• Korean Journal of Materials Research
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• v.29 no.4
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• pp.233-240
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• 2019

This study analyzes the mechanical properties, including the attrition rate, of $50{\mu}m$ size yttria-stabilized zirconia (YSZ) beads with different microstructures and high-energy milling conditions. The yttria distribution in the grain and grain-boundary of the fully sintered beads relates closely to Vickers hardness and the attrition rate of the YSZ beads. Grain size, fractured surfaces, and yttrium distribution are analyzed by electronic microscopes. For standardization and a reliable comparison of the attrition rate of zirconia beads with different conditions, Zr content in milled ceramic powder is analyzed and calculated by X-ray Fluorescence Spectrometer(XRF) instead of directly measuring the weight change of milled YSZ beads. The beads with small grain sizes sintered at lower temperature exhibit a higher Vickers hardness and lower attrition rate. The attrition rate of $50{\mu}m$ YSZ beads is measured and compared with the various materials properties of ceramic powders used for high-energy milling. The attrition rate of beads appears to be closely related to the Vickers hardness of ceramic materials used for milling, and demonstrates more than a 10 times higher attrition rate with Alumina(Hv ~1650) powder than $BaTiO_3$ powder (Hv ~315).

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.2
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• pp.120-127
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• 2011

Purpose: The purpose of this study was to examine the effects of chromium chloride addition on coloration, mechanical property and microstructure of 3Y-TZP. Materials and methods: Chromium chloride was weighed as 0.06, 0.12, and 0.25 wt% and each measured amount was dissolved in alcohol. $ZrO_2$ powder was mixed with each of the individual slurry to prepare chromium doped zirconia specimen. The color, physical properties and microstructure were observed after the zirconia specimen were sintered at $1450^{\circ}C$. In order to evaluate the color, spectrophotometer was used to analyze the value of $L^*$, $C^*$, $a^*$ and $b^*$, after placing the specimen on a white plate, and measured according to the International Commission on Illumination (CIE) standard, Illuminant D65 and SCE system. The density was measured in the Archimedes method, while microstructures were evaluated by using the scanning electron microscopy (SEM) and XRD. Fracture toughness was calculated Vickers indentation method and indentation size was measured by using the optical microscope. The data were analyzed with 1-way ANOVA test (${\alpha}$ = 0.05). The Tukey multiple comparison test was used for post hocanalysis. Results: 1. Chromium chloride rendered zirconia a brownish color. While chromium chloride content was increased, the color of zirconia was changed from brownish to brownish-red. 2. Chromium chloride content was increased; density of the specimen was decreased. 3. More chromium chloride in the ratio showed increase size of grains. 4. But the addition of chromium chloride did not affect the crystal phase of zirconia, and all specimens showed tetragonal phase. 5. The chromium chloride in zirconia did not showed statistically significant difference in fracture toughness, but addition of 0.25 wt% showed a statistically significant difference (P<.05). Conclusion: Based on the above results, this study suggests that chromium chlorides can make colored zirconia while adding in a liquid form. The new colored zirconia showed a slight difference in color to that of the natural tooth, nevertheless this material can be used as an all ceramic core material.

• The Journal of Advanced Prosthodontics
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• v.14 no.2
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• pp.122-132
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• 2022

PURPOSE. This in-vitro analysis aimed to compare the intaglio trueness, the antagonist's wear volume loss, and fracture load of various single-unit zirconia prostheses fabricated by different manufacturing techniques. MATERIALS AND METHODS. Zirconia crowns were prepared into four different groups (n = 14 per group) according to the manufacturing techniques and generations of the materials. The intaglio surface trueness (root-mean-square estimates, RMS) of the crown was measured at the marginal, axial, occlusal, and inner surface areas. Half of the specimens were artificially aged in the chewing simulator with 120,000 cycles, and the antagonist's volume loss after aging was calculated. The fracture load for each crown group was measured before and after hydrothermal aging. The intaglio trueness was evaluated with Welch's ANOVA and the antagonist's volume loss was assessed by the Kruskal-Wallis tests. The effects of manufacturing and aging on the fracture resistance of the tested zirconia crowns were determined by two-way ANOVA. RESULTS. The trueness analysis of the crown intaglio surfaces showed surface deviation (RMS) within 50 ㎛, regardless of the manufacturing methods (P = .053). After simulated mastication, no significant differences in the volume loss of the antagonists were observed among the zirconia groups (P = .946). The manufacturing methods and simulated chewing had statistically significant effects on the fracture resistance (P < .001). CONCLUSION. The intaglio surface trueness, fracture resistance, and antagonist's wear volume of the additively manufactured 3Y-TZP crown were clinically acceptable, as compared with those of the 4Y- or 5Y-PSZ crowns produced by subtractive milling.

• The Journal of Advanced Prosthodontics
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• v.9 no.5
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• pp.394-401
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• 2017

PURPOSE. The purpose of this study was to compare the optical properties of pre-colored dental monolithic zirconia ceramics of various thicknesses sintered in a microwave and those in a conventional furnace. MATERIALS AND METHODS. A2-shade of pre-colored monolithic zirconia ceramic specimens ($22.0mm{\times}22.0mm$) in 3 thickness groups of 0.5, 1.0, and 1.5 mm were divided into 2 subgroups according to the sintering methods (n=9): microwave and conventional sintering. A spectrophotometer was used to obtain CIELab color coordinates, and translucency parameters and CIEDE2000 color differences (${\Delta}E_{00}$) were measured. The relative amount of monoclinic phase ($X_m$) was estimated with x-ray diffraction. The surface topography was analyzed by atomic force microscope and scanning electron microscope. Statistical analyses were conducted with two-way ANOVA (${\alpha}=.05$). RESULTS. There were small interaction effects on CIE $L^*$, $a^*$, and TP between sintering method and thickness (P<.001): $L^*$ (partial eta squared ${{\eta}_p}^2=0.115$), $a^*$ (${{\eta}_p}^2=0.136$), and TP (${{\eta}_p}^2=0.206$), although higher $b^*$ values were noted for microwave sintering regardless of thickness. Color differences between two sintering methods ranged from 0.52 to 0.96 ${\Delta}E_{00}$ units. The $X_m$ values ranged from 7.03% to 9.89% for conventional sintering, and from 7.31% to 9.17% for microwave sintering. The microwave-sintered specimen demonstrated a smoother surface and a more uniform grain structure compared to the conventionally-sintered specimen. CONCLUSION. With reduced processing time, microwave-sintered pre-colored dental monolithic zirconia ceramics can exhibit similar color perception and translucency to those by conventional sintering.

• Journal of Technologic Dentistry
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• v.38 no.4
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• pp.281-290
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• 2016

Purpose: The increased aesthetic requirements and demands of patients have resulted in the developments of coloring liquid for zirconia. Methods: In this study, zirconia block was dipped into $Fe(NO_3)_3$solution, which showed a color and then concentration of $Fe(NO_3)_3$and zirconia's color and physical properties depending on the dipping time were observed and compared with exclusive coloring solutions. As the result, the following conclusions were obtained. Results: When compared with the specimens that were colored using exclusive solutions, $L^*$ value rose overall depending on the concentration of $Fe(NO_3)_3$and $a^*$ value was red in the form of (+) in all the specimens. Also, $b^*$ value was in the form of (+) at 0.5 to $1{\ss}fl$, but was in the form of (-) at 1.5 to $2{\ss}fl$. The dipping time did not highly influence $L^*$ value, but $a^*$ value and $b^*$ value were directly opposite to the specimens, which were not colored, except the sample that was dipped for only 2 seconds. When compared with exclusive coloring solutions, $Fe(NO_3)_3$had the most similar color at 0.5 to $1{\ss}fl$ and the longer the coloring time, the higher the rate of color change became. In relation to the density change depending on the addition of $Fe(NO_3)_3$, there was the lowest density at $2{\ss}fl$ and the density was increased in the specimens that were not colored. Conclusion: These results show that $Fe(NO_3)_3$solution can be used to make colored zirconia. It is expected that newly made colored zirconia can be used in clinical practice because the colored zirconia not only possesses the mechanical properties that all ceramic core material should have but also was biocompatible to a living cells.

• The korean journal of orthodontics
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• v.53 no.3
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• pp.139-149
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• 2023

Objective: To assess the color stability and translucency of full cubic stabilized zirconia (FSZ) following orthodontic bonding with different surface treatments and coffee thermocycling (CTC). Methods: This in vitro study was conducted on 120 disc-shaped specimens of FSZ. Thirty specimens were selected as the control group and remained intact. The remaining specimens were randomly divided into three groups based on the type of surface treatment (n = 30): airborne particle abrasion (APA), silica-coating (CoJet), and carbon dioxide (CO₂) laser. After metal bracket bonding in the test groups, debonding and polishing were performed. Subsequently, all specimens underwent CTC (10,000 cycles). Color parameters, color difference (ΔE₀₀), and translucency parameter (TP) were measured three times at baseline (t0), after debonding and polishing (t1), and after CTC (t2). Data were statistically analyzed (α = 0.05). Results: Significant difference existed among the groups regarding ΔE₀₀t0t2 (p < 0.001). The APA group showed minimum (ΔE₀₀ = 1.15 ± 0.53) and the control group showed maximum (ΔE₀₀ = 0.19 ± 0.02) color stability, with no significant difference between the laser and CoJet groups (p = 0.511). The four groups were significantly different regarding ΔTPt0t2 (p < 0.001). Maximal increases in TP were noted in the CoJet (1.00 ± 0.18) and APA (1.04 ± 0.38) groups while minimal increase was recorded in the control group (0.1 ± 0.02). Conclusions: Orthodontic treatment makes zirconia restorations susceptible to discoloration and increased translucency. Nonetheless, the recorded ΔE₀₀ and ΔTP did not exceed the acceptability threshold.

• Bulletin of the Korean Chemical Society
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• v.26 no.11
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• pp.1795-1802
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• 2005

Potential energy curves and internuclear (M-X) distance variations for dissociation reactions of $[MX_4]^{2-}$ into ($[MX_3]^-$ + $X^-$) have been calculated using ab initio Hartree-Fock (HF), second order M$\ddot{o}$ller-Plesset perturbation (MP2), and Density Functional Theory (DFT) methods with a triple zeta plus polarization (TZP) basis set. The equilibrium geometrical structures of $[MX_4]^{2-}$ are optimized to tetrahedral geometry for $[NiX_4]^{2-}$ and square planar geometry for ($[PdX_4]^{2-}$ and $[PtX_4]^{2-}$). The bond (M-X) distances of $[NiCl_4]^{2-}$, $[NiBr_4]^{2-}$, $[PdCl_4]^{2-}$, $[PdBr_4]^{2-}$, $[PtCl_4]^{2-}$, and $[PtBr_4]^{2-}$ at the DFT level are 2.258, 2.332, 2.351, 2.476, 2.367, and 2.493 $\AA$, respectively. The dissociation energies for the bond dissociation of ($[MX_3]^-$${\cdot}{\cdot}{\cdot}$$X^-$) at the DFT level are found to be 4.73 eV for $[NiCl_4]^{2-}$, 4.89 eV for $[NiBr_4]^{2-}$, 4.93 eV for $[PdCl_4]^{2-}$, 5.57 eV for $[PdBr_4]^{2-}$, 5.44 eV for $[PtCl_4]^{2-}$, and 5.87 eV for $[PtBr_4]^{2-}$. As the (M${\cdot}{\cdot}{\cdot}$X) distance of ($[MX_3]^-$${\cdot}{\cdot}{\cdot}$$X^-$) increases, the distance variation (Rt) of trans (M-X) bond at the trans-position is shorter than those (Rc) of two cis (M-X) bonds at the cisposition. Simultaneously the atomic charge variation of trans-X atom is more positive than those of equilibrium $[MX_4]^{2-}$ structures, while the variation of leaving X group is more positive.

• The Journal of Advanced Prosthodontics
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• v.7 no.1
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• pp.1-7
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• 2015

PURPOSE. This study was performed to evaluate shear bond strength (SBS) between three dual-cured resin cements and silica coated zirconia, before and after thermocycling treatment. MATERIALS AND METHODS. Sixty specimens were cut in $15{\times}2.75mm$ discs using zirconia. After air blasting of $50{\mu}m$ alumina, samples were prepared by tribochemical silica coating with $Rocatec^{TM}$ plus. The specimens were divided into three groups according to the dual-cure resin cement used: (1) Calibra silane+$Calibra^{(R)}$, (2) Monobond S+$Multilink^{(R)}$ N and (3) ESPN sil+$RelyX^{TM}$ Unicem Clicker. After the resin cement was bonded to the zirconia using a Teflon mold, photopolymerization was carried out. Only 10 specimens in each group were thermocycled 6,000 times. Depending on thermocycling treatment, each group was divided into two subgroups (n=10) and SBS was measured by applying force at the speed of 1 mm/min using a universal testing machine. To find out the differences in SBS according to the types of cements and thermocycling using the SPSS, two-way ANOVA was conducted and post-hoc analysis was performed by Turkey's test. RESULTS. In non-thermal aged groups, SBS of Multilink group (M1) was higher than that of Calibra (C1) and Unicem (U1) group (P<.05). Moreover, even after thermocycling treatment, SBS of Multilink group (M2) was higher than the other groups (C2 and U2). All three cements showed lower SBS after the thermocycling than before the treatments. But Multilink and Unicem had a significant difference (P<.05). CONCLUSION. In this experiment, Multilink showed the highest SBS before and after thermocycling. Also, bond strengths of all three cements decreased after thermocycling.

• The Journal of Korean Academy of Prosthodontics
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• v.53 no.4
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• pp.318-324
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• 2015

Purpose: This study compared shear bond strengths of five self-adhesive cements with phosphate monomer to zirconium oxide ceramic with and without airborn particle abrasion. Materials and methods: One hundred zirconia samples were air-abraded ($50{\mu}mAl_2O_3$). One hundred composite resin cylinders were fabricated. Composite cylinders were bonded to the zirconia samples with either Permacem 2.0 (P), $Clearfil^{TM}$ SA Luting (C), $Multilink^{(R)}$ Speed (M), $RelyX^{TM}$ U200 Automix (R), G-Cem $LinkAce^{TM}$ (G). All bonded specimens were stored in distilled water ($37^{\circ}C$) for 24 h and half of them were additionally aged by thermocycling ($5^{\circ}C$, $55^{\circ}C$, 5,000 times). The bonded specimens were loaded in shear force until fracture (1 mm/min) by using Universal Testing Machine (Model 4201, Instron Co, Canton, MA, USA). The failure sites were inspected under field-emission scanning electron microscopy. The data was analyzed with ANOVA, Tukey HSD post-hoc test and paired samples t-test ($\alpha$=.05). Results: Before and after thermocycling, $Multilink^{(R)}$ Speed (M) revealed higher shear-bond strength than the other cements. G-Cem $LinkAce^{TM}$ (G) showed significantly lower bond strengths after thermocycling than before treatment (P<.05), but the other groups were not significantly different (P>.05). Conclusion: Most self-adhesive cements with phosphate monomer showed high shear bond strength with zirconia ceramic and weren't influenced by thermocycling, so they seem to valuable to zirconia ceramic bonding.