牙科氧化锆陶瓷的低温时效性能研究

目的 研究时效对5种牙科氧化锆陶瓷结构稳定性的影响.方法 5种氧化锆预烧结块(A组:TZ-3YS;B组:Vita In-Ceram YZ;C组:Ivoclar;D组:Cercon Smart;E组:Kavo)各切取15 mm×15 mm×1.5 mm氧化锆试件18片,常压致密烧结.时效处理如下:置于高温高压消毒炉中进行循环热处理,条件是134℃,0.2 MPa压力,维持时间为0h、1h、2h、3h、4 h、5h.X射线衍射分析(X-ray diffraction,XRD)试件的晶相结构,计算试件表面单斜相(m相)的相对含量.原子力显微镜观察A组和D组时效1、4 h的抛光试件.A组氧化锆再制备25 mm×4 mm×1.2 mm的试件30根,均分为未退火组(时效前)、退火组(时效前)和时效组(时效后),测试试件的三点弯曲强度.结果 除D组试件外,A、B、C、E组试件的m相含量均随时效时间的延长而增加,A组试件的m相含量最高,E组次之,B组和C组相近.XRD未检测到D组试件表面有m相,但使用原子力显微镜可观察到D组试件有m相晶核的成核和生长.时效前后A组试件的三点弯曲强度未衰减,未退火组试件三点弯曲强度[(1301±169)MPa]显著高于退火组[(1120±185)MPa]和时效组[(1158±111)MPa],差异有统计学意义(P＜0.05);而退火组与时效组间差异无统计学意义(P＞0.05).结论 牙科氧化锆陶瓷的低温时效效应具有时间依赖性,但时效效应并未使TZ-3YS的三点弯曲强度降低.     

Effect of in vitro aging on the flexural strength and probability to fracture of Y-TZP zirconia ceramics for all-ceramic restorations

ObjectivesDental zirconia restorations should present long-term clinical survival and be in service within the oral environment for many years. However, low temperature degradation could affect their mechanical properties and survival. The aim of this study was to investigate the effect of in vitro aging on the flexural strength of yttrium-stabilized (Y-TZP) zirconia ceramics for ceramic restorations.MethodsOne hundred twenty bar-shaped specimens were prepared from two ceramics (ZENO Zr (WI) and IPS e.max^® ZirCAD (IV)), and loaded until fracture according to ISO 6872. The specimens from each ceramic (n_x = 60) were divided in three groups (control, aged for 5 h, aged for 10 h). One-way ANOVA was used to assess statistically significant differences among flexural strength values (P < 0.05). The variability of the flexural strength values was analyzed using the two-parameter Weibull distribution function, which was applied for the estimation of Weibull modulus (m) and characteristic strength (σ₀). The crystalline phase polymorphs of the materials (tetragonal, t, and monoclinic, m, zirconia) were investigated by X-ray diffraction (XRD) analysis, Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy.ResultsA slight increase of the flexural strength after 5 h, and a decrease after 10 h of aging, was recorded for both ceramics, however statistically significant was for the WI group (P < 0.05). Both ceramics presented a t → m phase transformation, with the m-phase increasing from 4 to 5% at 5 h to around 15% after 10 h.SignificanceThe significant reduction of the flexural strength after 10 h of in vitro aging, suggests high fracture probability for one of the zirconia ceramics tested.     

Effect of fatigue on biaxial flexural strength of bilayered porcelain/zirconia (Y-TZP) dental ceramics

Objectives

The aim of this study was to evaluate the effect of fatigue on biaxial flexural strength of bilayered disks of two Y-TZP cores.

Methods

Twenty bilayered veneer/zirconia disks were fabricated from each material (Lava veneer + core, 3 M/ESPE, and Cercon veneer + core, Densply). Ten specimens from each material were tested for biaxial flexural strength either with or without being subjected to fatigue (20,000 cycles, 2 Hz, 200 N load) in a universal testing machine (1 mm/min). Stresses generated at the core and the veneer, at the top and the bottom surfaces, and the interface of bilayered disk were calculated using Huesh's solutions. Data were statistically analyzed using Weibull statistics. The fractured core was also examined via Raman spectroscopy and the monoclinic fraction was calculated at the top, the middle of thickness, and the bottom of the cross-section of fractured core. The results of monoclinic fraction were statistically analyzed by Three-Factor ANOVA with Repeated Measures on One Factor.

Results

Weibull modulus (m) of Cercon control (CC), Cercon fatigue (CF), Lava control (LC) and Lava fatigue (LF) were between 11.8 and 14.3, 7.1 and 13.1, 9.4 and 13, and 7.1 and 8.2, respectively. There were no significant differences between characteristic strength (σ₀) of CC (970.9 MPa) and CF (947.7 MPa) (p > 0.05). For Lava, σ₀ of LF (1444.8 MPa) was significantly higher than LC (1240.5 MPa) (p < 0.05). At the interfaces, σ₀ values of CC and CF groups were not significantly different while LF showed significantly higher σ₀ than LC. The monoclinic zirconia was significantly lower for CF than CC and significantly higher for LF than LC.

Significance

Fatigue showed different effects on the strength of Cercon and Lava ceramic systems. Decreases in m values were observed at the interfaces of two materials after fatigue.     

Relative flexural strength of dental restorative ceramics

The relative flexural strengths of ten brands of dental restorative ceramics were evaluated by a three-point bending test. The materials consisted of three low-fusing and one high-fusing feldspathic porcelains and six reinforced dental restorative ceramics which are currently in clinical use. The reinforced ceramic materials investigated utilized a number of different strengthening processes, including alumina and ceramic fiber reinforcement and controlled crystallization. The results of the investigation indicate that significant differences exist among the measured breaking strengths of the various materials. The processes of controlled crystallization and alumina reinforcement appear to be adequate means of improving the bending strength of restorative dental ceramics.     

Impact of different pretreatments and aging procedures on the flexural strength and phase structure of zirconia ceramics

ObjectiveTo test the impact of zirconia pretreatment and aging on flexural strength and phase structure.MethodsFor flexural strength measurements, 180 3Y-TZP_0.25 specimens were fabricated and pretreated: (i) air-abraded (105-μm alumina, 0.25 MPa), (ii) air-abraded (50-μm alumina, 0.25 MPa), (iii) air-abraded (30-μm silica-coated alumina, 0.28 MPa) (iv) non-pretreated. Each pretreated group (n = 15) was aged: (a) hydrothermal (134 °C, 0.23 MPa, 2 h) (b) in a mastication simulator (1,200,000×, 5/55 °C) and (c) not aged. The fractured specimens were stored dry for 5 years (23 °C) for analysis of phase transformation. Additionally, specimens were fabricated from 3Y-TZP_0.25 (n = 12) and 3Y-TZP_0.05 (n = 8), pretreated (i, ii, iii, iv), and hydrothermally aged. Each air-abrasion method was alternated using 0.05, 0.25 and 0.4 MPa pressure. The phase transformation was examined by Raman spectroscopy and surface topography by scanning electron microscope. Data were analyzed using univariate ANOVA with the Scheffé post hoc test and partial-eta-squared (?_p²) (α = 0.05).ResultsThe highest impact on flexural strength was exerted by the pretreatment (η_P² = 0.261, p < 0.001), followed by interactions between pretreatment and aging (η_P² = 0.077, p = 0.033). Non-pretreated and non-aged specimens showed the lowest monoclinic percentage. Hydrothermal aging and 5 years of storage at room temperature increased the monolithic percentage of 3Y-TZP_0.25. The highest phase transformation was observed in groups air-abraded with 105-μm alumina particles. Increasing pressure during the air-abrading process increased the content of the monoclinic phase in zirconia surfaces.SignificanceAir-abrasion with 30-μm silica-coated alumina powder can be recommended for pretreatment of 3Y-TZP_0.25 and 3Y-TZP_0.05. For air-abrasion using alumina powder lower pressure should be used.     

Influence of grinding procedures on the flexural strength of zirconia ceramics

The surface of zirconia may be damaged during grinding, influencing the mechanical properties of the material. The purpose of this study was to compare the flexural strength of zirconia after different grinding procedures. Twenty bar-type zirconia specimens (21 x 5 x 2 mm) were divided into 4 groups and ground using a high-speed handpiece or a low-speed straight handpiece until the bars were reduced 1 mm using two different grinding times: continuous grinding and short-time grinding (n=5). Control specimens (n=5) were analyzed without grinding. The flexural strengths of the bars were determined by using 3-point bending test in a universal testing machine at a crosshead speed of 0.5 mm/min. The fracture load (N) was recorded, and the data were analyzed statistically by the Kruskal Wallis test at a significance level of 0.05. In the test groups, high-speed handpiece grinding for a short time had produced the highest mean flexural strength (878.5 ± 194.8 MPa), while micromotor continuous grinding produced the lowest mean flexural strength (733.8 ± 94.2 MPa). The control group was the strongest group (928.4 ± 186.5 MPa). However, there was no statistically significant differences among the groups (p>0.05). Within the limitations of the study, there was no difference in flexural strength of zirconia specimens ground with different procedures.     

Transformation-toughened zirconia for dental inlays, crowns and bridges: chemical stability and effect of low-temperature aging on flexural strength and surface structure.

OBJECTIVES: One concern, for transformation-toughened zirconia (Y-TZP) is their liability to low-temperature aging with accompanying alterations of properties such as strength. The loss in strength is attributed to the transformation of tetragonal grains to monoclinic. The transformation is related to loading of the dental inlays, crowns and bridges (reconstructions), temperature and time of exposure to surrounding media (aging) and the manufacturing process of Y-TZP. The purpose of this study was to determine chemical stability and effect of aging (4% acetic acid at 80 degrees C for 168 h) on flexural strength, surface and crystalline structures of two shades, P0 and P17, of a Y-TZP ceramic used for dental reconstructions. The hypotheses to be tested were that both shades of the dental Y-TZP ceramic have high flexural strength and chemical stability compared to other dental ceramics, and that the strength, surface and crystal structures of the ceramic were not affected by aging. METHODS: Forty specimens of Y-TZP, 20 of the shade P0 and 20 of the shade P17 were ground and polished. Ten specimens of each shade were exposed to low-temperature aging. The flexural strength of all 40 specimens was registered. Surfaces of the specimens were evaluated by using scanning electron microscopy (SEM), X-ray diffractometry and roughness recorder. The chemical solubility in 4% acetic acid was recorded by weight loss, and SEM was used to evaluate the surfaces of Y-TZP and dental feldspathic porcelain samples immersed in 8% SnF. Wilcoxon Signed Rank test was used for statistical analysis. RESULTS: As expected, the two shades, P0 and P17, of the studied dental Y-TZP had high strengths that were not affected by aging, and high chemical stability in the tested solutions. Contrary to what was assumed the crystal and surface structures of P0 and P17 were affected. Transformation from tetragonal to monoclinic structures occurred and small elevations on the ceramic surfaces were observed after aging. SIGNIFICANCE: The transformed-toughened Y-TZP ceramic used for dental inlays, crowns and bridges has high flexural strength compared to other dental ceramics and is chemically stable. The chemical solubility is well below the limit values of ISO 6872:1995 for dental ceramics.     

The biaxial flexural strength and fatigue property of Lava Y-TZP dental ceramic.

OBJECTIVES: The development of yttrium oxide partially stabilized zirconia (Y-TZP) has allowed the use of ceramic in load-bearing sites. The aim of this study was to evaluate and compare the biaxial flexural strength, hardness and fatigue life of colored and uncolored zirconia in the LAVAtrade mark system. MATERIALS AND METHODS: Eight groups (n=30) of standardized disc specimens (15mmx1.3mm) were used to examine the biaxial flexural strength (ISO 6872 standard) using a Dartec HC10 Fatigue Tester (Zwick Ltd., UK) and Vickers hardness was also measured. The uncolored, FS4, FS7 groups were also submitted to dynamic fatigue testing to produce stress-number curves. The strength reliability was analyzed using Weibull distribution. RESULTS: All groups had a mean biaxial flexural strength, hardness and Weibull modulus (m) of approximately 1100MPa, 1300HV and 9.8-12.9, respectively. One-way analysis of variance (ANOVA) showed no significant difference in biaxial flexural strength among the eight groups (p>0.05). Two-way ANOVA showed no significant differences in hardness values among groups except FS1 and FS5 which had significantly higher hardness values than FS4 and FS7 (p<0.001) and FS5 also had a higher hardness value than FS3 (p<0.05). Additionally, uncolored, FS4 and FS7 survived at 5x10(5) cycles at a stress level in the range of 60-65% of the mean biaxial flexural strength. CONCLUSION: There was no difference in flexural strength of uncolored and colored Y-TZP ceramic. The fatigue limit of uncolored, FS4 and FS7 zirconia may be defined as lying between 60 and 65% of the stress to failure.     

Effect of amount of grinding on flexural strength of dental ceramics

The aim of this study was to determine a suitable amount of grinding of a flexural test specimen for clinical evaluation of dental ceramics. Three dental ceramics (Crys-Cera, OCC and IPS Empress Cosmo) were selected. Five types of bar-shaped patterns were prepared for a three-point bending test, and four types of disk-shaped patterns for a biaxial flexural test. Ceramic specimens were fabricated using these patterns in accordance with the manufacturers' instructions. All specimens were ground with diamond polishing pads to yield either bar or disk specimens with the same final geometry. The surface roughness and X-ray diffraction (XRD) patterns of the specimens were examined. The flexural strength values of Crys-Cera and Empress decreased with increasing amounts of grinding, while that of OCC increased with increased grinding. The surfaces of all specimens were smoother when the amount of grinding was deeper. The XRD patterns of Crys-Cera and Empress changed with increased grinding; however, that of OCC did not change regardless of the extent of grinding. The flexural strengths of three dental ceramics differed with the amount of grinding probably because of changes of surface roughness and crystalline component composition. Unground specimens provided important insight into clinical failure modes.     

Effect of test method on flexural strength of recent dental ceramics

The purpose of the present study was to evaluate the relationships among three flexural strengths of recent dental ceramics using 3-point and 4-point bending tests and biaxial flexural test. Three brands of porcelain for veneering (d.SIGN, Supper porcelain AAA, Vintage Hallo), two injectable ceramics (Empress 2, OPC 3G), and one castable ceramic (Crys-Cera) were used. Twenty bar-shaped and 10 disc-shaped specimens of each ceramic type were prepared according to manufacturers' instructions, polished, and subjected to 3-point and 4-point bending tests and biaxial flexural test, respectively. Three flexural strengths for each ceramics were compared using one-way analysis of variance and Tukey comparison, and also investigated by Weibull analysis. The biaxial flexural strength and 3-point bending strength of all ceramics, except OPC 3G and Crys-Cera, were significantly greater than the corresponding 4-point bending strength. As for OPC 3G and Crys-Cera, their biaxial flexural strengths were significantly greater than their 3-point bending strengths, which is contrary to the other ceramics. The Weibull moduli ranged from 6.6 to 20.8. The Weibull moduli of examined ceramics, except Crys-cera, were statistically insignificant regardless of test methods.     

Effects of aging procedures on the topographic surface,structural stability,and mechanical strength of a ZrO2-based dental ceramic

ObjectiveTo determine the effects of different aging methods on the degradation and flexural strength of yttria-stabilized tetragonal zirconia (Y-TZP)MethodsSixty disc-shaped specimens (∅, 12 mm; thickness, 1.6 mm) of zirconia (Vita InCeram 2000 YZ Cubes, VITA Zahnfabrik) were prepared (ISO 6872) and randomly divided into five groups, according to the aging procedures (n = 10): (C) control; (M) mechanical cycling (15,000,000 cycles/3.8 Hz/200 N); (T) thermal cycling (6,000 cycles/5–55 °C/30 s); (TM) thermomechanical cycling (1,200,000 cycles/3.8 Hz/200 N with temperature range from 5 °C to 55 °C for 60 s each); (AUT) 12 h in autoclave at 134 °C/2 bars; and (STO) storage in distilled water (37 °C/400 days). After the aging procedures, the monoclinic phase percentages were evaluated by X-ray diffraction (XRD), and topographic surface analysis was performed by 3D profilometry. The specimens were then subjected to biaxial flexure testing (1 mm/min, load 100 kgf, in water). The biaxial flexural strength data (MPa) were analyzed by 1-way ANOVA and Tukey's test (α = 0.05). The data for monoclinic phase percentage and profilometry (Ra) were analyzed by Kruskal–Wallis and Dunn's tests.ResultsANOVA revealed that flexural strength was affected by the aging procedures (p = 0.002). The M (781.6 MPa) and TM (771.3 MPa) groups presented lower values of flexural strength than did C (955 MPa), AUT (955.8 MPa), T (960.8 MPa) and STO (910.4 MPa). The monoclinic phase percentage was significantly higher only for STO (12.22%) and AUT (29.97%) when compared with that of the control group (Kruskal–Wallis test, p = 0.004). In addition, the surface roughnesses were similar among the groups (p = 0.165).SignificanceWater storage for 400 days and autoclave aging procedures induced higher phase transformation from tetragonal to monoclinic; however, they did not affect the flexural strength of Y-TZP ceramic, which decreased only after mechanical and thermomechanical cycling.     

牙科陶瓷材料弯曲强度可靠性和亚临界裂纹扩展研究

目的:研究口腔临床修复中常用的玻璃渗透氧化铝陶瓷(in-ceram alumina,IA)弯曲强度可靠性和循环载荷下亚临界裂纹扩展(SCG)情况。方法:采用Weibull法分析由三点弯曲强度测量方法获得15个IA样本的弯曲强度数据和由循环疲劳测试获得的15个IA样本循环疲劳断裂次数数据;通过帕里斯定律(Paris law)分析IA试件在循环载荷下的亚临界裂纹扩展情况,SCG行为通过裂纹扩展速度和最大应力强度因子(Kimax)的函数关系来描述。结果:通过Weibull法得到IA试件的Weibull模数为7.9,破坏概率为1%、5%、63.21%时弯曲强度分别为246.8、303.4、438.3 MPa。IA在循环载荷下发生亚临界裂纹扩展后导致材料断裂,在应力强度因子KI为临界应力因子KIC的55%时发生裂纹传播。结论:牙科玻璃渗透氧化铝陶瓷循环载荷下存在亚临界裂纹扩展;采用三点弯曲强度测试并结合使用Weibull分析方法能加深对牙科陶瓷弯曲强度可靠性的理解。     

暂时冠桥材料挠曲强度的体外研究

目的体外对比2种甲基丙烯酸酯类和3种bis-acryl类暂时冠桥材料的挠曲强度.方法依据ISO40492000标准,制作25mm×2 mm×2 mm条状试样,人工唾液中37℃保存24 h后,在万能力学实验机上三点加荷测定试样挠曲强度.结果5种材料挠曲强度值排序QuickResin＜Protemp Ⅱ＜Curefast＜Luxatemp＜Protemp 3 Garant.QuickResin、Protemp Ⅱ和Curefast之间没有统计学差异(P＞0.05).Protemp 3 Garant挠曲强度值高于Luxatemp(P＜0.05),他们均高于前三者(P＜0.05).结论bis-acryl类材料较甲基丙烯酸酯类材料强度好,但是早期bis-acryl类材料强度一般.临床医生应根据不同的病人选用合适的暂时冠桥材料.     

Wear evaluation of the human enamel opposing different Y-TZP dental ceramics and other porcelains

PurposeThis study examined the wear resistance of human enamel and feldspathic porcelain after simulated mastication against 3 zirconia ceramics, heat-pressed ceramic and conventional feldspathic porcelain.Materials and methodsHuman teeth and feldspathic porcelain cusp were tested against ceramic discs. 5 brands were tested – 3 monolithic zirconia, Prettau, Lava, and Rainbow, one lithium disilicate, IPS e.max Press, and one feldspathic porcelain, Vita-Omega 900. The surface was polished using a 600 grit and 1200 grit SiC paper. Each group was loaded for 300,000 cycles in a chewing simulator. The wear resistance was analyzed by measuring the volume of substance lost. The wear surfaces were observed by scanning electron microscopy to determine the wear characteristics.ResultsVita-Omega 900 led to the greatest amount of enamel wears followed by IPS e.max Press, Prettau, Lava and Rainbow. There was a significant difference between Vita-Omega 900 and IPS e.max Press (p < 0.05). The wear values for human enamel were significantly greater than those for feldspathic porcelain, regardless of the surface roughness of the ceramic specimens (p < 0.05).ConclusionThe wear behaviour of human enamel and feldspathic porcelain varies according to the type of substrate materials. On the other hand, 3 zirconia ceramics caused less wear in the abrader than the conventional ceramic.Clinical significanceDental professionals should be aware of the wear effect of dental restorations on the opposing teeth or restorations. The amount of enamel wear was highest in feldspathic porcelains whereas zirconia ceramics caused less wear on the opposing teeth.     

The effect of low temperature aging on the mechanical property & phase stability of Y-TZP ceramics

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 Säckingen, Germany) were prepared in 40 mm (length) × 4 mm (width) × 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℃ 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 (α= .05).

RESULTS

The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below 125℃ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above 150℃, 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℃. 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℃. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.     

多次热处理对Empress 2热压铸玻璃陶瓷强度及色泽的影响

目的 比较多次热处理对 Empress 2热压铸玻璃陶瓷材料的色泽及抗弯强度的影响和对支架瓷-饰瓷复合体的色泽的影响。方法 本实验有3个大试样组:A组试样为15个由支架瓷原料热压铸而成的直径9mm,厚(0.80±0.01)mm的碟形试样,每3个试样为一处理组;B组试样先依照A组试样的方法制作,再在其一个面上烧结饰瓷层使总厚度为(1.50±0.01)mm,共12个,每3个试样为一处理组;C组试样为20个由Empress 2支架瓷原料热压铸而成的规格为 2.0mm×3.0mm×25mm的试样,每 5个试样为一处理组。上述每个处理组都经过了不同次数的热处理后,A、B两组所有试样的色泽参数(L、a、b)由 ShadeEye NCC牙科色度仪测得;C组试样的三点抗弯强度都由MTS Synergie综合测试仪以及Testwork4软件测出。最后用单因素方差分析和t检验来比较各处理组间数据的差异(P<0.05)。结果A,B两组中各处理组间的色泽参数无显著差异;C组中各处理组间的抗弯强度也无显著差异。结论 一定次数的热处理不会对 Empress 2牙科陶瓷的色泽及抗弯强度产生影响。没有证据表明需要对 Empress 2热压铸玻璃陶瓷饰瓷烧结以及上釉等热处理工序的次数进行过于严格的限制。