• 한국재료학회지
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• 제29권4호
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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).

• 대한치과보철학회지
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• 제49권2호
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• pp.120-127
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• 2011

연구 목적: 본 연구의 목적은 색소체인 크롬염화물을 지르코니아에 첨가함으로써 지르코니아의 색상 및 물리적 성질, 그리고 미세구조가 어떻게 변화하는지 알아보고자 한다. 연구 재료 및 방법: 크롬염화물의 함량이 지르코니아 분말에 각각 0.06, 0.12, 0.25 wt%가 되도록 측량하고 알코올에 녹여 액상상태의 크롬염화물을 준비하였다. 지르코니아 분말과 각각의 액상상태의 크롬염화물을 혼합하고 혼합된 분말을 이용하여 디스크형태의 지르코니아 시편을 제작하였다. 제작된 시편은 $1450^{\circ}C$에서 완전소결 후 색상 및 물리적 성질, 그리고 미세구조를 관찰하였다. 색상은 분광측색장치를 이용하여 국제조명위원회 (CIE) ISO 기준인 D65 광원, SCE 방식으로 측정하여 $L^*$, $C^*$, $a^*$, $b^*$ 값으로 분석하였다. 밀도는 아르키메데스 법으로 측정하였고, 주사전자현미경과 X선 회절 분석기를 이용하여 시편의 미세구조 및 결정상을 관찰하였다. 파괴인성은 압흔 형성법(Vickers indentation법)을 이용하여 시편에 압흔 형성 후, 광학현미경으로 압흔의 크기를 측정하고 이를 이용하여 파괴인성을 구하였다. 결과는 일원배치분산분석 (one-way ANOVA)으로 통계처리 하였고, Tukey test로 사후 검정하였다. 결과: 1. 크롬염화물을 첨가하여 지르코니아의 색상을 조절할 수 있음을 확인하였으며, 크롬염화물 첨가 함량이 증가함에 따라 지르코니아 색상은 백색계통의 갈색에서 짙은 색의 갈색으로 변하였다. 2. 크롬염화물의 첨가는 시편의 밀도를 점점 감소시켰으며, 크롬염화물이 첨가되지 않은 시편과 비교 시, 크롬염화물의 첨가량이 증가할수록 통계학적으로 유의한 차이를 보였다 (P<.05). 3. 크롬염화물이 첨가된 시편은 첨가되지 않는 시편에 비해 결정립 크기가 증가하였다. 4. X-선 회절 분석결과, 크롬염화물의 첨가 여부와 첨가 함량에 상관없이 지르코니아 결정상의 차이점은 관찰되지 않았다. 5. 지르코니아에 크롬염화물을 첨가 시 크롬염화물의 첨가 함량에 따라 파괴인성값은 감소하였고, 특히 0.25 wt%의 크롬염화물을 첨가 시 가장 낮은 파괴인성 값을 보였다 (P<.05). 결론: 이상의 결과로 크롬염화물을 액체상태로 첨가하여 지르코니아의 색상을 조절할 수 있음을 확인하였으며, 제작한 유색 지르코니아의 색상은 자연치아 색상과 다소 차이가 있지만, 본 소재는 임상에서 사용되는 완전도재관 코어 (Core) 재료로써 사용할 수 있을 것으로 생각한다.

• The Journal of Advanced Prosthodontics
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• 제14권2호
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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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• 제9권5호
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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.

• 대한치과기공학회지
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• 제38권4호
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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.

• 대한치과교정학회지
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• 제53권3호
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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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• 제26권11호
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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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• 제7권1호
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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.

• 대한치과보철학회지
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• 제53권4호
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• pp.318-324
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• 2015

목적: 본 연구에서는 서로 다른 인산염계 기능성 단량체가 첨가된 5종의 자가 접착 레진시멘트와 지르코니아 사이의 열순환 전후 전단결합강도를 비교 평가하고자 하였다. 재료 및 방법: Airborne particle abrasion ($50{\mu}m$ $Al_2O_3$)을 시행한 디스크 모양의 Y-TZP 지르코니아 블록을 총 100개 준비하였다. 그리고 composite resin cylinder ($Filtek^{TM}$ Z250, 3M ESPE, St. Paul, MN, USA) 100개를 준비하였다. 서로 다른 인산염계 기능성 단량체가 첨가된 5종의 이중 중합형 자가 접착 레진시멘트 즉, Permacem 2.0 (DMG, Hamburg, Germany), $Clearfil^{TM}$ SA Luting (Kuraray Medical, Tokyo, Japan), $Multilink^{(R)}$ Speed (Ivoclar Vivadent, Schaan, Liechtenstein), $RelyX^{TM}$ U200 Automix (3M ESPE, Neuss, Germany), G-Cem $LinkAce^{TM}$ (GC Corporation, Tokyo, Japan)를 이용하여 지르코니아 블록과 composite resin cylinder를 접착하고 1군당 20개의 시편을 갖는 5개의 군을 만들었다. 시편을 $37^{\circ}C$ 의 증류수에 24시간 동안 보관한 후 각 군의 시편 절반(n=10)은 곧 바로 그리고 나머지 절반(n=10)은 5000회 열순환(5 - $55^{\circ}C$) 후에 전단결합강도를 측정하였다. 파절면은 FE-SEM을 이용하여 관찰하였다. 통계분석은 레진시멘트 종류 및 열순환 유무에 따른 전단결합강도의 비교를 위해 Two/One-way ANOVA를 시행하고 Tukey HSD post-hoc test를 이용하여 사후 검정하였으며, 열순환 전후의 비교를 위해 paired t-test를 이용하였다($\alpha$=.05). 결과: 열순환 전과 후 모두 $Multilink^{(R)}$ Speed 군은 나머지 4종류의 시멘트 군 보다 큰 전단결합강도를 나타내었다. G-Cem $LinkAce^{TM}$ 군은 열순환 전과 비교하여 열순환 후에 유의하게 낮은 전단결합강도를 나타내었지만, 다른 4종류 군은 열순환 전후 유의한 차이가 없었다. 결론: 인산염계 단량체를 포함한 대부분의 이중 중합형 자가 접착 레진시멘트는 지르코니아와 높은 전단결합강도를 보이고 열순환에 의해 유의한 영향을 받지 않아 지르코니아 보철물의 접착에 유용할 것이라고 사료된다.