白榴石微晶化增强牙科玻璃陶瓷的热处理温度制度的研究

目的 探索白榴石微晶化的热处理温度制度。方法 根据白榴石的化学式和K20-Na2O-Al2O3-SiO2系统相图制定原材料配比，在预设的熔融、成核、析晶温度中选择最佳温度；利用偏振光显微镜和x射线衍射分析仪观察样品的形态及显微结构特性。结果 玻璃融熔温度为1600℃，成核温度为1200℃，晶化温度为1500℃；微晶化后的自榴石晶粒约0．8μm，在玻璃基质中分布均匀。结论 按照一定的热处理温度制度。白榴石可以在玻璃中微晶化。     

白榴石对牙科玻璃陶瓷强度的影响

利用内部增强剂是目前提高牙科陶瓷强度的主要方法之一［１］。由列支敦士登Ｉｖｏｃｌａｒ公司推出的ＩＰＳ—Ｅｍｐｒｅｓ铸造陶瓷系统和美国产品ＯｐｅｃｔＨＳＰ等均是以白榴石（Ｌｅｕｃｉｔｅ）为内部增强剂的牙科陶瓷［２、３］。本文就白榴石与牙科玻璃陶瓷强度的...     

牙科陶瓷循环和静态疲劳的对比实验

目的 比较牙科陶瓷循环和静态加载后的强度下降规律以及结构损伤差异。方法应用赫兹触压实验方法对可切削陶瓷标准试件（VitamarkⅡ）进行循环和静态加载，测试试件的残余三点挠曲强度，观测试件表面及表面下损伤，数据进行单因素方差分析。结果试件在两种加载模式下，首次加载后残余强度均降低，同时出现外锥型损伤。循环加载至1000次时，内锥型损伤出现并伴随强度进一步降低，差异有统计学意义（P〈0．05）。不同加载时间下的静态加载试件强度下降的差异无统计学意义，同时不伴随内锥状裂纹的产生。结论静态加载和循环加载都能降低陶瓷试件的强度，但循环加载使损伤更严重。     

白榴石含量对K2O-Al2O3-SiO2系统牙科玻璃陶瓷的断裂韧性影响的实验研究

目的：确定白榴石含量与K2O-Al2O3-SiO2系统牙科玻璃陶瓷材料断裂韧性的关系,探讨白榴石含量影响K2O-Al2O3-SiO2系统牙科玻璃陶瓷断裂韧性的机理。方法：选择5组相同组分、不同比例的玻璃陶瓷原材料,经＂白榴石微晶化＂热处理工艺加工,制成含有不同白榴石含量的K2O-Al2O3-SiO2系统牙科玻璃陶瓷试件;用单边切口弯曲梁法测试样品的断裂韧性,计算断裂韧性值;分析样品的显微结构和测定白榴石含量;对5组样品的白榴石含量和断裂韧性值数据进行相关回归统计学分析。结果：白榴石晶粒约1.0μm、在玻璃基质中分布均匀;K2O-Al2O3-SiO2系统牙科玻璃陶瓷的断裂韧性与白榴石含量有相关关系。结论：白榴石含量对K2O-Al2O3-SiO2系统牙科玻璃陶瓷的断裂韧性有明显影响,在一定范围内,该陶瓷的断裂韧性随白榴石含量增高而增大。     

粘接树脂的色调对白榴石增强玻璃陶瓷色参数的影响

目的:探讨粘接树脂的色调对白榴石增强玻璃陶瓷色参数的影响.方法:制作28个直径10 mm、厚1 mm的白榴石增强玻璃陶瓷试件(IPS Empress,A2色),实验组在试件表面涂塑厚度为0.2 mm的Variolink Ⅱ树脂粘接剂,色调分别为黄、棕和白,各7个;未涂塑树脂粘接剂者为对照组.用PR-650分光光度仪测量各组试件的颜色参数并计算组间色差,对测量的数据进行统计学分析.结果:粘接树脂的色调对IPS Empress铸瓷试件的色参数有显著影响(P＜0.05),实验组较对照组的L*值降低, a*、b*值增高;实验组与对照组间及各实验组间的色差有统计学意义(P＜0.05).结论:粘接树脂的色调对白榴石增强玻璃陶瓷色参数有显著影响,临床上粘接白榴石增强玻璃陶瓷修复体时应考虑这一影响.     

牙科可切削云母微晶玻璃呈色的研究

目的 研制用于牙科计算机辅助设计与辅助制作磨牙冠、可提供多种颜色选择的可切削四硅酸氟云母微晶玻璃。方法 采用正交设计技术，对影响微晶玻璃颜色的基础配方、色料组成及热处理制度进行筛选。结果 从基础配方中选择出影响呈色的2个主要因素：晶核剂F含量、Mg^2 ／K^ 比例；从多种色料中选择出主要色料CeO2；从热处理制度中选择出成核制度：650℃保持1h和晶化制度：1000℃或1050℃保持3h～4h,，结论 所研制的云母微晶玻璃，可提供4～5种牙科颜色，其切削性能良好，完全可以满足计算机辅助设计．辅助制作(CAD／CAM)系统的要求。     

牙科用可切削云母基玻璃陶瓷析晶行为研究

目的:采用阶梯烧结法制备K2O-MgO-Al2O3-SiO2-F系列玻璃陶瓷,分析不同热处理工艺对所制玻璃陶瓷性能的影响。方法:通过X射线衍射(XRD)、扫描电子显微镜(SEM)、背散射(BSE)及抗弯强度测试,研究氟硅云母玻璃陶瓷的析晶行为特点。结果:680℃核化1 h后,若在1 000~1 120℃之间晶化,则析出主晶相为四氟硅云母,晶体形状由颗粒状逐渐变成立方状或扁平状。陶瓷在大于1 160℃晶化出现晶体熔化。结论:680℃核化1 h后,1 040℃析出的云母晶体符合材料的微观要求,过高的温度不利于云母晶体的析出;二次融入3%的四方氧化锆多晶体(Y-TZP)完全熔解于K2O-MgO-Al2O3-SiO2-F玻璃系统中。     

牙科纳米氧化铝陶瓷的烧结研究

目的：探讨干压成型、低温烧结制备牙科纳米氧化铝陶瓷的工艺方法。方法：采用Al2O3-CaO-MgO-SiO2系统来研制纳米氧化铝陶瓷,通过扫描电子显微镜（SEM）及力学性能测试,比较了不同MgO含量、成型压力及烧结温度对氧化铝陶瓷的密度及力学性能的影响。结果：1．29wt% MgO试样组的陶瓷晶粒均匀且发育比较完全;随着粉料成型压力的升高,烧结后瓷体的密度及维氏硬度均增大;在1300℃烧结后,晶体发育差且气孔较多,随着烧结温度的升高,晶粒逐渐增大,在1450℃时可见瓷体晶形发育较完全。结论：选择适当的复合烧结助剂、成型压力及烧结温度可制得较理想的纳米氧化铝陶瓷。     

K2O-Na2O-Al2O3-SiO2系统牙科微晶玻璃匹配氧化铝陶瓷的初步研究

目的:研究 K₂O-Na₂O-Al₂O₃-SiO₂系统牙科微晶玻璃匹配氧化铝陶瓷的热处理温度制度。方法:根据氧化铝陶瓷的热膨胀系数调整K₂O-Na₂O-Al₂O₃-SiO₂系统牙科微晶玻璃的原材料配比,利用K₂O-Na₂O-Al₂O₃-SiO₂系统牙科微晶玻璃的热处理温度制度形成微晶玻璃-氧化铝陶瓷复合材料;利用偏振光显微镜和X射线衍射分析仪观察样品的形态及显微结构特性,利用材料试验机测试材料的抗压强度。结果:经过原材料组份的调整,白榴石晶粒约1.0 μm、在玻璃基质中分布均匀;微晶玻璃-氧化铝陶瓷复合材料的抗压强度为500 MPa。结论:K₂O-Na₂O-Al₂O₃-SiO₂系统牙科微晶玻璃的热处理温度制度适合匹配氧化铝陶瓷。     

超韧牙科氟金云母玻璃陶瓷的可加工性能初探

目的 分析不同晶化温度和晶化时间对一种氟金云母玻璃陶瓷加工性能的影响,探讨其延性切削行为的机制.方法 使用SiO2-B2O3-R:O-Al2O3-ZnO-MgO-F(R为碱金属)玻璃陶瓷粉制备晶化温度和晶化时间分别为650 ℃(60 min)、680 ℃(60 min)、710 ℃(60 min)、740 ℃(60 min)、680 ℃(30 min)、680 ℃(120 min)、680 ℃(240 min)的试件,分为A、B、C、D、E、F、G组,每组6个;长石质可切削陶瓷试件作为对照组.测定8组试件钻孔30 s后的钻孔深度,并进行车床切削实验定性分析.扫描电镜和X射线衍射分析观察试件的微观结构.结果 A组钻孔深度最大,为(7.1±0.8)mm;D组最小,为(0.5±0.1)mm.除D组外,其余组钻孔深度均大于对照组[(0.8±0.1)mm],差异均有统计学意义(P＜0.05).A组试件可在普通车床高速车削条件下形成连续带状切屑,其晶体相含量约为40%.结论 这种云母玻璃陶瓷具有良好的可加工性,其机制可能与云母晶体的互锁结构和玻璃相黏滞流动作用相关.     

Water-enhanced crystallization of leucite in dental porcelain

OBJECTIVE: The purpose of this study was to determine whether long-term exposure of dental porcelain to saliva during temporary cementation of a porcelain-fused-to-metal (PFM) restoration could enhance leucite crystallization if the restoration is refired. Such water-enhanced leucite crystallization in dental porcelains could lead to porcelain-metal thermal incompatibility problems. METHODS: Six commercial dental body porcelains and the Component No. 1 (leucite-containing) frit of the Weinstein et al. [13] patent were studied. For each porcelain, 30 coupon specimens were randomly assigned to a treatment group. Ten specimens were placed in artificial saliva, 10 in distilled water, and 10 in a desiccator and were stored for six months. At the end of the six months, an additional 10 coupons of each porcelain were prepared to serve as a control. All 40 specimens of each porcelain were randomized and subjected to one additional firing. Leucite weight fraction was determined by quantitative X-ray powder diffraction analysis via an internal standard technique. RESULTS: Comparisons among the treatments via the least-squares-means test-adjusting for porcelain showed that the saliva group mean leucite weight fraction was significantly higher than that of the other groups. The change in porcelain thermal expansion that would be associated with a leucite change in this range would be between 0.2 x 10(-6) K-1 and 0.3 x 10(-6) K-1. SIGNIFICANCE: The results of this work constitute the first demonstration that moisture absorbed by a porcelain can act as a glass modifier and enhance the crystallization of the glass during subsequent firing. The effect was sufficiently large to generate thermal expansion changes that would exceed the maximum safe mismatch between porcelain and metal.     

Effect of different veneering techniques on the fracture strength of metal and zirconia frameworks

PURPOSE

To determine whether the fracture strengths and failure types differed between metal and zirconia frameworks veneered with pressable or layering ceramics.

MATERIALS AND METHODS

A phantom molar tooth was prepared and duplicated in 40 cobalt-chromium abutments. Twenty metal (IPS d.SIGN 15, Ivoclar, Vivadent, Schaan, Liechtenstein) and 20 zirconia (IPS e.max ZirCAD, Ivoclar) frameworks were fabricated on the abutments. Each framework group was randomly divided into 2 subgroups according to the veneering material: pressable and layering ceramics (n=10). Forty molar crowns were fabricated, cemented onto the corresponding abutments and then thermocycled (5-55℃, 10,000 cycles). A load was applied in a universal testing machine until a fracture occurred on the crowns. In addition, failure types were examined using a stereomicroscope. Fracture load data were analyzed using one-way ANOVA and Tukey HSD post-hoc tests at a significance level of 0.05.

RESULTS

The highest strength value was seen in metal-pressable (MP) group, whereas zirconia-pressable (ZP) group exhibited the lowest one. Moreover, group MP showed significantly higher fracture loads than group ZP (P=.015) and zirconia-layering (ZL) (P=.038) group. No significant difference in fracture strength was detected between groups MP and ML, and groups ZP and ZL (P>.05). Predominant fracture types were cohesive for metal groups and adhesive for zirconia groups.

CONCLUSION

Fracture strength of a restoration with a metal or a zirconia framework was independent of the veneering techniques. However, the pressing technique over metal frameworks resisted significantly higher fracture loads than zirconia frameworks.     

The effect of core material, veneering porcelain, and fabrication technique on the biaxial flexural strength and weibull analysis of selected dental ceramics

Purpose: The objective of this study was to compare the effect of veneering porcelain (monolithic or bilayer specimens) and core fabrication technique (heat‐pressed or CAD/CAM) on the biaxial flexural strength and Weibull modulus of leucite‐reinforced and lithium‐disilicate glass ceramics. In addition, the effect of veneering technique (heat‐pressed or powder/liquid layering) for zirconia ceramics on the biaxial flexural strength and Weibull modulus was studied. Materials and Methods: Five ceramic core materials (IPS Empress Esthetic, IPS Empress CAD, IPS e.max Press, IPS e.max CAD, IPS e.max ZirCAD) and three corresponding veneering porcelains (IPS Empress Esthetic Veneer, IPS e.max Ceram, IPS e.max ZirPress) were selected for this study. Each core material group contained three subgroups based on the core material thickness and the presence of corresponding veneering porcelain as follows: 1.5 mm core material only (subgroup 1.5C), 0.8 mm core material only (subgroup 0.8C), and 1.5 mm core/veneer group: 0.8 mm core with 0.7 mm corresponding veneering porcelain with a powder/liquid layering technique (subgroup 0.8C‐0.7VL). The ZirCAD group had one additional 1.5 mm core/veneer subgroup with 0.7 mm heat‐pressed veneering porcelain (subgroup 0.8C‐0.7VP). The biaxial flexural strengths were compared for each subgroup (n = 10) according to ISO standard 6872:2008 with ANOVA and Tukey's post hoc multiple comparison test (p≤ 0.05). The reliability of strength was analyzed with the Weibull distribution. Results: For all core materials, the 1.5 mm core/veneer subgroups (0.8C‐0.7VL, 0.8C‐0.7VP) had significantly lower mean biaxial flexural strengths (p < 0.0001) than the other two subgroups (subgroups 1.5C and 0.8C). For the ZirCAD group, the 0.8C‐0.7VL subgroup had significantly lower flexural strength (p= 0.004) than subgroup 0.8C‐0.7VP. Nonetheless, both veneered ZirCAD groups showed greater flexural strength than the monolithic Empress and e.max groups, regardless of core thickness and fabrication techniques. Comparing fabrication techniques, Empress Esthetic/CAD, e.max Press/CAD had similar biaxial flexural strength (p= 0.28 for Empress pair; p= 0.87 for e.max pair); however, e.max CAD/Press groups had significantly higher flexural strength (p < 0.0001) than Empress Esthetic/CAD groups. Monolithic core specimens presented with higher Weibull modulus with all selected core materials. For the ZirCAD group, although the bilayer 0.8C‐0.7VL subgroup exhibited significantly lower flexural strength, it had highest Weibull modulus than the 0.8C‐0.7VP subgroup. Conclusions: The present study suggests that veneering porcelain onto a ceramic core material diminishes the flexural strength and the reliability of the bilayer specimens. Leucite‐reinforced glass‐ceramic cores have lower flexural strength than lithium‐disilicate ones, while fabrication techniques (heat‐pressed or CAD/CAM) and specimen thicknesses do not affect the flexural strength of all glass ceramics. Compared with the heat‐pressed veneering technique, the powder/liquid veneering technique exhibited lower flexural strength but increased reliability with a higher Weibull modulus for zirconia bilayer specimens. Zirconia‐veneered ceramics exhibited greater flexural strength than monolithic leucite‐reinforced and lithium‐disilicate ceramics regardless of zirconia veneering techniques (heat‐pressed or powder/liquid technique).     

Luting glass ceramic restorations using a selfadhesive resin cement under different dentin conditions

Objectives

The aim of this study was to investigate the bond strength of ceramic restorations luted using a self-adhesive resin cement (RelyX Unicem, 3M ESPE) under different dentin conditions.

Material and Methods

In the experimental groups, ceramic restorations were luted to bovine incisors with RelyX Unicem under the following conditions: [Dry dentin]: surface was dried using air stream for 15 s; [Moist dentin]: excess dentin moisture was removed with absorbent paper; [Bonding agent]: Clearfil SE Bond (Kuraray) self-etching adhesive system was previously applied to dentin. In the Control group, cementation was done using an etch-and-rinse adhesive (Excite DSC) and Variolink II resin cement (Ivoclar Vivadent). Photoactivation of the resin cements was performed with UltraLume LED 5 unit (Ultradent). The restorations (n=5 per group) were sectioned into beams and microtensile testing was carried out. Data were subjected to ANOVA and Tukey''s test (p<0.05). Failure modes were classified under Scanning Electron Microscopic (SEM) (×120 magnification).

Results

The bond strength was dependent on the moisture status of the dentin. Bond strength in the "dry dentin group" was significantly lower than that of all other groups, which showed similar results. A predominance of mixed failures was detected for the control group, while a predominance of adhesive failures was observed for the "bonding agent" and "dry dentin" groups. The "moist dentin" group presented predominantly cohesive failures within the luting material. The previous application of a self-etching adhesive showed no significant effect.

Conclusions

Only excess dentin moisture should be removed for the cementation of ceramic restorations with self-adhesive resin cements.     

牙科纳米氧化锆陶瓷粉体的制备

目的 :探讨用于增韧牙科氧化铝陶瓷的纳米氧化锆陶瓷粉体的制备方法。方法 :应用沉淀法 ,比较不同前驱物浓度和 pH值等条件下 ,所制备氧化锆粉体的物理性能。 结果 :ZrOCl2 ·8H2 O浓度为 0 .3～ 0 .5mol/L、pH 8.5时 ,经 70 0℃煅烧 2h后 ,可获得性能优良、粒径约为 10 0nm的氧化锆陶瓷粉体。 结论 :选择适当的条件 ,该方法可制得粒径小、团聚少的纳米氧化锆陶瓷粉体。     

GI—Ⅱ型牙用玻璃渗透氧化铝陶瓷的生物安全性评价

目的：研究评价GI－Ⅱ型牙用玻璃渗透氧化铝陶瓷材料的生物安全性。方法：利用仓鼠,NIH纯系小鼠,豚鼠等实验动物对材料进行急性毒性,细胞毒性,致敏性,口腔粘膜刺激性,溶血,微核等试验研究,结果：材料的溶血率低于5％,有良好的血液相容性,无明显的细胞毒性作用,未见任何急性毒性反应,对口腔粘膜无刺激性,无致敏性,微核试验未见潜在致突变性。结论：GI－II型牙用玻璃渗透氧化铝陶瓷材料的临床应用具有可靠的生物安全性。     

Transient and residual stresses induced during the sintering of two dentin ceramics

Objectives

To characterize the stress induced deformation of bi-axial flexure strength (BFS) test specimens during processing to provide an insight into sintering effects and associated BFS determination.

Methods

40 Vitadur-Alpha and 80 IPS e.max Ceram disc-shaped specimens were condensed and a sintered on a silicon nitride refractory tray under controlled firing and cooling parameters. The mean of the maximum deflection (μm) and Ra values (μm) were determined using a high resolution profilometer and were related to the orientation of the measured surface within the furnace. BFS testing of the subsequent groups (n = 20) was performed and the data related to the measured deformation of the sintered specimens. A two-way analysis of variance (ANOVA) where factors were identified as surface state and firing orientation with post hoc Tukey's tests was complemented by pair-wise comparisons with a Student's t-test for each measurement (P < 0.05).

Results

The mean of the maximum deflection values and the mean BFS for Vitadur Alpha discs were not significantly influenced by firing orientation (P = 0.248 and P = 0.284, respectively). However, the Ra values were significantly different (P < 0.001). The two-way ANOVA revealed a significant impact on the mean of the maximum deflection measurements for surface state (P < 0.001) and firing orientation (P < 0.001) during sintering (P < 0.001). The mean Ra values were not significantly influenced. The BFS of sintered IPS e.max Ceram discs was sensitive to firing orientation (P < 0.001).

Significance

Conventional glass theory explains that residual thermal stress gradients induced during sintering can cause test specimen deformation which can alter the expected BFS data. The study demonstrates that variability such as firing orientation during sintering which is very rarely reported in the literature can have a significant impact on the reported BFS data and can confound its interpretation.     

Zirconia toughened mica glass ceramics for dental restorations

Objective

The objective of the present study is to understand the role of yttria stabilized zirconia (YSZ) in achieving the desired spectrum of clinically relevant mechanical properties (hardness, elastic modulus, fracture toughness and brittleness index) and chemical solubility of mica glass ceramics.