively (p<0.05). 3. The changes of crystal phase observed by XRD between before and after bleaching weren't shown of any difference, but microporous structure of surface observed by SEM was shown of increase with the increased concentration and the extended application. 4. The biaxial flexural strength was significantly decreased from bleaching of specimen with 30% hydrogen peroxide for 7 and 10 days respectively (p<0.05) 5. Microhardness was significantly decreased from bleaching with 15% hydrogen peroxide for 10 days and with 30% for 3, 7 and 10 days respectively (p<0.05). Although the tooth bleaching effect was greater when the high concentration was applied, further in vivo experiment will be needed to prove it's safety.