• Korean Journal of Materials Research
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• v.19 no.6
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• pp.300-304
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• 2009

The domain structures of annealed (001)-oriented $Pb(Mg_{1/3}Nb_{2/3})O_3-x%PbTiO_3$ (PMN-x%PT) crystals for x = 10, 20, 30, 35, and 40 at% were investigated by Polarized Optical Microscopy (POM) and Scanning Force Microscopy (SFM) in the piezoresponse mode. Both Polar Nano-Domains (PND) and long strip-like domains were clearly observed. The results also showed how the domain structure changed between phases with an increasing x in the PMN-x%PT crystals and the domain hierarchy on various length scales ranging from 40 nm to 0.1 mm. Distorted pseudo-cubic phase (x < 20%) consisted of PNDs that did not self-assemble into macro-domain plates. The rhombohedral phase (x = 30%) consisted of PNDs that began to self-assemble into colonies along preferred {110} planes. The monoclinic phase (x = 35%) consisted of miniature polar domains on the nm scale, whereas, the tetragonal phase (x = 40%) consisted of {001} oriented lamella domains on the mm scale that had internal nano-scale heterogeneities, which self-assembled into macro-domain plates oriented along {001} the mm scale.

• Journal of Powder Materials
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• v.30 no.5
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• pp.402-408
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• 2023

This study focused on improving the phase stability and mechanical properties of yttria-stabilized zirconia (YSZ), commonly utilized in gas turbine engine thermal barrier coatings, by incorporating Gd₂O₃, Er₂O₃, and TiO₂. The addition of 3-valent rare earth elements to YSZ can reduce thermal conductivity and enhance phase stability while adding the 4-valent element TiO₂ can improve phase stability and mechanical properties. Sintered specimens were prepared with hot-press equipment. Phase analysis was conducted with X-ray diffraction (XRD), and mechanical properties were assessed with Vickers hardness equipment. The research results revealed that, except for Z10YGE10T, most compositions predominantly exhibited the t-phase. Increasing the content of 3-valent rare earth oxides resulted in a decrease in the monoclinic phase and an increase in the tetragonal phase. In addition, the t(400) angle decreased while the t(004) angle increased. The addition of 10 mol% of 3-valent rare-earth oxides discarded the t-phase and led to the complete development of the c-phase. Adding 10 mol% TiO₂ increased hardness than YSZ.

• Journal of the Korean Ceramic Society
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• v.40 no.6
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• pp.525-529
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• 2003

Biotribological properties, such as wear rate and friction coefficient, of 3Y-TZP and Low Temperature Degradation (LTD) free materials were investigated via a ball(SiC)-on-plate sliding wear test to evaluate the relationship between wear mechanism and phase transformation. Wear test was conducted with a sliding speed of 0.035 m/s at room temperature and at 25$0^{\circ}C$ in air under a normal load of 49 N, respectively. Although friction coefficient of 3Y-TZP was the lowest due to the fine grain size, the highest wear loss and rate were observed due to the debris of monoclinic grains introduced during sliding and their values increased drastically with raising temperature. However, the biotribological properties of LTD-free materials were insensitive to temperature due to the inertness of the phase transformation, suggesting that they may be applicable to the biomechanical parts.

• Journal of the Korean Ceramic Society
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• v.31 no.9
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• pp.1060-1068
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• 1994

Stable zirconia sol was prepared from zirconium butoxide Zr(OC4O9)4 as a precursor and ethylacetoacetate(EAcAc) or diethylene glycol(DEG) as a chelating agent under ambient agent under ambient atmosphere by Sol-Gel process. The sythesized sol was coated on 304 stainless steel substrate by dip coating, thereafter zirconia film could be obtained by heat-treatment at $600^{\circ}C$. The characteristics of coating film were determined by FT-IR, XRD, and ellipsometion peak represented Zr-O-Zr bonding of tetragonal phase was shown at 470cm-1. Crystallization of zirconia gel and film from amorphous state to tetragonal phase started at 40$0^{\circ}C$, and then transformed into monoclinic phase around $700^{\circ}C$. Zirconia film coated on 304 stainless steel substrate showed relatively low porosity of 16% when it was coated with 0.4M zirconia sol and thereafter heat-treated at 80$0^{\circ}C$ and the film was densified continuously up to 90$0^{\circ}C$. The zirconia film of 10 nm thick acted as a protective layer against oxidation up to $700^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.47 no.5
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• pp.439-444
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• 2010

The usual ceramic process of mixing and milling in state of oxide of $ZrO_2$ and $CeO_2$ was adopted in wet process to manufacture Ce-TZP in this study. The maximum dispersion point of every slurry manufactured with mixture of $ZrO_2$ and $CeO_2$ was neat at pH10. The stable slurry in average particle size of 90 nm can be manufactured when it is dispersed with use of ammonia water and polycarboxylic acid ammonium. The sintered Ce-TZP ceramics manufactured with addition of $CeO_2$ less than 10 mol% was progressed to the fracture of specimen due to the monoclinic phase existence more than 30% at the room temperature. More than 99% of tetragonal phase was created for the sintered body with addition of $CeO_2$ beyond 18 mol%, but the mechanical property degrade on the entire specimen was brought due to the $CeO_2$ existing above 3%. Consequently, the optimal Ce-TZP combined in oxide state was identified in 16 mol% of $CeO_2$ contents.

• Nuclear Engineering and Technology
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• v.55 no.5
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• pp.1885-1891
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• 2023

The present work aims to fabricate Na_1+xZr₂Si_xP_3-xO₁₂ compound at various calcination temperatures based on the zircon mineral. The fabricated compound was calcinated at 250, 500, and 1000℃. The effect of calcination temperature on the structure, crystal phase, and radiation shielding properties was studied for the fabricated compound. The X-ray diffraction diffractometer demonstrates that, the monoclinic crystal phase appeared at a calcination temperature of 250℃ and 500℃ is totally transformed to a high-symmetry hexagonal crystal phase under a calcination temperature of 1000℃. The radiation shielding capacity was also qualified for the fabricated compounds using the Monte Carlo N-Particle transport code in the g-photons energy interval between 15keV and 122keV. The impacts of calcination temperature on the g-ray shielding behavior were clarified in the present study, where the linear attenuation coefficient was enhanced by 218% at energy of 122keV, when the calcination temperature increased from 250 to 1000℃, respectively.

• The Journal of Advanced Prosthodontics
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• v.11 no.1
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• pp.1-6
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• 2019

PURPOSE. The purpose of this in vitro study was to evaluate the effect of surface grinding and polishing procedures using high speed zirconia diamond burs with different grit sizes on the phase transformation and flexural strength of zirconia. MATERIALS AND METHODS. Forty disc shape specimens ($15{\times}1.25mm$) with a cylindrical projection in the center of each disc ($1{\times}3mm$) were fabricated with 3Y-TZP (Prettau, Zirkonzahn, Italy). The specimens were divided into 4 groups (n=10) according to the grinding and polishing procedures: Control group - grinding (coarse-grit diamond bur), Group 1 - grinding (coarse-grit diamond bur) + polishing, Group 2 - grinding (fine-grit diamond bur) + polishing, and Group 3 - grinding (fine grit diamond bur). Each specimen was analyzed by 3D-OM, XRD analysis, and biaxial flexural strength test. RESULTS. Based on the surface morphology by 3D-OM images, polished specimens showed smoother surface and lower roughness value (Ra). In the result of XRD analysis, partial phase transformation from tetragonal to monoclinic zirconia occurred in all groups. Control group, ground with a coarse grit diamond bur, showed more $t{\rightarrow}m$ phase transformation and lower flexural strength than Groups 1 and 2 significantly. CONCLUSION. The flexural strength in all specimens after grinding and polishing showed over 500 MPa, and those were clinically acceptable. However, grinding with a coarse grit diamond bur without polishing induced the phase transformation and low strength. Therefore, surface polishing is required for the occlusal adjustment using a high speed zirconia diamond bur to reduce the phase transformation and to prevent the decrease of flexural strength of zirconia.

• The Journal of Advanced Prosthodontics
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• v.6 no.3
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• pp.224-232
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• 2014

PURPOSE. The purpose of the present study was to evaluate the effect of thermocycling and mechanical loading on the biaxial flexural strength and the phase transformation of one Ce-TZP/$Al_2O_3$ and two Y-TZP core materials. MATERIALS AND METHODS. Thirty disc-shaped specimens were obtained from each material. The specimens were randomly divided into three groups (control, thermocycled, and mechanically loaded). Thermocycling was subjected in distilled water for 10000 cycles. Mechanical loading was subjected with 200 N loads at a frequency of 2 Hz for 100000 times. The mean biaxial flexural strength and phase transformation of the specimens were tested. The Weibull modulus, characteristic strength, 10%, 5% and 1% probabilities of failure were calculated using the biaxial flexural strength data. RESULTS. The characteristic strengths of Ce-TZP/$Al_2O_3$ specimens were significantly higher in all groups compared with the other tested materials (P<.001). Statistical results of X-ray diffraction showed that thermocycling and mechanical loading did not affect the monoclinic phase content of the materials. According to Raman spectroscopy results, at the same point and the same material, mechanical loading significantly affected the phase fraction of all materials (P<.05). CONCLUSION. It was concluded that thermocycling and mechanical loading did not show negative effect on the mean biaxial strength of the tested materials.

• Restorative Dentistry and Endodontics
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• v.46 no.4
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• pp.54.1-54.10
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• 2021

Objectives: The purpose of this study was to quantify phase transformation after hydrofluoric acid (HF) etching at various concentrations on the surface of yttria-stabilized tetragonal zirconia polycrystal (Y-TZP), and to evaluate changes in bonding strength before and after thermal cycling. Materials and Methods: A group whose Y-TZP surface was treated with tribochemical silica abrasion (TS) was used as the control. Y-TZP specimens from each experimental group were etched with 5%, 10%, 20%, and 40% HF solutions at room temperature for 10 minutes. First, to quantify the phase transformation, Y-TZP specimens (n = 5) treated with TS, 5%, 10%, 20% and 40% HF solutions were subjected to X-ray diffraction. Second, to evaluate the change in bond strength before and after thermal cycling, zirconia primer and MDP-containing resin cement were sequentially applied to the Y-TZP specimen. After 5,000 thermal cycles for half of the Y-TZP specimens, shear bond strength was measured for all experimental groups (n = 10). Results: The monoclinic phase content in the 40% HF-treated group was higher than that of the 5%, 10%, and 20% HF-treated groups, but lower than that of TS-treated group (p < 0.05). The 40% HF-treated group showed significantly higher bonding strength than the TS, 5%, and 10% HF-treated groups, even after thermal cycling (p < 0.05). Conclusions: Through this experiment, the group treated with SiO₂ containing air-borne abrasion on the Y-TZP surface showed higher phase transformation and higher reduction in bonding strength after thermal cycling compared to the group treated with high concentration HF.

• Journal of the Korean Ceramic Society
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• v.24 no.3
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• pp.243-250
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• 1987

The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.