Effects of post surface conditioning before silanization on bond strength between fiber post and resin cement

PURPOSE

Post surface conditioning is necessary to expose the glass fibers to enable bonding between fiber post and resin cement. The purpose of the present study was to evaluate the effect of different surface conditioning on tensile bond strength (TBS) of a glass fiber reinforced post to resin cement.

MATERIALS AND METHODS

In this in vitro study, 40 extracted single canal central incisors were endodontically treated and post spaces were prepared. The teeth were divided into four groups according to the methods of post surface treatment (n=10): 1) Silanization after etching with 20% H₂O₂, 2) Silanization after airborne-particle abrasion, 3) Silanization, and 4) No conditioning (Control). Adhesive resin cement (Panavia F 2.0) was used for cementation of the fiber posts to the root canal dentin. Three slices of 3 mm thick were obtained from each root. A universal testing machine was used with a cross-head speed of 1 mm/minute for performing the push-out tests. Two-way ANOVA and Tukey post hoc tests were used for analyzing data (α=0.05).

RESULTS

It is revealed that different surface treatments and root dentin regions had significant effects on TBS, but the interaction between surface treatments and root canal regions had no significant effect on TBS. There was significant difference among H₂O₂ + Silane Group and other three groups.

CONCLUSION

There were significant differences among the mean TBS values of different surface treatments. Application of hydrogen peroxide before silanization increased the bond strength between resin cements and fiber posts. The mean TBS mean values was significantly greater in the coronal region of root canal than the middle and apical thirds.     

不同方向剪切力作用下两种树脂粘结剂与人牙釉质的剪切粘结强度研究

目的：考察不同施力方向上树脂粘结剂与人牙釉质的剪切粘结强度。方法：使用树脂类粘结剂A（Clearfil SE BOND）和B（Prime＆Bond NT），将各自配套的复合树脂粘结在离体人牙釉质面上，当剪切力沿根尖、骀面、近中和远中方向作用时测量其剪切粘结强度。结果：粘结剂A和B与牙釉质的剪切粘结强度值显示，根尖方向[分别为（44．38±3．68）Pa和（45．50±2．88）Pa]〉近中方向[分别为（37．81±7．56）Pa和（40．15±2．59）Pa]和远中方向[分别为（35．71±3．34）Pa和（35．75±4．15）Pa]〉[牙合]面方向[分别为（29．19±3．75）Pa和（33．44±3．79）Pa]，近中方向和远中方向间差异无统计学意义（P〉0．05），根尖方向与[牙合]面方向间差异有统计学意义（P〈0．05）。结论：树脂粘结剂与人牙釉质剪切粘结强度的大小与剪切力作用的方向相关。     

树脂水门汀与氧化锆陶瓷剪切粘接强度的研究

目的评估不同实验条件下树脂水门汀与氧化锆瓷之间的剪切粘接强度（SBS）。 方法使用计算机辅助设计与制作（CAD/CAM）设备切割并烧结制作6个边长为2 cm的正方体氧化锆试件。按不同实验条件将8种双固化树脂水门汀分为13组（n = 20）：（1）Monobond N + Multilink N（MMN组）;（2）Ivoclean + Monobond N + Multilink N（IMM组）;（3）Ivoclean + Monobond N + Multilink N[无喷砂,IMM（ns）组];（4）Tetric N-Bond Universal + Multilink Speed（TUM组）;（5）Multilink Speed（MLS组）;（6）Z-Prime Plus + TheraCem（ZPT组）;（7）Z-Prime Plus + Duo-Link（ZPD组）;（8）Single Bond Universal + RelyX U200（SRU组）;（9）RelyX U200（RXU组）;（10）Single Bond Universal + RelyX Ultimate Clicker（SRU组）;（11）OptiBond Versa + Kerr NX3（OVK组）;（12）Clearfil Universal Bond + Clearfil SAC（CUS组）;（13）Clearfil SAC（SAC组）。将每组树脂水门汀自混合注入透明模具并将其无压力置于氧化锆面后进行光照固化。所有试件在37 ℃水中存储24 h后进行SBS测试。采用SPSS 19.0软件One-Way ANOVA（P<0.05）对SBS进行统计学分析。利用电子体视显微镜观察氧化锆端断裂界面。 结果本实验中13组树脂水门汀的SBS（单位：MPa）降序排列依次为：OVK（27.51 ± 3.65）>IMM（27.28 ± 3.79）>SRC（26.77 ± 3.62）>CUS（25.36 ± 3.10）>TUM（25.22 ± 4.88）>ZPD（23.96 ± 6.25）>MLS（23.13 ± 2.74）>MMN（23.07 ± 3.71）>SAC（22.20 ± 3.59）>IMM（ns）（21.99 ± 3.50）>SRU（19.19 ± 2.27）>ZPT（18.62 ± 2.08）>RXU（15.04 ± 4.02）。 结论（1）不同树脂水门汀的SBS具有材料依赖性;（2）在氧化锆表面进行喷砂处理、使用专用清洗剂或将通用型粘接剂作为底漆使用有利于提高树脂水门汀的SBS。     

Push-out bond strength and failure mode of single adjustable and customized glass fiber posts

PurposeTo evaluate the push-out bond strength (PBS) and failure mode of single adjustable (SAP) and customized (CP) posts cemented to root canal dentin using conventional (RelyX Ultimate) or self-adhesive (RelyX U200) dual-cure resin cements.MethodsHerein, 40 bovine mandibular incisors were divided into four groups (n = 10): SAP cemented with RelyX Ultimate (SAP-UT), SAP cemented with RelyX U200 (SAP-U2), CP cemented with RelyX Ultimate (CP-UT), and CP cemented with RelyX U200 (CP-U2). PBS and failure modes were analyzed. Three-way repeated measures ANOVA test followed by Tukey’s test and Fisher–Freeman–Halton exact test were used for data analysis (α = 5%).ResultsThe PBS values for SAP (p < .05) were higher than those for CP and were not influenced by the root third and resin cement (p > .05). When conventional resin cement was used, the SAP showed significant differences compared to CP (p < .05). When cemented with RelyX Ultimate, a higher prevalence of mixed and adhesive failures for SAP and CP, respectively, was observed (p < .05). For the self-adhesive resin cement, the failures were mostly adhesive (p < .05).ConclusionSAP showed better performance than CP. The root third and resin cements did not influence the PBS. The most prevalent failures were adhesive and mixed.     

Push-out bond strength of fiber posts to root dentin using glass ionomer and resin modified glass ionomer cements

Objective

The purpose of this study was to assess the push-out bond strength of glass fiber posts to root dentin after cementation with glass ionomer (GICs) and resin-modified glass ionomer cements (RMGICs).

Material and Methods

Fifty human maxillary canines were transversally sectioned at 15 mm from the apex. Canals were prepared with a step back technique until the application of a #55 K-file and filled. Post spaces were prepared and specimens were divided into five groups according to the cement used for post cementation: Luting & Lining Cement; Fuji II LC Improved; RelyX Luting; Ketac Cem; and Ionoseal. After cementation of the glass fiber posts, all roots were stored at 100% humidity until testing. For push-out test, 1-mm thick slices were produced. The push-out test was performed in a universal testing machine at a crosshead speed of 0.5 mm/minute and the values (MPa) were analyzed by Kolmogorov-Smirnov and Levene''s tests and by two-way ANOVA and Tukey''s post hoc test at a significance level of 5%.

Results

Fiber posts cemented using Luting & Lining Cement, Fuji II LC Improved, and Ketac Cem presented the highest bond strength to root dentin, followed by RelyX Luting. Ionoseal presented the lowest bond strength values (P>0.05). The post level did not influence the bond strength of fiber posts to root dentin (P=0.148). The major cause of failure was cohesive at the cement for all GICs and RMGICs.

Conclusions

Except for Ionoseal, all cements provided satisfactory bond strength values.     

热冷循环对托槽抗剪切强度影响的研究

目的 比较冷热循环前后两种粘接剂抗剪切粘接强度，从而研究冷热循环实验对粘接剂抗剪切强度的影响。方法 90颗因正畸需要而拔除的人类前磨牙按照粘接剂（超强粘接剂和京津釉质粘合剂）和储存条件（室温蒸馏水中、37℃人工唾液中、冷热循环实验）的不同随机均分为6组，粘接金属方丝弓托槽，测定并记录抗剪切粘接强度和牙面残留粘接剂指数。结果 方差分析显示两种粘接剂粘接强度无明显差剐，但冷热循环后粘接强度均明显降低（P〈0．01）；牙面残留粘接剂指数无明显差别。结论 冷热循环实验可明显降低托槽抗剪切粘接强度，体外粘接强度研究应进行冷热循环实验。     

Comparison of the effect of storage media on shear punch strength of resin luting cements

Objectives

To measure the shear punch strength of eight resin-containing luting cements before and after immersion in acidic solution and ethanol at different temperatures (37° C and 60 °C). Method: Specimens were prepared from six resin luting cements; Set (SDI), Panavia F (Kuraray), RelyX Veneer (3M/ESPE), VarioloinkII (Ivoclar), Maxcem (Kerr), Nexus2 (Kerr) and two Resin-modified glass-ionomer luting cements (RM-GICs); GC Fuji Plus (GC Corporation), RelyX Luting 2 (3 M/ESPE). For each material a total of 114 disc-shaped specimens were prepared. Six specimens were immersed in distilled water for 24 h at 37 °C, polished and subjected to baseline measurement for shear punch strength. The remaining 108 specimens were randomly divided into 18 groups of six, and immersed in three solutions; distilled water, 0.01 mol/L lactic acid, and 50% ethanol at 37 °C or 60 °C, for 1 week, 1 month or 3 months. Specimens were washed, dried and tested for final shear punch strength.

Results

Values were material and solution dependent. Values of Nexus 2 and Rely X Veneer are the highest, and Rely X Luting 2 the lowest. Ethanol and lactic acid specimens showed significantly lower values compared with the distilled water specimens. Conclusion: The shear punch strengths of the resin-containing luting cements were affected by time and storage solution. While some of the resin luting cements had significantly higher values compared to that of the RM-GICs, there were no significant differences between the RM-GICs and resin cements such as Panavia F and Set.     

自粘接型树脂粘接剂对玻璃陶瓷粘接耐久性的研究

目的 评价自粘接型和普通型树脂粘接剂与玻璃陶瓷粘接的耐久性,以期为树脂粘接剂的临床应用提供参考.方法 按照ISO 4049 国际标准,对粘接剂A(自粘接型,G-CEM)和粘接剂B(普通型,Linkmax HV)各5个试件在6周内的最大吸水值和溶解值以及其光照射后0.5、24 h和6周的表面显微硬度进行测量.对64个陶瓷试件分别使用硅烷偶联剂A(Monobond S)、B(Clearfil Ceramic Primer)和C(GC Ceramic Primer)进行表面处理或不进行表面处理,再分别使用粘接剂A和B粘接,并于冷热循环前和冷热循环30 000次后测量试件粘接强度.结果 粘接剂A的吸水值和溶解值分别为(79.62±5.63)和(4.78±3.33)μg/mm～3,明显高于粘接剂B[分别为(35.03±3.33)和(0.00±0.00)μg/mm～3].两种粘接剂的表面显微硬度在光照射后24 h达到最大值.冷热循环30 000次后未行表面处理和硅烷偶联剂A、B、C处理后的陶瓷试件与粘接剂A的粘接强度分别为(0.00±0.00)、(2.86±3.25)、(12.75±1.55)和(11.98±2.35)MPa,与粘接剂B对应试件粘接强度[分别为(0.00±0.00)、(5.15±5.20)、(10.94±3.30)和(14.18±3.13)MPa]的差异无统计学意义.结论 在使用硅烷偶联剂的前提下,自粘接型树脂粘接剂可以代替普通型树脂粘接剂进行玻璃陶瓷粘接.     

三种金属处理剂对金属与复合树脂间剪切粘接强度影响的研究

目的 研究崩瓷树脂修复中，三种不同金属处理剂对金属与复合树脂间剪切粘接强度的影响。方法 40个Ni-Cr合金试件随机分4组。模拟口内喷砂后，除对照组外，其他试件分别采用couplingsilane、alloyprimer、metalphot0primer三种不同金属处理剂对金属表面处理，然后所有试件使用VocoCLmara崩瓷修复系统粘接修复，经37℃恒温水浴24小时后，测定金属试件与复合树脂之间剪切粘接强度，进行统计分析。结果 三种金属处理剂组所获得的Ni-Cr合金与复合树脂间剪切粘接强度值显著高于对照组（P〈0．05）；metalphotoprimer组与alloyprimer组所获得的Ni-Cr合金与复合树脂间剪切粘接强度值显著高于couplingsilane组（P〈0．05）；但metalphotoprimer组与alloy primer组之间无统计差异（P〉0．05）。20倍OPTON体视显饭镜下观察到金属与复合树脂的剪切断面均位于金属一复合树脂粘接界面，未发生复合树脂内聚断裂。结论 couplingsilane、alloyprimermetalphotoprimer三种金属处理剂可以显著提高金属-复合树脂间粘接强度。     

Evaluation of shear bond strength between dual cure resin cement and zirconia ceramic after thermocycling treatment

PURPOSE

This study was performed to evaluate shear bond strength (SBS) between three dual-cured resin cements and silica coated zirconia, before and after thermocycling treatment.

MATERIALS AND METHODS

Sixty specimens were cut in 15 × 2.75 mm discs using zirconia. After air blasting of 50 µm alumina, samples were prepared by tribochemical silica coating with Rocatec™ plus. The specimens were divided into three groups according to the dual-cure resin cement used: (1) Calibra silane+Calibra®, (2) Monobond S+Multilink® N and (3) ESPN sil+RelyX™ Unicem Clicker. After the resin cement was bonded to the zirconia using a Teflon mold, photopolymerization was carried out. Only 10 specimens in each group were thermocycled 6,000 times. Depending on thermocycling treatment, each group was divided into two subgroups (n=10) and SBS was measured by applying force at the speed of 1 mm/min using a universal testing machine. To find out the differences in SBS according to the types of cements and thermocycling using the SPSS, two-way ANOVA was conducted and post-hoc analysis was performed by Turkey''s test.

RESULTS

In non-thermal aged groups, SBS of Multilink group (M1) was higher than that of Calibra (C1) and Unicem (U1) group (P<.05). Moreover, even after thermocycling treatment, SBS of Multilink group (M2) was higher than the other groups (C2 and U2). All three cements showed lower SBS after the thermocycling than before the treatments. But Multilink and Unicem had a significant difference (P<.05).

CONCLUSION

In this experiment, Multilink showed the highest SBS before and after thermocycling. Also, bond strengths of all three cements decreased after thermocycling.     

TMPT对实验牙本质封闭剂与树脂水门汀粘接性能的影响

目的:探讨TMPT添加型实验牙本质封闭剂对树脂水门汀粘接性能的影响.方法:通过添加不同比例的TMPT于“劲润”牙本质保护膜(HyC)中试制牙本质封闭剂T0、T33、T67和T100,采用剪切强度测试结合体式显微镜观察断面破坏方式,评价各组实验牙本质封闭剂与Super-Bond C＆B(SU)、Panavia F(PA)及G-CEM(G-CEM)等不同种类水门汀之间的粘接性能.结果:SU与各组实验牙本质封闭剂之间粘接力均较强,达20 MPa以上;G-CEM及PA与T0之间粘接力分别为16.60和12.26 MPa.随着TMPT的添加,SU组粘接力呈现增大趋势,而G-CEM与PA组呈现减小趋势.结论:HyC及TMPT添加型实验牙本质封闭剂与Super-Bond C＆B的粘接性能较好.     

不同酸性水解催化液对硅基质陶瓷与树脂粘接效果的影响

目的 研究使用新型双液型硅烷底涂剂(A、B液)对树脂-硅基质陶瓷粘接效果的影响.方法 将432个陶瓷实验体分为9组(每组48个),分别使用9种实验性底涂剂处理陶瓷表面.9种底涂剂中A液均为50 g/L甲基丙烯酰氧基丙基三甲氧基硅烷(γ-methacryloxypropyletrimethoxysilane,MPTS)的乙醇溶液,B液分别为0.10、0.05、0.01 mol/L盐酸、磷酸和醋酸水溶液与同体积99％乙醇配比的混合溶液.处理后陶瓷与树脂粘接剂(Link Max,GC,日本)粘接形成实验体.其后将每组分为3个亚组(每个亚组各16个实验体)分别在24h后、5000次和10000次冷热循环后测试剪切强度.结果 冷热循环前后最高剪切强度均在0.05 mol/L盐酸组,分别为(19.5±3.7)、(15.7±3.0)、(14.6±3.0) Mpa.10 000次冷热循环后,当酸性溶液浓度为0.10 mol/L时,盐酸组的(10.6±3.5)Mpa和磷酸组的(9.5±2.7)Mpa明显高于醋酸组的(6.3±2.5) Mpa (P＜0.05);当酸性溶液浓度为0.05 mol/L时,盐酸组的(14.6±3.0)Mpa明显高于磷酸组的(6.3±1.9) Mpa和醋酸组的(4.7±1.8) Mpa (P＜0.05);当酸性溶液浓度为0.01 mol/L时,盐酸组的(12.7±3.2) Mpa明显高于磷酸组的(2.3±1.2) Mpa和醋酸组的(1.5±1.2) Mpa (P＜0.05).结论 选择0.05 mol/L盐酸作为水解催化液的硅烷底涂剂可得到较高的硅基质陶瓷-树脂粘接强度及粘接耐久性.     

树脂加强型玻璃离子粘固剂粘结强度的研究

目的 检测树脂加强型玻璃离子粘固剂的粘结强度,探讨影响粘结性能的相关因素.方法 30颗健康离体前磨牙分成两组,分别用京津釉质粘合剂和树脂加强型玻璃离子粘固剂初次、二次粘接托槽,测剪切强度及粘结剂残余指数.结果 树脂加强型玻璃离子粘固荆的粘结强度与临床普遍使用的京津釉质粘合剂的粘结强度相近,差异无显著性(P>O.05).结论 树脂加强型玻璃离子粘固剂可以替代复合树脂粘结剂.能够满足临床需要.     

Conventional dual-cure versus self-adhesive resin cements in dentin bond integrity

During post preparation, the root canal is exposed to the oral cavity, and endodontic treatment may fail because of coronal leakage, bacterial infection and sealing inability of the luting cement.

Objective

this study quantified the interfacial continuity produced with conventional dual-cure and self-adhesive resin cements in the cervical (C), medium (M) and apical (A) thirds of the root.

Material and methods

Forty single-rooted human teeth were restored using Reforpost # 01 conical glass-fiber posts and different materials (N=10 per group): group AC=Adper™ ScotchBond™ Multi-purpose Plus + AllCem; group ARC=Adper™ ScotchBond™ Multi-purpose Plus + RelyX ARC; group U100=RelyX U100; and group MXC=Maxcem Elite. After being kept in 100% humidity at 37ºC for 72 hours, the samples were sectioned parallel to their longitudinal axis and positive epoxy resin replicas were made. The scanning electron micrographs of each third section of the teeth were combined using Image Analyst software and measured with AutoCAD-2002. We obtained percentage values of the interfacial continuity.

Results

Interfacial continuity was similar in the apical, medium and cervical thirds of the roots within the groups (Friedman test, p>0.05). Comparison of the different cements in a same root third showed that interfacial continuity was lower in MXC (C=45.5%; M=48.5%; A=47.3%) than in AC (C=85.9%, M=81.8% and A=76.0%), ARC (C=83.8%, M=82.4% and A=75.0%) and U100 (C=84.1%, M=82.4% and A=77.3%) (Kruskal-Wallis test, p<0.05).

Conclusions

Allcem, Rely X ARC and U100 provide the best cementation; cementation was similar among root portions; in practical terms, U100 is the best resin because it combines good cementation and easy application and none of the cements provides complete interfacial continuity.     

Push-out bond strengths of fiber-reinforced composite posts with various resin cements according to the root level

PURPOSE

The aim of this study was to determine whether the push-out bond strengths between the radicular dentin and fiber reinforced-composite (FRC) posts with various resin cements decreased or not, according to the coronal, middle or apical level of the root.

MATERIALS AND METHODS

FRC posts were cemented with one of five resin cement groups (RelyX Unicem: Uni, Contax with activator & LuxaCore-Dual: LuA, Contax & LuxaCore-Dual: Lu, Panavia F 2.0: PA, Super-Bond C&B: SB) into extracted human mandibular premolars. The roots were sliced into discs at the coronal, middle and apical levels. Push-out bond strength tests were performed with a universal testing machine at a crosshead speed of 0.5 mm/min, and the failure aspect was analyzed.

RESULTS

There were no significant differences (P>.05) in the bond strengths of the different resin cements at the coronal level, but there were significant differences in the bond strengths at the middle and apical levels (P<.05). Only the Uni and LuA cements did not show any significant decrease in their bond strengths at all the root levels (P>.05); all other groups had a significant decrease in bond strength at the middle or apical level (P<.05). The failure aspect was dominantly cohesive at the coronal level of all resin cements (P<.05), whereas it was dominantly adhesive at the apical level.

CONCLUSION

All resin cement groups showed decreases in bond strengths at the middle or apical level except LuA and Uni.     

不同树脂粘固剂对瓷与牙本质粘接强度的比较研究

目的 评价不同种类树脂粘固剂与瓷-牙本质粘接强度的差异,以期为临床提供参考.方法选取无龋坏青年人前磨牙制备牙本质粘接面,铸造直径为3 mm、高为3 mm的圆柱状瓷块(IPS e.max Press)80个,分为A、B、C、D、E 5组.分别选用树脂粘固剂A(Variolink Ⅱ)、B(MultilinkAutomix)、C(Multilink Sprint)、D(Rely X Unicem)和E(BisCem)将瓷块粘固于牙本质粘接面上,每组制成16个试样.37℃水储24 h后每组8个试样直接测试剪切粘接强度,另8个试样进行5000次冷热循环后测试粘接强度,扫描电镜观察粘接面形态.对同种粘固剂冷热循环前后的粘接强度进行双样本t检验.结果冷热循环前A组粘接强度[(22.3±3.9)MPa]最大,B组[(18.1±3.5)MPa]次之,再次为D组[(14.1±2.3)MPa]和E组[(11.7±4.2)MPa],C组[(11.3±3.6)MPa]最小.冷热循环后A组粘接强度[(17.8±2.3)MPa]仍最大,B组[(14.4±3.5)MPa]和D组[(13.2±2.5)MPa]次之,再次为E组[(8.9±3.2)MPa],C组[(7.0±2.4)MPa]最小.与冷热循环前相比,冷热循环后A、B、C 3组粘接强度均下降,差异有统计学意义(P<0.05);D组和E组粘接强度下降不明显(P>0.05).结论以全酸蚀粘接技术为基础的树脂粘固剂的粘接强度大于以自酸蚀粘接技术为基础的树脂粘固剂和自粘接型树脂粘固剂.     

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。     

喷砂处理对二氧化锆陶瓷表面性状及树脂粘接的影响

目的 探讨Al2O3喷砂处理对二氧化锆陶瓷表面粗糙度、元素构成及树脂粘接耐久能力的影响.方法 可切削二氧化锆陶瓷片试件60个经烧结、研磨、清洗后,30个试件表面在0.3 MPa压力下接受50 μm Al2O3颗粒喷砂处理20 s,形成喷砂后试件(另30个不喷砂试件为喷砂前试件).使用激光共聚焦显微镜对喷砂前、后的陶瓷表面粗糙度进行测量.使用X射线能谱仪对喷砂前、后的陶瓷表面元素成分进行定性定量分析.试件分为6组,每组10个:1、2组分别由喷砂前、后试件与常规树脂粘接剂(Duolink)粘接;3、4组分别由喷砂前、后试件分别与含磷酸酯类功能性单体的树脂粘接剂(Panavia F)粘接;5和6组分别由喷砂前、后试件经含磷酸酯类功能性单体的硅烷偶联剂(Clearfil Ceramic Primer)处理后与Panavia F粘接.各组试件分为两个亚组,分别经0、10 000次冷热循环后测量剪切粘接强度.使用单因素方差分析和独立样本t检验进行统计.结果 喷砂后陶瓷表面氧元素原子百分比[(65.03±1.48)%]显著低于喷砂前 [(75.85±1.61)%],锆元素原子百分比[(17.30±1.43)%]显著高于喷砂前[(9.62±0.29)%](P<0.001),同时表面粗糙度高于喷砂前(P<0.001).冷热循环降低了所有组粘接强度(P<0.001),其中1、2组试件在循环过程中全部脱落,3、5组粘接强度[(0.59±0.17)、(0.89±0.84)MPa]显著低于4、6组粘接强度[(14.63±3.03)、(16.64±1.90) MPa],6组粘接强度显著高于4组(P<0.001).所有试件粘接断裂模式均为陶瓷-粘接剂界面断裂.结论 Al2O3喷砂处理在增加二氧化锆陶瓷表面粗糙度和表面积的同时,也增加了表面锆元素的质量和原子百分比,从而提高了二氧化锆陶瓷与含磷酸酯类功能性单体的树脂粘接剂间的化学粘接耐久能力.

Abstract：

Objective To evaluate the effect of Al2O3 particles sandblasting on the surface roughness, element composition and resin bond durability of zirconia ceramic. Methods Sixty 2.5 mm thick computer aided design and computer aided manufacture(CAD/CAM) zirconia ceramic (Vita Inceram YZ) plates were fired, polished and cleaned. Half of polished ceramic plates was sandblasted with 50 μm alumina particles at 0.3 MPa for 20 s. The surface roughness of polished and sandblasted ceramic surface were measured by 3D-laser scanning microscope, and the surface element weight and atom ratio of the ceramic surface were measured by energy disperse spectroscopy(EDS). Then polished and sandblasted ceramic plates were randomized into six groups. In Group 1 and 2 the polished and sandblasted ceramic plates were bonded irrespectively with conventional resin cement(DUOLINK) . In Group 3 and 4 the ceramic plates were bonded with resin cement containing MDP(Panavia F), In Group 5 and 6 the specimens were pretreated with silane coupler acitivated by MDP(Clearfil Ceramic Primer), then bond with Panavia F. The specimens of each test group were then divided into two subgroups, and to received shear test after 0 and 10 000 time thermal cycle. The data was analyzed by one-way ANOVA and independent t test. ResultsComparing with polishing, sandblasting reduced the oxygen atom and weight ratio of zirconia ceramic surface (P<0.001), and increased the zirconium atom and weight ratio (P<0.001), meanwhile increased the surface roughness (P<0.001). The bond strength between ceramic plates and resin cement in all test groups decreased after thermocycling (P<0.001). All specimen in test group 1 and 2 lost bond, and the bond strength of test group 3 and 5[(0.59±0.17), (0.89±0.84) MPa] were significantly lower than that of test group 4 and 6[(14.63±3.03), (16.64±1.90) MPa], and the bond strength of test group 6 were significanlty higher than that of test group 4. Conclusions Sandblasting improves durability of bond between zirconia ceramic and resin cement containing MDP, not only by increasing the roughness and area of ceramic surface, but also by changing its surface element composition to obtain more chemical bond.     

过硼酸钠内漂白对牙本质与树脂粘接强度影响的实验研究

目的比较牙本质经过硼酸钠漂白后在不同时间粘接树脂,其抗剪强度变化及粘接界面的超微形态。方法18颗恒前磨牙随机分为3组。A组为对照组：人工唾液内3周后制备牙本质粘接面,粘接树脂。B组：牙齿漂白3周后制备牙本质粘接面,粘接树脂;C组：牙齿漂白3周,人工唾液内储存2周后制备牙本质粘接面,粘接树脂。电子万能材料实验机测试抗剪粘接强度;扫描电镜观察粘接界面超微形态。结果①抗剪强度测试结果：A组：18.61±3.56MPa;B组：12.10±2.64MPa;C组：16.78±2.84MPa。②统计学分析：单因素方差分析表明三组样本均数之间存在统计学差异（P〈0.05）。各样本均数的两两比较（SNK-q法）结果显示A与B组,B与C组的抗剪强度值差别有统计学意义（P〈0.05）,而A与C组的抗剪强度值之间无统计学差异（P〉0.05）。③粘接界面的SEM观察结果：A组粘接界面上可见大量的树脂突渗入牙本质小管内,树脂突的长度较长并且均匀。B组粘接界面上的树脂突稀少,长度较短并且长短不一。C组粘接界面可见有较多的树脂突,长度均匀但较为短小。结论过硼酸钠漂白后牙本质的粘接时间对牙本质与树脂的粘接强度有影响：牙齿漂白后即刻粘接树脂,会降低牙本质与树脂的粘接强度,而漂白后延迟2周再粘接树脂能够恢复牙本质与树脂的粘接强度。