• Journal of dental hygiene science
• /
• v.15 no.5
• /
• pp.577-584
• /
• 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 hygiene science
• /
• v.14 no.1
• /
• pp.29-34
• /
• 2014

The purpose of this study was to evaluate the influence of low temperature degradation (LTD) on the bonding strength of yttria-stabilized tetragonal zirconia polycrystal (Y-TZP). The push-shear bond test method was used to investigate the core-veneer bonding strength of industrially manufactured Y-TZP core ceramic and manufacturer recommended veneering ceramic. Four groups from ceramic-zirconia specimens (n=28; n=7 per group) were assigned into four experimental aging conditions, namely storage in an autoclave at $134^{\circ}C$ for 0, 3, 5, 10 hours. Bonding strength was obtained using a universal testing machine with crosshead speed 0.5 mm/min. Data were statistically analyzed using one-way ANOVA and Tukey's test (${\alpha}=0.05$). In bonding strength test, the group which was treated with LTD showed lower bonding strength than no treated group. The ceramic-zirconia bonding strength was affected by LTD (p<0.05). Digital microscope examination of the fracture surface showed mixed failures with adhesive and cohesive types in LTD with treated Y-TZP groups.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06b
• /
• pp.55-85
• /
• 1996

지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.

• Korean Journal of Materials Research
• /
• v.28 no.6
• /
• pp.349-354
• /
• 2018

Particle size reduction is an important step in many technological operations. The process itself is defined as the mechanical breakdown of solids into smaller particles to increase the surface area and induce defects in solids, which are needed for subsequent operations such as chemical reactions. To fabricate nano-sized particles, several tens to hundreds of micron size ceramic beads, formed through high energy milling process, are required. To minimize the contamination effects during high-energy milling, the mechanical properties of zirconia beads are very important. Generally, the mechanical properties of $Y_2O_3$ stabilized tetragonal zirconia beads are closely related to the mechanism of phase change from tetragonal to monoclinic phase via external mechanical forces. Therefore, $Y_2O_3$ distribution in the sintered zirconia beads must also be closely related with the mechanical properties of the beads. In this work, commercially available $100{\mu}m-size$ beads are analyzed from the point of view of microstructure, composition homogeneity (especially for $Y_2O_3$), mechanical properties, and attrition rate.

• Journal of Powder Materials
• /
• v.4 no.3
• /
• pp.179-187
• /
• 1997

Milling media of steel and zirconia were used to produce $MoSi_2$ by mechanical alloying (MA) of Mo and Si powders. The effect of milling media on MA of Mo-65.8at%Si powder mixture has been investigated by SEM, XRD, DTh and in-situ thermal analysis. The powders mechanically alloyed by milling medium of steel for 8 hours showed the structure of fine mixture of Mo and Si, and those mechanically alloyed by milling medium of zirconia for longer milling time showed the structure of fine mixture of Mo and Si. The tetragonal $\alpha$-$MoSi_2$ Phase and the tetragonal $Mo_5Si_3$ phase appeared with small Mo peaks in the powders milled by milling medium of steel for 4 and 8 hours. The $\alpha$-$MoSi_2$ phase and the hexagonal $\beta$-$MoSi_2$ phase were formed after longer milling time. The $\alpha$-$MoSi_2$ phase appeared with large Mo peaks in the powders milled by milling medium of zirconia for 4 hours. The phases, $\alpha$-$MoSi_2$ and $\beta$-$MoSi_2$. were formed in the powders milled for longer milling time. DTA and annealing results showed that Mo and Si were transformed into $\alpha$-$MoSi_2$ and $Mo_5Si_3$, while $\beta$-$MoSi_2$ into $\alpha$-$MoSi_2$. In-situ thermal analysis results demonstrated that there were a sudden temperature rise at 212 min and a gradual increase in temperature in case of milling media of steel and zirconia, respectively. The results indicate that MA can be influenced by materials of milling medium which can give either impact energy on powders or thermal energy accumulated in vial.

• Restorative Dentistry and Endodontics
• /
• v.45 no.4
• /
• pp.52.1-52.11
• /
• 2020

Objectives: Yttria-stabilized tetragonal phase zirconia has been used as a dental restorative material for over a decade. While it is still the strongest and toughest ceramic, its translucency remains as a significant drawback. To overcome this, stabilizing the translucency zirconia to a significant cubic crystalline phase by increasing the yttria content to more than 8 mol% (8YTZP). However, the biocompatibility of a high amount of yttria is still an important topic that needs to be investigated. Materials and Methods: Commercially available 8YTZP plates were used. To enhance cell adhesion, proliferation, and differentiation, the surface of the 8YTZP is sequentially polished with a SiC-coated abrasive paper and surface coating with type I collagen. Fibroblast-like cells L929 used for cell adherence and cell proliferation analysis, and mouse bone marrow-derived mesenchymal stem cells (BMSC) used for cell differentiation analysis. Results: The results revealed that all samples, regardless of the surface treatment, are hydrophilic and showed a strong affinity for water. Even the cell culture results indicate that simple surface polishing and coating can affect cellular behavior by enhancing cell adhesion and proliferation. Both L929 cells and BMSC were nicely adhered to and proliferated in all conditions. Conclusions: The results demonstrate the biocompatibility of the cubic phase zirconia with 8 mol% yttria and suggest that yttria with a higher zirconia content are not toxic to the cells, support a strong adhesion of cells on their surfaces, and promote cell proliferation and differentiation. All these confirm its potential use in tissue engineering.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 1998.11a
• /
• pp.311-314
• /
• 1998

The effects of the additions of transition metal oxides on ZrO$_2$ - Y$_2$O$_3$ (Y$_2$O$_3$ - containing tetragonal zirconia polycrystals : Y-TZP) system has been studied by investigating fracture toughness and phase stability of the sintered specimens. In the specimens sintered at 1450$^{\circ}C$ for 2hrs in air the phase transformation from tetragonal to monoclinic was observed. The ratios of monoclinic phase to tetragonal phase were changed with the additions of CoO, Fe$_2$O$_3$ and MnO$_2$, respectively, from 0.00 to 8.00wt%. The fracture toughness was increased with increasing the monoclinic to tetragonal phase ratio and was maximum at the ratio of about 18%. However, the hardness was decreased with increasing the ratio. The additions of CoO, Fe$_2$O$_3$ and MnO$_2$ together into Y-TZP resulted in more complex behaviors of fracture toughness and hardness. The specimen with the additions of 1.5wt% Fe$_2$O$_3$, 3.0wt% Al$_2$O$_3$ and 1.5wt% CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of 10.8 MPa.m$\^$$\frac{1}{2}$/ and Vickers hardness of 1201kgf/mm$^2$.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 2000.06a
• /
• pp.243-248
• /
• 2000

Effect of NiO addition on microstructure, stability of tetragonal phase and mechanical properties was investigated. (Y, Ni)-TZP solid solution was obtained by pressureless sintering. The fracture toughness was increased by solid solution of NiO. Neither reaction phase nor glassy phase was observed at the grain boundaries. From these results, it was determined that solid solution of NiO was destabilized tetragonal phase of Y-TZP. Y-TZP/Ni nanocomposite that contained nano-sized Ni particles was also fabricated by internal reduction method. Some evaluations and discussions were carried out for both (Y, Ni)-TZP solid solution and Y-TZP/Ni nanocomposite.

• Journal of the Korean Ceramic Society
• /
• v.28 no.7
• /
• pp.541-548
• /
• 1991

Sinterability and stability of TZP ceramics co-stabilized by 12 mol% CeO2 and divalent or trivalent oxides less than 1 mol% were investigated. Divalent and trivalent oxides increased stability of tetragonal ZrO2. 100% tetragonal ZrO2 phase was obtained by doping 12 mol% CeO2 and 0.2 mol% CaO and MgO respectively when sintering was carried out at 1500$^{\circ}C$ for 2 hours. Divalent and trivalent oxides improved sinterability and inhibit grain growth of ZrO2. And it was found that CaO was the most effective sintering aid and grain growth inhibitor for ZrO2 in this study. Incorporation of divalent and trivalent oxides into 12Ce-TZP increased the strength of 12Ce-TZP and particulary 12Ce, 0.4Ca-TZP exhibited a flexural strength of about twofold greater than 12Ce-TZP.

• Journal of the Korean Ceramic Society
• /
• v.30 no.12
• /
• pp.1059-1065
• /
• 1993

The sliding wear behavior of the plasma sprayed zirconia containing 8wt% yttria was investigated over a range of room temperature to 800℃. Both of the friction coefficient and the wear loss increased reaching its maximum at about to 499℃. and then decreased again with increasing temperature up to 800℃. The worn surface at elevated temperature were observed and analyzed by scanning electron microscopy and X-ray diffractometer to study the mechanisms of high temperature wear behavior. Surface morphology of the worn samples changes with temperature. Monoclinic (m)/tetragonal (t) x-ray peak intensity ratio of wear debris and worn surface decreased with increasing temperature. Non-transformable tetragonal (t') to metastable tetragonal (t) phase transformation of worn surface increased with increasing temperature. The results indicate that dehumidification and above phase changes are contributing to the high temperature wear behavior of the plasma sprayed ZrO2-Y2O3 coatings.