Influence of surface conditioning and cleaning methods on resin bonding to zirconia ceramic

Objectives

The purpose of this laboratory study was to evaluate the influence of different surface conditioning, new ceramic primers and cleaning methods on the bond strength of luting resin to zirconia ceramic (e.max ZirCAD).

Methods

A total of 96 zirconia ceramic discs were divided into six groups (n = 16) according to surface conditioning, cleaning methods and ceramic primers. Zirconia ceramic discs were either air-abraded with 110 μm alumina particles or tribochemically silica-coated (Rocatec). Visible dust resulting from air-borne particle abrasion or silica coating was removed either by oil-free air stream or by ultrasonic cleaning in alcohol. Then either a conventional silane (Espe Sil) or a universal primer containing a silane and a phosphate monomer (Monobond Plus) were applied to the conditioned surface. Transparent plastic tubes filled with composite resin were bonded to the zirconia ceramic discs using a luting resin (MultiLink Automix). The bonded specimens were stored in water at 37 °C for 3 days and for 30 days with 7500 thermal cycles between 5 °C and 55 °C prior to tensile test. Statistical analyses were conducted with three-, two- and one-way ANOVAs followed by comparison of means with Tukey's HSD test.

Results

Tensile bond strength ranged from 31.5 to 45.2 MPa after 3 days and from 10.6 to 38.8 MPa after 30 days storage in water with thermal cycling. After artificial aging the decrease in bond strength was significant when the conventional silane was applied after silica coating or when the universal primer was used after air-borne particle abrasion without ultrasonic cleaning (P < .05). However after artificial aging, the decrease in bond strength was not significant (P > .05) when the universal primer was used after air-borne particle abrasion with ultrasonic cleaning or after silica coating.

Significance

A new universal primer improved bonding to zirconia ceramic while the cleaning method had little or no effect.     

2种贴面材料在不同粘接系统下粘接强度的对比研究

目的:比较2种不同贴面材料与3种不同的瓷贴面粘接系统粘接后的粘接强度。方法:应用3种不同的瓷贴面粘接系统(Panavia F、Variolink Veneer、RelyX Veneer),将经过相同处理的离体牙和2种不同的贴面材料(IPS e.max铸瓷和CERAM-AGE聚合瓷)粘接,每组中随机选取一半试件(n=8)37℃水浴24 h,另一半(n=8)冷热循环5 000次后测试其剪切强度,电镜下观察断裂模式。结果:IPS e.max铸瓷组和CERAMAGE聚合瓷组中Variolink Veneer粘接系统在37℃水浴24 h后或5 000次冷热循环后都表现出了最高的粘接强度(P<0.05),所有试件在经过5 000次冷热循环后的粘接强度除Panavia F组外都有明显下降。结论:对于IPS e.max铸瓷和CERAMAGE聚合瓷,Variolink Veneer粘接系统的粘接强度高于Panavia F和RelyXVeneer粘接系统。     

粘结剂使用方式对全酸蚀树脂水门汀与牙本质粘结性能影响的研究

目的评价粘结剂的3种不同使用方式（不使用粘结剂,粘结剂不固化及粘结剂固化10 s）对全酸蚀树脂水门汀与牙本质间粘结性能的影响。方法新鲜拔除的无龋人第三磨牙45颗,随机分为9组（n=5）,流水降温下磨除冠部牙釉质,制备标准牙本质粘结面,酸蚀冲洗后表面按全酸蚀粘结技术处理,牙本质粘结剂处理方式按设计进行,然后与3种全酸蚀树脂水门汀（Rely X ARC、Calibra、VariolinkⅡ）粘结并测试微拉伸粘结强度,用扫描电镜观察粘结界面。结果对于3种全酸蚀树脂水门汀,不使用粘结剂组未测得粘结强度;粘结剂不固化组及粘结剂固化10 s组均获得较为满意的粘结强度,不固化组的微拉伸粘结强度（15.534±2.099;22.827±6.968;10.736±3.199）显著高于粘结剂固化10 s组（13.476±2.710;14.076±5.165;7.736±3.052）（P〈0.05）。结论①全酸蚀树脂水门汀应结合粘结剂同时使用。②牙本质涂布粘结剂后不单独固化可显著提高全酸蚀树脂水门汀与牙本质的粘结强度。     

Comparison of shear bond strength and bonding time of a novel flash-free bonding system

Objective:To evaluate the bonding time, shear bond strength (SBS), and adhesive residue index (ARI) of APC(TM) Flash-Free bonding system.Materials and Methods:Thirty-six extracted human maxillary premolars were randomly divided into three groups (12 per group) and used for this in vitro study: group 1, APC Flash-Free Adhesive Coated Appliance System; group 2, Clarity ADVANCED Ceramic Bracket pasted manually; group 3 (control group), 3M APC PLUS Adhesive prepasted brackets bonded with the extruded flash removed. Bonding time was measured using a stopwatch. Bond strength was measured using an Instron at a cross-head speed of 1 mm/min. The ARI was graded on a scale from 1 to 5. Repeated-measures analysis of variance and post hoc Tukey tests were used for statistical analysis.Results:It took significantly (P < .001) less time to bond in the APC Flash-Free Adhesive group (30.7 ± 3.3 seconds) compared with the control group (41.8 ± 4.0 seconds) and the manual group (39.2 ± 2.8 seconds). The APC Flash-Free Adhesive coated bracket had significantly (P < .001) greater SBS (13.7 ± 2.2 MPa) compared with the control group (10.8 ± 2.0 MPa) and the manual group (10.4 ± 1.4 MPa). The ARI was significantly (P < .001) greater with the APC Flash-Free Adhesive coated bracket compared with that of the other two groups.Conclusions:Compared with other methods of bonding, the APC Flash-Free Adhesive Coated System can potentially reduce bonding time while increasing SBS.     

Durability of Resin Bonds to Pure Titanium

Purpose This study evaluated the bond strength and bond durability of new adhesive systems to pure titanium. Materials and Methods Plexiglass tubes filled with composite were bonded to titanium discs. Groups of 24 samples were bonded using six different bonding systems. Subgroups of eight bonded samples were stored in an isotonic artificial saliva solution (37°C) for 1, 30, or 150 days. In addition, the 30- and 150-day samples were thermal cycled for 7,500 or 37,500 cycles between 5°C and 55°C, respectively. After these storage conditions, all samples were debonded in tension. Results The bond strength of a conventional bisphenol-A glycidyl methacrylate composite to sandblasted titanium was significantly lower than using chemomechanical bonding systems and decreased slightly during the storage time of 150 days. The additional use of a silane on sandblasted titanium resulted in an insignificant increase in bond strength and decreased over storage time to the same level as on sandblasted-only titanium. Statistically significant higher bond strengths were achieved either with the combination of silica coating and use of a conventional bisphenol-A glycidyl methacrylate composite or with the combination of sandblasting and the use of composites modified with a phosphate monomer. In the latter systems, the bond strengths were only limited by the cohesive strength of the composite resins. A new phosphate monomer containing composite showed a tendency to lose cohesive strength over time (statistically not significant). Conclusions Using chemomechanical bonding systems, ie, silica-coating systems or modified composites with adhesive monomers, resulted in 2 to 2.5 times increased bond strength to titanium compared with the bond strength of a conventional bisphenol-A glycidyl methacrylate composite. With chemomechanical bonding systems, the resin bond to titanium was durable over 150 days, even after being stored in water and thermal cycled.     

不同表面处理对义齿软衬树脂黏结强度的影响

目的:探讨4种不同表面处理对义齿软衬树脂与硬质树脂之间黏结强度影响。方法:制作热凝硬质基托树脂试件(直径8mm,长度15mm)和热凝义齿软衬树脂试件(厚4mm,直径10mm),然后将2个硬质树脂试件黏结在软衬树脂正反两面的中心。采用4种不同表面处理方式——第1组,对照组,不加任何处理;第2组,喷砂粗化处理;第3组,专用黏结剂涂布表层;第4组,表层涂布 喷砂粗化。每组各10个试件,分别测定黏结强度,采用SPSS10.0软件进行单因素方差分析。结果:第1、2、3、4组的平均黏结强度分别为3.518、2.834、4.077和3.852MPa。F=6.40,P<0.0014。表层涂布组的黏结强度最高,而喷砂组的黏结强度最低。结论:使用专用黏结剂表层涂布,可显著增强义齿软衬树脂的黏结强度;而进行喷砂处理,反而会使黏结强度下降。     

Effect of time on tensile bond strength of resin cement bonded to dentine and low-viscosity composite

OBJECTIVES: The purpose of this study was to evaluate the tensile bond strength (TBS) of Panavia F resin cement (PF) applied on dentine pre-treated with ED Primer (ED) and Clearfil Liner Bond 2V (CLB) coated with a layer of low-viscosity composite Protect Liner F (PLF) at 10 min, 24 h and 12 months after curing. METHODS: The labial surfaces of 60 bovine lower incisors were ground to obtain a flat dentine surface, allowing a demarcation of a 4.0 mm-diameter area with adhesive tape. The teeth were randomly divided in six groups; ED was applied in groups A I, A II and A III and CLB was applied, followed by PLF, in groups B I, B II and B III. A resin composite rod with a wire loop was luted directly to the prepared surface of each group with PF. The specimens of groups A I and B I were submitted to TBS test after 10 min. Groups A II and B II were submitted to TBS test after 24 h storage and groups A III and B III were submitted to TBS test after 12 months storage. Each specimen was inspected by SEM and classified according to the failure mode. Additionally, two representative specimens of each failure mode were sectioned for a composite/dentine interface SEM evaluation. RESULTS: No significant statistical differences were observed among the groups at 10 min and 24 h. Groups A III and B III presented the lowest TBS values (p<0.05) after 12 months storage. PF on resin-coated dentin (PLF) showed the highest TBS values and was statistically different to PF on dentine for all the groups. The fracture pattern was generally cohesive on the adhesive/hybrid layer for groups A I, A II and A III and cohesive on composite resin for B I, B II and B III. SIGNIFICANCE: The use of a less hydrophilic self-etching system to pre-treat dentine, coating with a low-viscosity composite layer prior luting with resin cement, may provide a protection of the hybridised complex, allowing a dentine seal during the 12 months storage period.     

Durability of Adhesion between Feldspathic Ceramic and Resin Cements: Effect of Adhesive Resin,Polymerization Mode of Resin Cement,and Aging

Purpose : Adhesive cementation is an important step for restorations made of feldspathic ceramic as it increases the strength of such materials. Incorrect selection of the adhesive resin and the resin cement to adhere to the ceramic surface and their durability against aging can affect the adhesion between these materials and the clinical performance. This study evaluated the effect of adhesive resins with different pHs, resin cements with different polymerization modes, and aging on the bond strength to feldspathic ceramic. Materials and Methods : One surface of feldspathic ceramic blocks (VM7) (N = 90) (6.4 × 6.4 × 4.8 mm³) was conditioned with 10% hydrofluoric acid for 20 seconds, washed/dried, and silanized. Three adhesive resins (Scotchbond Multi‐Purpose Plus [SBMP], pH: 5.6; Single Bond [SB], pH: 3.4; and Prime&Bond NT [NT], pH: 1.7) were applied on the ceramic surfaces (n = 30 per adhesive). For each adhesive group, three resin cements with different polymerization modes were applied (n = 10 per cement): photo‐polymerized (Variolink II base), dual polymerized (Variolink II base + catalyst), and chemically polymerized (C&B). The bonded ceramic blocks were stored in water (37°C) for 24 hours and sectioned to produce beam specimens (cross‐sectional bonded area: 1 ± 0.1 mm²). The beams of each block were randomly divided into two conditions: Dry, microtensile test immediately after cutting; TC, test was performed after thermocycling (12,000×, 5°C to 55°C) and water storage at 37°C for 150 days. Considering the three factors of the study (adhesive [3 levels], resin cement [3 levels], aging [2 levels]), 18 groups were studied. The microtensile bond strength data were analyzed using 3‐way ANOVA and Tukey's post hoc test (α= 0.05). Results : Adhesive resin type (p < 0.001) and the resin cement affected the mean bond strength (p= 0.0003) (3‐way ANOVA). The NT adhesive associated with the chemically polymerized resin cement in both dry (8.8 ± 6.8 MPa) and aged conditions (6.9 ± 5.9 MPa) presented statistically lower bond strength results, while the SBMP adhesive resin, regardless of the resin cement type, presented the highest results (15.4 to 18.5 and 14.3 to 18.9 MPa) in both dry and aged conditions, respectively (Tukey's test). Conclusion : Application of a low‐pH adhesive resin onto a hydrofluoric acid etched and silanized feldspathic ceramic surface in combination with chemically polymerized resin cement did not deliver favorable results. The use of adhesive resin with high pH could be clinically advised for the photo‐, dual‐, and chemically polymerized resin cements tested.     

不同表面处理方式对丙烯酸树脂表面性状和粘接强度的影响

目的探讨不同表面处理方式对丙烯酸树脂表面性状和粘接强度的影响。方法制备硅橡胶与丙烯酸树脂构成的重叠联合模型。根据树脂条的不同表面处理方式,将模型随机分为4组:对照组、MMA浸润组、喷砂组、MMA浸润+喷砂组。用扫描电镜观察各组树脂处理后的表面形态变化,用粗糙度仪检测其粗糙度,万能材料试验机测定树脂条和硅橡胶之间的粘接强度。结果 1.电镜观察显示,未经处理的树脂条表面打磨痕迹明显,经过MMA浸润后,表面出现溶解的痕迹,经过喷砂后,表面粗糙凸凹不平;2.粗糙度:喷砂组(3.12±0.02)μm和MMA浸润+喷砂组(3.11±0.01)μm>对照组(0.73±0.01)μm和MMA浸润组(0.71±0.01)μm,且差异有统计学意义(P<0.05);3.粘接强度:MMA浸润+喷砂组(2.34±0.03)MPa>喷砂组(2.02±0.01)MPa>MMA浸润组(1.81±0.02)MPa>对照组(1.50±0.01)MPa,且差异有统计学意义(P<0.05)。结论 MMA单体浸润与喷砂的处理方式可以使丙烯酸树脂表面的形貌发生变化,更有利于硅橡胶与丙烯酸树脂的结合,获到良好的粘接效果,可在临床推广使用。     

Resin bonding to enamel and dentin with one–component UDMA/HEMA adhesives

The aim of this study was to investigate the potential of UDMA/HEMA mixtures as priming and sealing components of dental adhesives. The monomers were mixed in weight ratios 100/0, 80/20, 60740, 50/50, 40/60, 20/80, 10/90, and 0/100, light activated, and dissolved in acetone at equal parts. The 60/40 UDMA/HEMA mixture served as a reference which was modified with 5, 10, 20, and 30 parts 4-MET relative to the mass of the basic monomer mixture. Shear bond strengths (24 h) of resin composite cylinders, bonded with the adhesive monomers on human enamel and dentin, were determined following a total etch technique with phosphoric acid and application of the adhesives in 2 coats on moist tooth surfaces. Average bond strength to enamel was 32 MPa with no difference between the adhesives. On dentin, significantly different bond strengths were found between UDMA (12.9 MPA) and HEMA (19.4 MPa), whereas all binary mixtures bond strengths were not significantly different (mean 16.2 MPa). Addition of 5 to 20 wt% 4-MET resulted in a significantly increased mean shear bond strength of 22.3 MPa on dentin. At 10%, a maximum mean strength of 25.4 MPa was recorded. It is concluded that mixtures of commonly used polymerizable monomers, characterized by hydrophilic moieties and dissolved in acetone, are promising candidates for effective resin bonding to enamel and dentin, provided application by the moist bonding technique.     

瓷表面不同处理方法及粘结剂对全瓷剪切强度的影响

目的:观察喷砂、酸蚀及硅烷偶联剂等表面处理方法对热压铸陶瓷,玻璃渗透陶瓷和氧化锆陶瓷与不同种粘结剂的粘结强度的影响。方法:样本分为热压铸陶瓷组,渗透陶瓷组和氧化锆陶瓷组。分别应用不同表面处理方法和粘结剂,测其剪切强度。结果:方差分析表明,热压铸陶瓷组中酸蚀涂硅烷树脂粘结组粘结强度最高,渗透陶瓷组中喷砂玻璃离子粘结组粘结强度最高,氧化锆陶瓷组中喷砂玻璃离子粘结组粘结强度最高。结论:应用常规树脂粘结剂粘固热压铸陶瓷修复体取得较好的粘固效果,采用酸蚀和硅烷偶联剂的表面处理,可取得最大粘结强度。     

脉冲Nd:YAG激光照射对牙釉质粘结性能的影响

目的 :探讨脉冲Nd :YAG激光作为牙体表面处理技术对牙釉质粘结性能的影响。方法 :分别用 1W、2 0Hz,1W、15Hz,1.5W、2 0Hz,1.5W、15Hz,2W、15Hz共 5个能量输出组照射离体牙釉质表面 ,测定其与复合树脂的抗张粘结强度 ,并与未处理组、35 %磷酸酸蚀组进行对照。结果 :激光照射组中输出能量为 1W、15Hz时抗张粘结强度最高 (3.87± 1.91MPa) ,其次是 1W、2 0Hz(3.4 3± 1.4 8MPa) ,两组间无显著差异 (P >0 .0 5 ) ,但都显著高于其它三个激光照射组及未处理组 (P <0 .0 5 )。酸蚀组的抗张粘结强度最高 (8.5 0± 3.0 2MPa) ,显著高于其它 6个实验组(P <0 .0 5 )。结论 :脉冲Nd :YAG激光处理牙釉质表面可改善粘结性能 ,抗张粘结强度受激光输出能量的影响 ,当激光输出能量为 1W、15Hz时抗张粘结强度最高 ,但低于酸蚀组。脉冲Nd :YAG激光能否作为一种牙釉质表面处理技术应用于临床尚需进一步研究     

Mechanical properties and bonding of maxillofacial silicone elastomer mixed with nano-sized anti-microbials

ObjectivesThe antibacterial efficacy of silicone is improved by impregnating it with antimicrobials such as chlorohexidine and zinc oxide. The purpose of this study was to examine mechanical properties and bonding of maxillofacial silicone elastomer mixed with Zinc Oxide nanoparticles (ZnO-NP), and Chlorohexidine Diacetate Salt (CHX) at three different concentrations (1 %, 3 %, and 5 %).MethodsSpecimens of a silicone elastomer (M511) were prepared and divided into 7 groups. Group 1 was control of no additive. Groups 2–4 included silicone elastomer mixed with ZnO-NP (surface area = 67 m²/g) at 3 different concentrations (by weight %); 1 %, 3 % and 5 %. Groups 5–7 included silicone elastomer mixed with CHX at the same concentrations. Tear and tensile strengths, elongation percentage, modulus of elasticity, and shear bond strength to primed acrylic resin surfaces were evaluated. Data was analyzed with 1-way ANOVA, Bonferroni, and Dunnett’s T3 post-hoc tests (P < 0.05).ResultsThere was significant effect of the additives on the tensile strength, elongation percentage, tear strength, and shear bond strength (P < 0.05). Shear bond strengths ranged from 0.55 to 0.96 MPa. Silicone elastomer mixed with CHX (5 %) resulted in the highest shear bond strength (P < 0.05). Non-linear regressions between tensile strength and ZnO and CHX additives were 0.95 and 0.96 respectively.SignificanceAll additives reduced the tensile strength of the silicone. However, CHX at 5 % optimized shear bond strength and thus is proposed in order to fabricate maxillofacial prostheses of sufficient mechanical properties, bonding and antimicrobial activity.     

瓷表面处理对正畸托槽与瓷黏结抗剪强度的影响

目的:探讨不同瓷表面处理技术对正畸托槽与瓷黏结抗剪强度的影响。方法:采用4组不同的瓷表面处理方式,使用光固化正畸黏结剂将瓷面分别与金属和陶瓷托槽黏结,每组再平均分为2组分别在37℃水浴24h和7d后冷热循环500次(5～55℃),测量黏结抗剪强度,并统计其黏结剂残留指数,在扫描电镜下观察其瓷面显微结构的变化。结果:4种瓷表面处理技术对2种不同材料托槽处理的结果近似,均可达到有效正畸黏结强度。结论:磷酸酸蚀结合硅烷偶联剂是正畸托槽与瓷黏结的较佳方式之一。     

Using bonding agent prior to pits and fissure sealant application enhances the microtensile bond strength and the interface morphology

BackgroundA pits and fissures sealant is an effective method for preventing dental caries. Using a bonding agent before applying the sealant may increase its retention. This study aimed to compare the microtensile strength (µTBS) of a fissure sealant with and without a bonding agent and to characterize the enamel-sealant interface using confocal laser scanning microscopy (CLSM). The null hypothesis was that the use of a bonding agent before fissure sealant application would not change the microtensile strength or the enamel-sealant interface.Materials and methodsTwenty caries-free premolars were used. Each tooth was divided into four parts. The first two parts were assigned to the bonded group, where a bonding system was used before sealant application. The remaining two parts were treated only with a fissure sealant (i.e., the nonbonded group). In each group, the µTBS was examined after 24 h (n = 20) and after a 3-month aging period (n = 20). Five other caries-free extracted premolars were used to assess the enamel-sealant interface using CLSM. Two-way analysis of variance (ANOVA) and Pearson chi-square statistical analysis tests were used to analyze the µTBS and the enamel-sealant interface, respectively.ResultsThe mean µTBS for the bonded group was significantly higher (p = 0.001) in the immediate group (36.87 ± 14.95 MPa) and the aged group (31.08 ± 15.88 MPa) than in the respective nonbonded groups (19.77 ± 9.67 MPa and 19.52 ± 14.14 MPa). The µTBS was not significantly different in either group after aging (p = 0.46 [bonded group] and p = 0.98 [nonbonded group]). In addition, using a dental adhesive, before applying a fissure sealant resulted in a significantly higher (53%) resin penetration into the enamel with the continuous integrity of the resin.ConclusionThe use of a bonding agent before the application of fissure sealant resulted in superior microtensile bond strength immediately and after aging. In addition, the enamel-sealant interface characteristics were improved.     

Repair of glass ionomer cements — methods for conditioning the surface of the cement to achieve bonding

Two chemically different glass ionomer cements (Ketac Fil® and ChemFil II® Caps) and three different methods of conditioning the surface for repair were evaluated. Specimens of each material were prepared, aged and sectioned. The cut surfaces were treated with either phosphoric acid, polyacrylic acid or a combination of phosphoric acid followed by polyacrylic acid. Freshly mixed glass ionomer cement was injected against the treated surface and allowed to set under simulated intra-oral conditions. The specimens were then tested to failure in flexion after 7 days storage. The flexural strength of the repaired specimens was compared with that of control specimens of the same materials. The flexural strength of the repaired specimens was less than that of the controls. Treatment of the fractured surface with polyacrylic acid produced the weakest repair, and the use of phosphoric acid as the conditioning agent produced repaired specimens approximately 80% of the strength of the controls.     

树脂粘结剂与瓷表面处理对全瓷粘结微拉伸强度的影响

目的 研究3种树脂粘结剂配合2种瓷表面处理方法对全瓷粘结微拉伸强度的影响.方法 制作60个体积为5mm×6mm×8mm瓷试件(Empress Ⅱ),抛光后分成两组:对照组和HF SIL组(5%氢氟酸酸蚀20秒,硅烷处理1分钟).分别采用3种树脂粘结剂(RelyX Unicem, Variolink或Panavia F)与复合树脂粘结,37℃保存7天,切割成接触面积为1.0mm2的75个柱形体.试件经热循环(5℃～55℃循环3000次)后,测量粘结微拉伸强度(uTBS).结果 表面处理因素有重要意义(HF SIL组>对照组).对照组中Rely X Unicem的uTBS明显高于Variolink和Panavia F.HF SIL组中经RelyX Unicem和Variolink的uTBS明显高于Panavia F.结论 无论使用何种树脂粘结剂,在粘结前进行酸蚀和硅烷处理都是必要的.     

喷砂结合化学处理对软衬材料粘结效果的影响

[摘要]目的：研究喷砂结合化学处理对硅橡胶软衬材料与基托树脂间粘结强度及基托树脂挠曲强度的影响。方法：制备48块30mm×10mm×7．5mm热凝聚甲基丙烯酸甲酯树脂块,每2个树脂块配成一个试件,24个试件随机分为4组,每组6个试件,即：（1）喷砂组：喷嘴与试件轻接触,采用250txm的氧化铝,在0．62MPa压力下喷砂30S;（2）喷砂＋丙酮组：粘结面喷砂处理同前,喷砂后的粘结面浸泡在丙酮溶液中30S;（3）喷砂＋甲基丙烯酸甲酯单体组（后简称单体）：粘结面喷砂处理同上,喷砂后的树脂块粘结面浸泡在甲基丙烯酸甲酯溶液中180S;（4）对照组：表面不处理。每个试件的两树脂块间衬以3mm厚的软衬材料,冷热循环5000次后,置于万能测试机上,以5mm／min的加载速度测试其拉伸粘结强度。另制备24块65mm×10mm×3．3mm长方体树脂块,分组及表面处理同前,涂布软衬材料粘结剂后测试挠曲强度。结果：喷砂组、喷砂＋丙酮组、喷砂＋甲基丙烯酸甲酯组及对照组试件的拉伸粘结强度分别为（1．31±0．45）MPa、（1．75±0．34）MPa、（1．96±0．50）MPa及（0．90±0．17）MPa。喷砂组与对照组间差别无统计学意义（P〉0．05）。喷砂＋丙酮组及喷砂＋单体组的拉伸粘结强度与对照组相比有统计学差异（P〈0．05）;喷砂＋丙酮组与喷砂＋单体组组间比较无统计学差异;四组间挠曲强度均无统计学差异（P〉0．05）。结论：喷砂结合化学处理树脂表面能增强硅橡胶软衬材料与基托树脂间的粘结强度,且对基托树脂挠曲强度没有影响。     

Development of a novel surface modification for improved bonding to zirconia

Objective

This report presents a novel pretreatment technique, whereby the zirconia surface is converted to a more reactive zirconium oxyfluoride, enabling improved chemical bonding to other dental substrates via conventional silanation approaches.

Methods

The study leverages a novel gas-phase fluorination process that creates a thin oxyfluoride conversion layer on the surface of zirconia, making it more reactive for conventional adhesive bonding techniques. Zirconia specimens, polished and roughened, were pretreated and composite cylinders bonded using conventional adhesive techniques. All specimens were subjected to a force at a crosshead speed of 0.5 mm/min in an electro-mechanical testing device. Single-factor analysis of variance (ANOVA) at a 5% confidence level was performed for the bonding strength data. Optical microscopy and scanning electron microscopy (SEM) were used to evaluate and quantify failure surfaces.

Results

Shear bond strengths were analyzed using single-factor ANOVA (p < 0.05). Mechanical testing results revealed that fluorinated zirconia specimens (both rough and polished) displayed the highest shear bond strengths as compared to other commercially available treatments. X-ray photoelectron spectroscopy analysis helped determine that this novel pretreatment created a more reactive, 2-4 nm thick oxyfluoride conversion layer with approximate stoichiometry, ZrO₃F₄.

Conclusion

Simple shear bond mechanical tests demonstrated that a fluorination pre-treatment is a viable method to chemically modify zirconia to produce a reactive surface for adhesive bonding.