通用型粘接剂和树脂水门汀对氧化锆 剪切粘接强度的影响

目的 研究通用型粘接剂和树脂水门汀对氧化锆陶瓷剪切粘接强度和耐久性的影响。方法 氧化锆陶瓷烧结制作20 mm×10 mm×10 mm和10 mm×10 mm×10mm两种尺寸的试件,实验分为12组,将这2种试件分别采用不同的树脂水门汀（RelyX Ultimate树脂水门汀、Clearfil SAC自粘接树脂水门汀）和通用粘接剂（无粘接剂、Scotchbond通用粘接剂、Clearfil SE One粘接剂）在不同的储存条件（水浴、水浴+冷热循环）下进行粘接。测试剪切粘接强度,分析断裂形态。结果 水门汀（F=8.41,P<0.01）和粘接剂（F=30.34,P<0.01）对氧化锆剪切粘接强度的影响有统计学意义;储存条件对剪切粘接强度的影响无统计学意义（F=1.83,P=0.18）。RelyX Ultimate树脂水门汀、无粘接剂、水浴+冷热循环储存时的剪切粘接强度最低（14.02 MPa±6.86 MPa）,RelyX Ultimate树脂水门汀、Scotchbond通用粘接剂、水浴+冷热循环储存时的剪切粘接强度最高（54.12 MPa±8.37 MPa）。结论 通用型粘接剂可提高树脂水门汀对氧化锆的粘接耐久性。非自粘接的树脂水门汀如不使用通用型粘接剂则其粘接耐久性下降。     

通用型粘接剂和树脂水门汀对氧化锆剪切粘接强度的影响

目的 研究通用型粘接剂和树脂水门汀对氧化锆陶瓷剪切粘接强度和耐久性的影响。方法 氧化锆陶瓷烧结制作20 mm×10 mm×10 mm和10 mm×10 mm×10mm两种尺寸的试件,实验分为12组,将这2种试件分别采用不同的树脂水门汀（RelyX Ultimate树脂水门汀、Clearfil SAC自粘接树脂水门汀）和通用粘接剂（无粘接剂、Scotchbond通用粘接剂、Clearfil SE One粘接剂）在不同的储存条件（水浴、水浴+冷热循环）下进行粘接。测试剪切粘接强度,分析断裂形态。结果 水门汀（F=8.41,P<0.01）和粘接剂（F=30.34,P<0.01）对氧化锆剪切粘接强度的影响有统计学意义;储存条件对剪切粘接强度的影响无统计学意义（F=1.83,P=0.18）。RelyX Ultimate树脂水门汀、无粘接剂、水浴+冷热循环储存时的剪切粘接强度最低（14.02 MPa±6.86 MPa）,RelyX Ultimate树脂水门汀、Scotchbond通用粘接剂、水浴+冷热循环储存时的剪切粘接强度最高（54.12 MPa±8.37 MPa）。结论 通用型粘接剂可提高树脂水门汀对氧化锆的粘接耐久性。非自粘接的树脂水门汀如不使用通用型粘接剂则其粘接耐久性下降。     

Effect of silane and MDP-based primers on physico-chemical properties of zirconia and its bond strength to resin cement

ObjectiveTo evaluate the effect of surface treatments on yttria-tetragonal zirconia polycrystal (Y-TZP) characteristics and on resin-mediated zirconia bond.MethodsY-TZP slabs were grit blasted with 45 μm alumina or with 30 μm silica-coated alumina particles. The chemical treatments were: no-chemical treatment (NC), silane-containing primer (SP), MDP (10-Methacryloyloxydecyl dihydrogen phosphate) and silane-containing primer (MPS), MDP-containing primer (MP) and MDP and silane-containing adhesive (MPA). Contact angle as a function of surface roughness (θ_m) and surface roughness parameter (Sdr) were measured using Fringe Projection Phase Shifting (FPPS). Surface free energy (γ_s^TOT) was calculated with a goniometer. Chemical interaction between primers/adhesive and zirconia was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS). Resin cement microshear bond strength (μSBS) was analyzed at either 24-h or 8-months water storage (37 °C). θ_m values, Sdr values, γ_s^TOT and μSBS values were analyzed using Analysis of variance (ANOVA) and post hoc Tukey test (α = 0.05).ResultsChemical treatment had an effect (p < 0.001) on all surface parameters analyzed: θ_m, γ_s^TOT and Sdr. MP-treated group showed higher incidence of P–O–Zr bonds than the other groups, indicating more chemical linkages. Grit blasting (p < 0.001) and the interaction chemical treatment*storage (p < 0.001) did not affect μSBS; all silane-containing primers showed significant drop in μSBS after aging.SignificanceMDP and/or silane-based solutions affect the physicochemical properties of blasted-zirconia. An MDP-based primer is fundamental to achieve a stable resin-zirconia bonding, but the chemical reactivity of MDP is impaired when this molecule is present in a multicomponent system.     

氧化锆陶瓷与三种树脂粘接剂粘接剪切强度比较

目的探讨适合牙科氧化锆陶瓷的粘接材料。方法将烧结后的氧化锆陶瓷片分为3组,每组32片,分别采用三种自酸蚀粘接剂RelyX Unicem、PanaviaTM F、Superbond C﹠B与喷砂后的氧化锆陶瓷片粘接,水浴24h和水浴30d后,测试其粘接剪切强度。数据用SAS9.12软件进行统计学分析,粘接断面用扫描电镜观察。结果 PanaviaTMF树脂粘接材料粘接强度最好,分别为（31.36±3.49）MPa（水浴24h）、（29.52±3.44）MPa（水浴30d）。Superbond C﹠B能够取得较好的初期粘接强度（31.85±3.61）MPa（水浴24h）,但水浴30d后明显下降至（21.32±2.58）MPa,P〈0.05。RelyX Unicem的初期（水浴24h）粘接强度最小为（13.29±3.05）MPa,P〈0.0001,但水浴30d后粘接强度为（12.06±2.28）MPa,未见明显降低,P（0.05。结论含有MDP磷酸单体的树脂粘接材料可以使牙科氧化锆陶瓷获得最好的粘接效果。使用不含无机填料的化学固化型纯树脂粘接剂可以取得较好的初期粘接强度但长期效果欠佳。一步法自酸蚀树脂粘接剂虽然没有很高的初期粘接强度,但粘接效果尚能持久。     

喷砂对不同粘接剂与氧化锆粘接强度的影响

目的研究喷砂对不同粘接剂与氧化锆粘接强度的影响,筛选出比较理想的粘接剂。方法将由ZrO2制成的大瓷片（140个）和小瓷片（140个）随机配对分成14组。对ZrO2的表面分别不作处理和喷砂处理,选用临床常用的7种粘接剂,将较小瓷片粘接在较大瓷片上。置于37℃蒸馏水里保存24h后,进行剪切粘接强度测试,并进行统计学分析。结果喷砂组的粘接强度明显高于非喷砂组（P〈0.01）。PanaviaF、Super-BondC＆B与ZrO2的粘接强度明显高于BifixQM与ZrO2的粘接强度（P〈0.01）。结论喷砂能明显提高粘接剂与ZrO2的粘接强度,Panavia F、Super-Bond C＆B是比较理想的粘接剂。     

Effectiveness of pre-silanization in improving bond performance of universal adhesives or self-adhesive resin cements to silica-based ceramics: Chemical and in vitro evidences

Objectives

To examine effectiveness of pre-silanization in improving bond performance of multipurpose products such as universal adhesives or self-adhesive resin cements to silica-based ceramics.

不同粘接剂及表面处理对氧化锆的粘接强度的影响

目的:评价不同粘接剂及表面处理方法对氧化锆陶瓷与粘接剂的粘接强度的影响.方法:将较大氧化锆瓷片和较小氧化锆瓷片派对,随机分成12组,每组10对.粘接剂选用Ketac Cem Easymix、Rely X luting、Bifix QM和Panavia F,对氧化锆的表面分别喷砂、硅烷化或喷砂联合硅烷化处理,并进行剪切粘接强度测试.结果:在使用Ketac Cem Easymix和Rely X luting时,喷砂提高了粘接强度(P＜0.01).在使用Bifix QM和Panavia F时,喷砂、硅烷化或喷砂联合硅烷化处理提高了粘接强度(P＜0.01).表面处理相同时,Panavia F与氧化锆的粘接强度高于其它粘接剂(P＜0.01).结论:使用Panavia F联合喷砂加硅烷化处理的粘接强度最高.     

Effect of multi-purpose primers on the bond durability between tri-n-butylborane initiated resin and gold alloy

Purpose

This study investigated the influence of an interaction between sulfur-containing monomers and other monomers in multipurpose primers on the bond durability of a tri-n-butylborane (TBB)-initiated acrylic resin to a gold alloy.

4种黏结材料与氧化锆陶瓷黏结剪切强度的比较

目的:探讨适合牙科氧化锆陶瓷的黏结材料。方法:将烧结后的氧化锆陶瓷片分为4组,每组16片,分别采用RelyXTM ARC、PanaviaTM F、RelyXTM Luting、Fuji plus4种黏结材料与喷砂后的氧化锆陶瓷片黏结,水浴24h和水浴30d后,测试其黏结剪切强度,数据用SAS6.12软件进行统计学分析,黏结断面用扫描电镜观察。结果:PanaviaTMF树脂黏结材料黏结强度最好,分别为(34.7±3.44)MPa(水浴24h)、(31.5±3.44)MPa(水浴30d),与其他组黏结强度差别有统计学意义(P<0.01)。RelyXTM Luting,Fuji plus2种树脂改良型玻璃离子可以获得较好的初期(水浴24h)黏结强度,分别为(15.5±2.71)MPa和(16.0±1.77)MPa,但水浴30d后明显下降至(6.80±1.24)MPa和(3.38±2.32)MPa,P<0.05。结论:含有MDP磷酸单体的树脂黏结材料可以使牙科氧化锆陶瓷获得最好的黏结效果,使用树脂改良型玻璃离子可以产生较好的初期黏结强度,但黏结效果不能持久。     

不同表面处理和不同粘结剂对氧化锆粘结强度的影响

目的探讨不同表面处理和不同粘结剂对氧化锆粘结强度的影响。方法将氧化锆分别制成直径为12.0mm和4.0mm的瓷片,各120个,分别随机分成12组。粘结剂选用磷酸锌粘结剂、聚羧酸锌粘结剂、BifixQM和Super-Bond CB。对氧化锆的表面分别进行不处理、喷砂、硅烷化、先喷砂后硅烷化处理。用上述4种粘结剂将4.0mm瓷片粘结在12.0mm瓷片上,置于37℃蒸馏水中保存24h后,进行剪切粘结强度测试。结果粘结剂相同时,不同表面处理时的粘结强度有显著统计学差异(P0.01),由小到大依次为不处理喷砂硅烷化先喷砂后硅烷化处理;表面处理相同时,不同粘结剂之间的粘结强度有显著统计学差异(P0.01),由小到大依次为磷酸锌粘结剂聚羧酸锌粘结剂Bifix QMSuper-Bond CB。结论粘结剂相同时,表面处理提高了粘结强度。Super-Bond CB的粘结强度比较理想。使用Super-Bond CB时,喷砂后硅烷化处理是一种比较理想的表面处理方法。     

表面处理对粘结剂与氧化锆粘结强度的影响

目的：评价出比较理想的粘结剂和ZrO2表面处理方法。方法：将由ZrO2制成的较大瓷片（120个）和较小瓷片（120个）,随机派对分成12组。对ZrO2的表面分别不作处理、喷砂、硅烷化,先喷砂后硅烷化处理。用Bifix QM、Super-BondC＆B和Panavia F三种树脂粘结剂将较小瓷片粘结在较大瓷片上。置于37℃蒸馏水里保存24h后,进行剪切粘结强度测试。结果：3种表面处理都提高了粘结强度（P〈0．01）,其中,先喷砂后硅烷化处理对粘结强度提高得最明显（P〈0．01）。Panavia F、Super-Bond C＆B与ZrO2的粘结强度明显高于BifixQM与ZrO2的粘结强度（P〈0．01）。结论：先喷砂后硅烷化处理是一种比较理想的表面处理方法,Panavia F、Super-Bond C＆B是比较理想的树脂粘结剂。     

Evaluation of surface treatments of monolithic zirconia in different sintering stages

Purpose

This study evaluated the effect of surface treatment of zirconia in pre-sintered and post-sintered stages on its surface roughness, phase transformation, and biaxial flexural strength (BFS).

Immediate enamel bond strength of universal adhesives to unground and ground surfaces in different etching modes

The purpose of this study was to determine the immediate bond effectiveness of universal adhesives to unground and ground enamel surfaces in different etching modes, through shear bond strength (SBS) tests and scanning electron microscopy observations. Three universal adhesives, a conventional two‐step self‐etch adhesive, and a conventional single‐step self‐etch adhesive were compared. Human enamel specimens from lower anterior teeth were divided into four groups and subjected to the following treatments: (i) unground enamel in self‐etch mode; (ii) ground enamel in self‐etch mode; (iii) unground enamel in etch‐&‐rinse mode; and (iv) ground enamel in etch‐&‐rinse mode. Bonded assemblies were subjected to SBS testing. All the adhesives showed significantly higher SBS values in etch‐&‐rinse mode than in self‐etch mode, regardless of whether enamel was unground or ground. The influence of the enamel surface condition on SBS was different in different etching modes. Without pre‐etching, all tested materials showed lower SBS values in unground enamel than in ground enamel. In etch‐&‐rinse mode, no significant differences in SBS values were observed between unground enamel and ground enamel for any of the adhesives tested. Phosphoric acid pre‐etching before application of self‐etch adhesives to an unground enamel surface is essential to enhance initial enamel bond effectiveness.     

Effect of surface treatment on the micro-shear bond strength to zirconia

The constant quest for finding the ultimate esthetic dental restorative material has led to numerous alternatives. These materials, in addition to possessing optical properties simulating natural teeth, should also have physical properties that can withstand the harsh oral environment. Due to their greater toughness, zirconium oxide materials have been used as a core material for all-ceramic restorations.

Objective

The objective of this study was to evaluate the resin-composite micro-shear bond strength to zirconia using different techniques of surface treatment.

Materials and methods

Fully sintered zirconia (LAVA, 3M-ESPE, Seefeld, Germany) discs were used in combination with resin-composite (Filtek Supreme, 3M-ESPE, Seefeld, Germany) discs and divided into four groups of surface treatments. The micro-shear bond strength was measured by applying an axial load on the bonded interface until failure occurred. Failure load (N) was determined and the samples were examined under a SEM and the failure type was identified. One-way analysis of variance (ANOVA) was used to analyze the data with the level of significance α = 0.05.

Results

Data analysis revealed significant difference between the different tested surface treatments with the group using sandblasting and coated with an experimental primer showing the highest failure load and a cohesive fracture pattern.

Conclusion

Within the limitations of this in vitro study the use of an experimental primer achieved a better bond strength in combination with air-abrasion particles.     

底涂剂对硅橡胶与丙烯酸树脂材料黏结强度的影响

目的:比较不同底涂剂对硅橡胶和丙烯酸树脂黏结强度的影响。方法:取丙烯酸树脂试件8组,其中6组涂不同配方的自制底涂剂,1组涂Cosmesil G611底涂剂,对照组不涂底涂剂,晾干后,与硅橡胶黏结,测试其抗剪强度。应用傅立叶变换红外光谱法对D配方底涂剂的特征吸收谱带进行分析。结果:D配方底涂剂可产生2.20MPa的抗剪强度,Cosmesil G611底涂剂组的抗剪强度为1.44MPa,不涂底涂剂组没有任何黏结力。结论:γ-MPS的浓度与二者的黏结强度密切相关,D配方底涂剂组硅橡胶和丙烯酸树脂间的黏结强度最高。     

涂底剂对氧化锆陶瓷短期粘结强度影响的研究

目的 评价几种新型涂底剂对氧化锆陶瓷与树脂短期粘结强度的影响。方法 加工氧化锆瓷片随机分为6组分别对粘结面进行以下处理:组A,氧化铝喷砂;组B,摩擦化学法硅涂层+硅烷偶联剂;组C,喷砂+Clearfil Ceramic Primer涂底剂;组D,喷砂+ Clearfil SE-Bond涂底剂;组E,喷砂+Z-Prime Plus涂底剂;组F,喷砂+Metal/Zirconia Primer涂底剂。制作复合树脂试件并以传统Bis-GMA基质的树脂水门汀将其粘固于各组氧化锆瓷片上。室温水储24 h后测试剪切粘结强度。结果 组A和组B分别显示了最低和最高的粘结强度,其余各组间无显著差别。结论 氧化锆涂底剂能够提高氧化锆陶瓷的短期树脂粘结强度,但效果弱于硅涂层结合硅烷化的方法。     

The effect of alumina and aluminium nitride coating by reactive magnetron sputtering on the resin bond strength to zirconia core

PURPOSE

Although several surface treatments have been recently investigated both under in vitro and in vivo conditions, controversy still exists regarding the selection of the most appropriate zirconia surface pre-treatment. The purpose of this study was to evaluate the effect of alumina (Al) and aluminium nitride (AlN) coating on the shear bond strength of adhesive resin cement to zirconia core.

MATERIALS AND METHODS

Fifty zirconia core discs were divided into 5 groups; air particle abrasion with 50 µm aluminum oxide particles (Al₂O₃), polishing + Al coating, polishing + AlN coating, air particle abrasion with 50 µm Al₂O₃ + Al coating and air particle abrasion with 50 µm Al₂O₃ + AlN coating. Composite resin discs were cemented to each of specimens. Shear bond strength (MPa) was measured using a universal testing machine. The effects of the surface preparations on each specimen were examined with scanning electron microscope (SEM). Data were statistically analyzed by one-way ANOVA (α=.05).

RESULTS

The highest bond strengths were obtained by air abrasion with 50 µm Al₂O₃, the lowest bond strengths were obtained in polishing + Al coating group (P<.05).

CONCLUSION

Al and AlN coatings using the reactive magnetron sputtering technique were found to be ineffective to increase the bond strength of adhesive resin cement to zirconia core.