• The Journal of Advanced Prosthodontics
• /
• v.1 no.3
• /
• pp.113-117
• /
• 2009

STATEMENT OF PROBLEM. Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported. PURPOSE. The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM). MATERIAL AND METHODS. Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad $S\ddot{a}ckingen$, Germany) were prepared in 40 mm (length) $\times$ 4 mm (width) $\times$ 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and $225^{\circ}C$ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences ($\alpha$= .05). RESULTS. The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below $125^{\circ}C$ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above $150^{\circ}C$, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa. CONCLUSION. The monoclinic phase started to appear after aging treatment above $100^{\circ}C$. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above $175^{\circ}C$. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

• The Journal of Advanced Prosthodontics
• /
• v.11 no.5
• /
• pp.253-261
• /
• 2019

PURPOSE. To evaluate the influence of cyclic loading on phase transformation of zirconia abutments and to compare the effectiveness of three different quantitative ageing assessment techniques. MATERIALS AND METHODS. Thirty two Y-TZP prostheses fabricated from two brands, InCoris ZI and Ceramill ZI, were cemented to titanium bases and equally divided into two subgroups (n=8): control group without any treatment and aged group with cyclic loading between 20 N and 98 N for 100,000 cycles at 4 Hz in distilled water at $37^{\circ}C$. The tetragonal-to-monoclinic phase transformation was assessed by (i) conventional x-ray diffraction (XRD), (ii) micro x-ray diffraction (${\mu}XRD$), and (iii) micro-Raman spectroscopy. The monoclinic-phase fractions (M%) were compared by two-way ANOVA. RESULTS. InCoris Zi presented significantly higher M% than Ceramill Zi in both control and aged groups (P<.001). Both materials exhibited significant phase transformation with monoclinicphase of 1 to 3% more in aged groups than controls for all three assessment techniques. The comparable M% was quantified by both ${\mu}XRD$ and XRD. The highest M% was assessed with micro-Raman. CONCLUSION. Cyclic loading produced significant phase transformation in tested Y-TZP prostheses. The micro-Raman spectroscopy could be used as an alternative to XRD and ${\mu}XRD$.

• Journal of Technologic Dentistry
• /
• v.33 no.3
• /
• pp.193-202
• /
• 2011

Purpose: The aim of this study was to evaluate the effect of pre-treatment of core and hydrothermal treatment on the bond strength and flexural strength of ceramic veneered zirconia. Methods: 3Y-TZP specimens(KaVo Zr, $25mm{\times}3mm{\times}1mm$)were prepared by five pre-treatment methods and divided into seven groups including control two groups, subsequently the specimens veneered with the E-MAX ceram according to manufacturer's information(total specimen thickness 1.5mm). Two groups from ceramic-zirconia specimens(n=105, n=15 per group)were assigned into two experimental fatigue conditions, namely storage in an autoclave at $134^{\circ}C$ for 5h, thermo-cycling(3,000cycles, between 5 and $55^{\circ}C$, dwell time 45s, transfer time 2s). A flexural strength test was performed in a universal testing machine(crosshead speed: 0.5mm/min). Data were statistically analyzed using one-way ANOVA and Tukey's test(${\alpha}$=0.05). Results: The ceramic-zirconia bond strength value for liner application group(LLW, $27.3{\pm}3.8$) were significantly lower than those of the pre-treatment groups($30.72{\pm}5.3$). The ceramic-zirconia bond strength and zirconia flexural strength was not affected by thermo-cycling(p>0.05), whereas it was affected by storage in an autoclave at $134^{\circ}C$ for 5h(p<0.05). Conclusion: The results indicated that the ceramic-zirconia bond strength and zirconia flexural strength was affected by low temperature degradation.

• 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.24 no.12
• /
• pp.677-681
• /
• 2014

To increase the mechanical property of zirconia, we have investigated the phase change and the resulting hardness of zirconia ceramics by hydroxyapatite (HA) powder bed sintering. It was observed using X-ray diffraction that the cubic zirconia phase, which has a higher hardness value than that of the tetragonal phase, was obtained at the surface of 3 mol% $Y_2O_3$ doped tetragonal zirconia polycrystal (3Y-TZP) ceramics during the sintering process; in our experimental conditions, the phase change at the surface increased as the sintering time increased. We believe that the observed crystalline phase change originated from the decomposition of HA and the diffusion of CaO, as follows. CaO, which was derived from the decomposition of HA at high temperature ($1400^{\circ}C$), diffused into the surface of 3Y-TZP and acted as a stabilizer. As a result, the Vickers hardness value of the treated specimens was higher than that of the non-treated specimen due to the formation of the cubic phase on the surface of 3Y-TZP.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 2001.05a
• /
• pp.160-160
• /
• 2001

• Journal of Korean Dental Science
• /
• v.8 no.2
• /
• pp.82-88
• /
• 2015

Purpose: To evaluate the effect of light-curing on the immediate and delayed micro-shear bond strength (${\mu}SBS$) between yttria-tetragonal zirconia polycrystal (Y-TZP) ceramics and RelyX Ultimate when using Single Bond Universal (SBU). Materials and Methods: Y-TZP ceramic specimens were ground with #600-grit SiC paper. SBU was applied and RelyX Ultimate was mixed and placed on the Y-TZP surface. The specimens were divided into three groups depending on whether light curing was done after adhesive (SBU) and resin cement application: uncured after adhesive and uncured after resin cement application (UU); uncured after adhesive, but light cured after resin cement (UC); and light cured after adhesive and light cured resin cement (CC). The three groups were further divided depending on the timing of ${\mu}SBS$ testing: immediate at 24 hours (UUI, UCI, CCI) and delayed at 4 weeks (UUD, UCD, CCD). ${\mu}SBS$ was statistically analyzed using one-way ANOVA and Student-Newman-Keuls multiple comparison test (P<0.05). The surface of the fractured Y-TZP specimens was analyzed under a scanning electron microscope (SEM). Result: At 24 hours, ${\mu}SBS$ of UUI group ($8.60{\pm}2.06MPa$) was significantly lower than UCI group ($25.71{\pm}4.48MPa$) and CCI group ($29.54{\pm}3.62MPa$) (P<0.05). There was not any significant difference between UCI and CCI group (P>0.05). At 4 weeks, ${\mu}SBS$ of UUD group ($24.43{\pm}2.88MPa$) had significantly increased over time compared to UUI group (P<0.05). The SEM results showed mixed failure in UCI and CCI group, while UUI group showed adhesive failure. Conclusion: Light-curing of universal adhesive before or after application of RelyX Ultimate resin cement significantly improved the immediate ${\mu}SBS$ of resin cement to air-abrasion treated Y-TZP surface. After 4 weeks, the delayed ${\mu}SBS$ of the non-light curing group significantly improved to the level of light-cured groups.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.7 no.3
• /
• pp.377-383
• /
• 1997

Yttria-stabilized TZP alloyed with pentavalent oxides $(Ta_2O_5,\;Nb_2O_5)$ were fabricated by the conventional sintering method at $1500^{\circ}C$ in air to construct the simplified ternary phase diagram. The phase stability of tetragonal -$ZrO_2$ from the quasi-binary system $ZrO_2-YTa(Nb)O_4$, which do not transform to monoclinic-$ZrO_2$ even for a wide range of grain size and annealing temperature, was investigated to determine composition region of the non-transformable $t-ZrO_2$ solid solution$(NT_{ss})$. Phase stability of $NT_{ss}$ was probably due to the enhanced stability of $_YTa(Nb)O4$ having the tetragonal fergusonite structure. It was experimentally found that mixtures having $NT_{ss}$ alloyed with $T_{ss}$ by weight%% showed both excellent phase stability of $t-ZrO_2$ and fracture toughness even though the calculated composition of the mixture /was located outside $NT_{ss}$ composition region.

• The Journal of Advanced Prosthodontics
• /
• v.12 no.4
• /
• pp.197-203
• /
• 2020

PURPOSE. The aim of this study was to evaluate the effect of multiple firings on the bond strength between yttriatetragonal zirconia polycrystals (Y-TZP) and 2 types of resin cements. MATERIALS AND METHODS. Sixty 3Y-TZP specimens (LAVA Frame Multi) were divided into 3 groups depending on the following firing procedures: (1) 2-firing cycles, (2) 5-firing cycles, (3) 10-firing cycles. Two samples from each group were investigated by using SEM to determine the morphological changes. All specimens were treated with 125 ㎛ airborne-particle abrasion and the surface roughness of each specimen was measured. The specimens from each firing group were then further divided into 2 subgroups (n = 9) to apply 2 types of resin cement (MDP-free resin cement: RelyX Unicem-RU, and MDP containing resin cement: Panavia F 2.0-PA). The shear bond strength (SBS) test was performed and failure types of all the debonded specimens were classified by using a stereomicroscope as adhesive, cohesive, and mixed. The statistical analysis of surface roughness and SBS data were performed by using 1-way ANOVA and 2-way ANOVA followed by Tukey-HSD tests (α=.05). Failure modes were calculated as a percentage for each group. RESULTS. The bond strength of RU and PA to the specimens obtained with 2 firings were not statistically different from each other (P=.1). However, the SBS values of PA were found to be significantly higher than RU for the specimens obtained with 5 and 10 firing cycles (P=.001 and P=.02, respectively). Surface roughness analysis revealed no statistical difference between groups (P=.2). The SEM analysis of samples fired 5- and 10- times showed irregularities and boundary loss in zirconia grains, and empty spaces between zirconia grains. CONCLUSION. The bond strength of PA cement was higher than that of RU to the zirconia subjected to repeated firings (5 and 10 firing cycles). When zirconia is subjected to multiple firings, using MDP-containing resin cement can be recommended.

• Korean Journal of Materials Research
• /
• v.24 no.12
• /
• pp.652-657
• /
• 2014

The purpose of this study was to investigate the microstructures and mechanical properties of zirconia toughened alumina (ZTA) ceramics prepared from two kinds of 3Y-TZP powders. ZTA composites were prepared by adding two kinds of 3Y-TZP powders, 3YEH (BET = $7m^2/g$) and 3YEM (BET = $16m^2/g$), to ${\alpha}$-alumina in the range of 5-25 wt%. It was found that the microstructure photographs of the ZTA composites showed that the average grain size of alumina decreased as the content of zirconia increased. In our present study, specimens containing 3YEM zirconia exhibited smaller grain sizes compared to those of 3YEH zirconia. The Vickers hardness of the ZTA composites that were sintered at $1600^{\circ}C$ for 2 hrs was found to smoothly decrease with increasing zirconia content because of the low Young modulus in zirconia. The Vickers hardness of the ZTA containing 3YEH zirconia was greater than that of the 3YEM zirconia. In substance, the fracture toughness ($K_{1c}$) of the ZTA composites increased as the content of zirconia increased. The fracture toughness ($K_{1c}$) of ZTA containing 3YEM zirconia was greater than that of 3YEH zirconia.