牙科氧化铝基陶瓷纳米硅涂层表面改性的研究

目的 探讨溶胶凝胶法制备纳米硅涂层的工艺,评价涂层对牙科氧化铝基陶瓷润湿性的改变,为提高其与树脂的粘接提供实验基础。方法 采用溶胶凝胶法在喷砂的In-Ceram氧化铝基片表面制备硅涂层;原子力显微镜(AFM)观察热处理后涂层凝胶的微观形态;红外光谱(IR)分析热处理前后的凝胶;计算瓷片抛光组、喷砂组、喷砂加纳米硅涂层组油酸接触角的改变。结果 在In-Ceram氧化铝基片表面置得纳米硅涂层,AFM观测显示热处理使纳米氧化硅粒子的直径长大;IR分析可知凝胶经热处理后Si-OH弯曲振动吸收峰消失;喷砂和喷砂加纳米硅涂层组油酸的接触角均小于抛光组(P=0.000,P=0.000),喷砂加纳米硅硅涂层组的接触角最小(P=0.000,P=0.003)。结论 溶胶凝胶法可以在牙科氧化铝基陶瓷表面制备纳米硅涂层;热处理加强了涂层凝胶微结构中的Si-O-Si网络,但会使纳米粒子部分团聚;喷砂能够提高氧化铝基陶瓷的润湿性,纳米硅涂层使润湿性进一步增强。     

硅涂层对牙科氧化铝陶瓷与树脂粘结强度的影响

目的 探讨在牙科氧化铝陶瓷表面进行SiO2水溶胶涂层对陶瓷与树脂粘结强度的影响.方法 32个氧化铝陶瓷试件根据计算机产生的伪随机数字表分为4组,每组8个,采用溶胶-凝胶法在试件表面分别进行20%SiO2水溶胶涂层+硅烷偶联剂(A组)、30%SiO2水溶胶涂层+硅烷偶联剂(B组)、40%溶胶涂层+硅烷偶联剂(C组)和硅烷偶联剂(对照组)处理,应用傅立叶红外光谱、扫描电镜、X射线能谱仪进行分析.制作陶瓷-复合树脂粘结体,剪切法测试各组剪切粘结强度.结果 溶胶-凝胶法可在氧化铝陶瓷试件表面制得纳米硅涂层.热处理后A、B、C 3组试件Si-O-Si反对称伸缩振动吸收峰、对称伸缩振动吸收峰、弯曲振动吸收峰均增强;扫描电镜显示纳米氧化硅粒子分布较均匀,局部粒子产生团聚;试件表面硅元素含量均明显增加.A、B、C组试件与树脂的剪切粘结强度分别为(3.196±0.171)Mpa、(4.852±0.178)Mpa、(3.576±0.671)Mpa,与对照组[(1.881±0.156)Mpa]相比,差异均有统计学意义(P＜0.05);B组的剪切粘结强度与A、C组相比,差异有统计学意义(P＜0.05).结论 3种浓度硅溶胶可在牙科氧化铝陶瓷表面制得纳米硅涂层.纳米硅涂层可显著提高氧化铝陶瓷与树脂的剪切粘结强度.其中30%浓度SiO2水溶胶制备的硅涂层提高剪切粘结强度的效果最明显.     

硅涂层溶胶-凝胶法制备过程中碳酸氢钠促凝对氧化锆陶瓷粘接强度的影响

目的 探讨硅涂层溶胶-凝胶法制备过程中碳酸氢钠(NaHCO3)促凝对氧化锆陶瓷粘接强度的影响,为溶胶-凝胶法制备硅涂层的临床应用提供实验依据.方法 对比掺杂质量分数为1％、3％、5％、7％、10％的NaHCO3后氧化硅溶胶的胶凝时间,选取胶凝时间最短者进行后续实验.制作5组氧化锆-复合树脂粘接试件,A组:氧化铝喷砂;B组:氧化铝喷砂+摩擦化学法制备硅涂层+硅烷化;C组:氧化铝喷砂+溶胶-凝胶法制备硅涂层+硅烷化;D组:氧化铝喷砂+溶胶-凝胶法制备硅涂层过程中使用NaHCO3促凝+硅烷化;E组:氧化铝喷砂+氧化锆涂底剂处理.测试5组试件抗剪切强度,即粘接强度.结果 掺杂10％的NaHCO3后氧化硅溶胶的胶凝时间最短.B、C、D、E组粘接强度[分别为(10.24±2.78)、(7.36±1.59)、(9.79±2.07)、(8.39 ±0.49) MPa]均比A组[(4.12±0.52) MPa]显著提高,C和D组间差异无统计学意义(P＞0.01).结论 掺杂NaHCO3后氧化硅溶胶的胶凝时间缩短,涂层制备过程中使用NaHCO3促凝不影响氧化锆陶瓷的粘接强度.     

纳米硅涂层对Cercon氧化锆陶瓷与牙本质黏结强度的影响

目的:探讨利用溶胶凝胶法进行纳米硅涂层表面处理对Cercon氧化锆陶瓷黏结强度的影响.方法:将烧结后的氧化锆陶瓷分为4组,每组16片,分别采用4种方式(空白对照、喷砂、喷砂+硅烷偶联剂、喷砂+纳米硅涂层+硅烷偶联剂)处理氧化锆陶瓷片表面,并通过树脂黏结剂与牙本质黏结,在水浴24h后测试其黏结剪切强度.采用SAS6.12软件包对数据进行方差分析,用扫描电镜观察处理后的陶瓷表明形貌.结果:喷砂+纳米硅涂层+硅烷偶联剂表面处理的氧化锆陶瓷的黏结强度最高,与其他各组黏结剪切强度的差别均有显著性(P=0.000):喷砂+硅烷偶联剂组与喷砂组之间差别无统计学意义(P=0.827);喷砂+硅烷偶联剂组和喷砂组与空白组比较均有统计学意义(P=0.001).结论:通过溶胶凝胶法在喷砂后的陶瓷表面制备纳米硅涂层配合使用硅烷偶联剂.可以显著提高Cercon氧化锆陶瓷的黏结强度.     

溶胶凝胶自组装法硅涂层对氧化锆陶瓷与树脂短期粘结强度的影响

目的　评价溶胶凝胶自组装法硅涂层对氧化锆陶瓷与树脂短期粘结强度的影响。方法　加工56 个氧化锆瓷块并随机分为4 组,分别对粘结面进行以下处理：A组：硅烷偶联剂;B组：溶胶凝胶浸涂1层硅涂层+硅烷偶联剂;C组：溶胶凝胶自组装2层硅涂层+硅烷偶联剂;D组：溶胶凝胶自组装3层硅涂层+硅烷偶联剂。制作56 枚光固化复合树脂圆柱并用树脂水门汀粘结于预处理后的氧化锆瓷块上,水浴24 h 后测试剪切粘结强度。以扫描电镜和表面能谱分析对不同表面处理的氧化锆进行表征分析,体视显微镜记录样品断裂模式。结果　A组到D组各组剪切粘结强度值分别为（3.05±0.26）MPa,（6.83±0.33）MPa、（10.51±0.58）MPa和（7.72±0.35）MPa。除B组和D组无统计学差异外,其余各组之间均具有统计学意义(P=0.000)。其中溶胶凝胶自组装2层硅涂层获得的剪切粘结强度值最大。结论　溶胶凝胶自组装法硅涂层可以提高氧化锆陶瓷表面粘结强度,其中溶胶凝胶自组装2层硅涂层组的效果最好。     

疏水性硅涂层对牙科氧化锆陶瓷的表面改性研究

目的：在牙科氧化锆陶瓷表面制备疏水性硅涂层,为提高其与树脂的粘结耐久性提供理论基础。方法：以正硅酸乙酯（tetraethoxysilane,TEOS）为硅源,甲基三甲氧基硅烷（methyltrimethoxysilane,MTMS）为改性剂,通过溶胶-凝胶法在牙科氧化锆陶瓷表面制备硅涂层。扫描电镜观察涂层形貌,X射线能谱分析仪分析涂层前后陶瓷表面结构变化,红外光谱分析疏水改性前后凝胶的化学结构。通过静态接触角测量评价瓷片润湿性的改变。结果：在牙科氧化锆陶瓷表面制得硅涂层。扫描电镜观察涂层致密平整,红外光谱分析证明改性后溶胶疏水基团的加入。硅涂层处理后的氧化锆表面硅元素明显增加。静态接触角测试表明对照组的接触角高于未改性硅涂层（P〈0.01）,而疏水改性后的硅涂层接触角明显高于对照组和未改性硅涂层组（P〈0.01）。结论：通过溶胶-凝胶法在氧化锆表面制备疏水性硅涂层,可以有效降低氧化锆陶瓷表面亲水性,有望在提高氧化锆-树脂界面抗水解能力的同时,增强粘结耐久性。     

牙科氧化锆陶瓷表面不同浓度硅溶胶改性对其粘接强度的影响

目的:探讨氧化锆陶瓷表面不同浓度硅溶胶涂层对其粘接强度的影响.方法:采用溶胶凝胶法用质量浓度分别为20%、30%、40%的硅溶胶在经喷砂的氧化锆陶瓷基片表面制备硅涂层,扫描电镜、X射线能谱仪分析涂层后结构变化.经烧结、抛光、喷砂的32 片氧化锆陶瓷片随机分为4 组,分别采取以下处理:(1)硅烷偶联剂;(2)20%硅溶胶涂层 硅烷偶联剂;(3)30%硅溶胶涂层 硅烷偶联剂;(4)40%硅溶胶涂层 硅烷偶联剂,制作陶瓷/复合树脂粘接体,室温下蒸馏水中放置24 h后,测定陶瓷和树脂的抗剪强度.结果:溶胶凝胶法制得氧化锆陶瓷表面纳米硅涂层.3 种浓度硅溶胶改性后氧化锆陶瓷表面硅元素含量都有明显增加.氧化锆陶瓷表面硅涂层可以提高陶瓷的粘接强度,与单纯硅烷偶联剂组相比差异有统计学意义(P<0.05),其中30%硅溶胶处理组的粘接强度最大为(5.27±0.37) MPa,与20%、40%组相比差异有统计学意义(P<0.05).结论:3 种浓度硅溶胶改性后氧化铝陶瓷表面硅元素含量均有明显增加.纳米硅涂层可以显著提高氧化铝陶瓷表面的粘接强度,30%浓度的硅溶胶效果最好.     

纳米硅涂层对玻璃渗透氧化铝陶瓷抗破裂强度的影响

目的 研究溶胶-凝胶法制备纳米硅涂层对玻璃渗透氧化铝陶瓷粘接后抗破裂强度的影响.方法 将In-Ceram氧化铝瓷片分为A、B、C、D、E组.各组试件均以树脂黏结剂粘于体外牙的牙本质,测试瓷片的抗破裂强度,制作相同试件并行电镜和双能X线吸收光谱分析.结果 5组间差异有统计学意义(P＜0.05),C、D、E组均高于A、B组...     

溶胶-凝胶法制备硅涂层提高牙科高强度陶瓷与复合树脂的粘接强度

目的:探讨溶胶-凝胶法在牙科高强度陶瓷表面改性对陶瓷和复合树脂粘接强度的影响。方法:喷砂玻璃氧化铝陶瓷和氧化锆陶瓷片各72片,每种陶瓷随机分为4组,每组18片,采取以下处理:A组,硅烷偶联剂;B组,20%硅溶胶涂层+硅烷偶联剂;C组,30%硅溶胶涂层+硅烷偶联剂;(D)40%硅溶胶涂层+硅烷偶联剂,制作陶瓷-复合树脂粘接体;每组样本再分为2个亚组,分别在37℃水浴中放置24 h和30 d后,测定陶瓷和树脂的剪切粘接强度。结果:2种陶瓷水浴24 h后,各涂层组粘接强度与单纯硅烷偶联剂组相比差异有统计学意义,其中30%硅溶胶处理组的粘接强度最高(P<0.05)。水浴30 d后,各组粘接强度均和水浴初期(24 h)相比差异无统计学意义,30%硅溶胶处理组的粘接强度最高(P<0.05)。结论:牙科氧化铝陶瓷和氧化锆陶瓷经过溶胶凝胶法纳米硅涂层表面改性结合硅烷偶联剂的处理可以显著提高陶瓷和树脂的粘接强度,并保持较好的粘接耐久性,30%硅溶胶提高粘接强度的效果最好。     

不同人工老化强度对氧化锆陶瓷粘结强度的影响

目的评价氧化锆陶瓷经几种表面处理后在不同强度的人工老化实验条件下的粘结耐久性。方法制备4组氧化锆陶瓷/树脂粘结试件128个,各组试件氧化锆陶瓷按照以下方式处理并使用不同种类的树脂水门汀。组A,摩擦化学法硅涂层+硅烷偶联剂;组B,氧化铝喷砂;组C,氧化铝喷砂+应用氧化锆涂底剂Z-Prime Plus;组D,氧化铝喷砂+应用氧化锆涂底剂Z-Prime Plus。组A和C使用传统Bis-GMA基光固化树脂水门汀,组B和D使用自粘结树脂水门汀。各实验组再分为4个亚组接受不同的人工老化。不接受人工老化(a),水储40 d(b);冷热循环1 200次(c);水储40 d后冷热循环12 000次(d)。测试各组剪切粘结强度值并进行统计学分析。摩擦化学法硅涂层和氧化铝喷砂的氧化锆陶瓷表面以扫描电镜观察并进行能谱分析。结果不论接受或不接受人工老化,4种表面处理间对氧化锆陶瓷的粘结强度值影响无统计学差异。各实验组单独来看,仅有人工老化方式d时粘结强度值都出现了下降,差别具有统计学意义。结论不同人工老化强度对氧化锆陶瓷粘结强度的影响不同。     

Influence of simplified silica coating method on the bonding strength of resin cement to dental alloy

This study evaluated the effectiveness of a simplified silica coating method (CoJet System) on the bonding strength of resin cements to dental alloy. Bonding strength of the specimens treated with metal primer after alumina sandblasting was compared with those treated with silica coating and silane coupling agent after alumina sandblasting. Furthermore, the influence of silane coupling agent on bonding strength was compared between one-liquid and two-liquid silane coupling agents. Measurement of shear bond strength before and after thermal cycling revealed that the group treated with silica coating in one step without alumina sandblasting yielded high bonding strength. As for the influence of silane coupling agent, treatment with two-liquid silane coupling agent achieved higher mean shear bond strength than with one-liquid silane coupling agent. Findings in this study indicated that silicatization by means of this simplified silica coating method was effective in improving the bonding strength to dental alloy.     

The effect of silica coating on the resin bond to the intaglio surface of Procera AllCeram restorations.

OBJECTIVES: This study investigated the influence of a silica-coating method on the resin bond of two different resin composite cements to the intaglio surface of Procera AllCeram densely sintered, high-purity, alumina ceramic restorations after long-term storage and thermocycling. METHOD AND MATERIALS: Densely sintered alumina ceramic specimens were fabricated with the intaglio surface of the Procera AlICeram coping and randomly divided into five adhesive groups (100 total specimens). Resin composite cylinders were bonded either to the untreated or to the tribochemical silica/silane-coated ceramic surface with either a conventional Bis-GMA resin cement or a resin composite containing an adhesive phosphate monomer (Panavia 21) in combination with their corresponding bonding/silane coupling agents. Panavia was also used without silanization to the untreated ceramic surface (control). Subgroups of 10 specimens were stored in distilled water for either 3 (baseline) or 180 days prior to shear bond strength testing. The 180-day samples were subjected to repeated thermocycling for a total of 12,000 cycles. Data were analyzed with one-way analysis of variance and Tukey's multiple comparison. RESULTS: Silica coating significantly increased overall bond strength to Procera AllCeram. RelyX ARC and silica coating revealed the highest bond strength at baseline. Long-term storage and thermocycling significantly decreased overall bond strength. Two groups revealed the significantly highest bond strength values after artificial aging: Panavia 21 with its silane/bonding agent to the original ceramic surface and Panavia 21 to the silica-coated ceramic surface. CONCLUSION: The use of a resin composite containing an adhesive phosphate monomer either in combination with a silane coupling/bonding agent or after tribochemical silica/silane coating revealed the highest long-term shear bond strength to the intaglio surface of Procera AllCeram restorations.     

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。     

Effect of zirconium-oxide ceramic surface treatments on the bond strength to adhesive resin

STATEMENT OF PROBLEM: Surface treatment methods used for resin bonding to conventional silica-based dental ceramics are not reliable for zirconium-oxide ceramics. PURPOSE: The aim of this study was to compare the effects of airborne-particle abrasion, silanization, tribochemical silica coating, and a combination of bonding/silane coupling agent surface treatment methods on the bond strength of zirconium-oxide ceramic to a resin luting agent. MATERIAL AND METHODS: Sixty square-shaped (5 x 5 x 1.5 mm) zirconium-oxide ceramic (Cercon) specimens and composite resin (Z-250) cylinders (3 x 3 mm) were prepared. The ceramic surfaces were airborne-particle abraded with 125-microm aluminum-oxide (Al(2)O(3)) particles and then divided into 6 groups (n = 10) that were subsequently treated as follows: Group C, no treatment (control); Group SIL, silanized with a silane coupling agent (Clearfil Porcelain Bond Activator); Group BSIL, application of the adhesive 10-methacryloyloxydecyl dihydrogen phosphate monomer (MDP)-containing bonding/silane coupling agent mixture (Clearfil Liner Bond 2V/ Porcelain Bond Activator); Group SC, silica coating using 30-microm Al(2)O(3) particles modified by silica (CoJet System); Group SCSIL, silica coating and silanization (CoJet System); and Group SCBSIL, silica coating and application of an MDP-containing bonding/silane coupling agent mixture (Clearfil Liner Bond 2V/Porcelain Bond Activator). The composite resin cylinders were bonded to the treated ceramic surfaces using an adhesive phosphate monomer-containing resin luting agent (Panavia F). After the specimens were stored in distilled water at 37 degrees C for 24 hours, their shear bonding strength was tested using a universal testing machine at a crosshead speed of 0.5 mm/min. Debonded specimen surfaces were examined with a stereomicroscope to assess the mode of failure, and the treated surfaces were observed by scanning electron microscopy. Bond strength data were analyzed using 1-way analysis of variance and the Duncan test (alpha = .05). RESULTS: The bond strengths (mean +/- SD; MPa) in the groups were as follows: Group C, 15.7 +/- 2.9; Group SIL, 16.5 +/- 3.4; Group BSIL, 18.8 +/- 2.8; Group SC, 21.6 +/- 3.6; Group SCSIL, 21.9 +/- 3.9; and Group SCBSIL, 22.9 +/- 3.1. The bond strength was significantly higher in Group SCBSIL than in Groups C, SIL, and BSIL (P<.001), but did not differ significantly from those in Groups SC and SCSIL. Failure modes were primarily adhesive at the interface between zirconium and the resin luting agent in Groups C and SIL, and primarily mixed and cohesive in Groups SC, SCSIL, and SCBSIL. CONCLUSION: Tribochemical silica coating (CoJet System) and the application of an MDP-containing bonding/silane coupling agent mixture increased the shear bond strength between zirconium-oxide ceramic and resin luting agent (Panavia F).     

The influence of internal surface treatments on tensile bond strength for two ceramic systems

STATEMENT OF THE PROBLEM: The ceramic composition and surface microstructure of all-ceramic restorations are important components of an effective bonding substrate. Hydrofluoric acid and sandblasting are well-known procedures for surface treatment; however, surface treatment for high alumina-containing and lithium disilicate ceramics have not been fully investigated. PURPOSE: This in vitro study evaluated the tensile bond strength of resin cement to two types of ceramic systems with different surface treatments. METHODS AND MATERIALS: Thirty specimens of each ceramic system were made according to the manufacturer's instructions and embedded in polyester resin. Specimens of In-Ceram Alumina [I] and IPS Empress 2 [E] were distributed to three groups with differing surface treatments (n = 10): sandblasting with 50 microm aluminum oxide (APA); sandblasting with 110 microm aluminum oxide modified with silica particles (ROCATEC System-RS); a combination of sandblasting with APA and 10% hydrofluoric acid etching (HA) for two minutes on In-Ceram and for 20 seconds for IPS Empress 2. After the respective surface treatments, all the specimens were silanated, and Rely-X resin cement was injected onto the ceramic surface and light polymerized. The specimens were stored in distilled water at 37 degrees C for 24 hours and thermally cycled 1,100 times (5 degrees C/55 degrees C). The tensile bond strength test was performed in a universal testing machine at a 0.5 mm/minute crosshead speed. RESULTS: The mean bond strength values (MPa) for IPS Empress 2 were 12.01 +/- 5.93 (EAPA), 10.34 +/- 1.77 (ERS) and 14.49 +/- 3.04 (EHA). The mean bond strength values for In-Ceram Alumina were 9.87 +/- 2.40 (IAPA) and 20.40 +/- 6.27 (IRS). All In-Ceram specimens treated with 10% hydrofluoric acid failed during thermal cycling. CONCLUSION: The Rocatec system was the most effective surface treatment for In-Ceram Alumina ceramics; whereas, the combination of aluminum oxide sandblasting and hydrofluoric acid etching for 20 seconds worked more effectively for Empress 2 ceramics.     

Bonding polycarbonate brackets to ceramic: effects of substrate treatment on bond strength.

This study evaluated the effects of 5 different surface conditioning methods on the bond strength of polycarbonate brackets bonded to ceramic surfaces with resin based cement. Six disc-shaped ceramic specimens (feldspathic porcelain) with glazed surfaces were used for each group. The specimens were randomly assigned to 1 of the following treatment conditions of the ceramic surface: (1) orthophosphoric acid + primer + bonding agent, (2) hydrofluoric acid gel + primer + bonding agent, (3) tribochemical silica coating (silicon dioxide, 30microm) + silane, (4) airborne particle abrasion (aluminum trioxide, 30microm) + silane, and (5) airborne particle abrasion (aluminum trioxide, 30microm) + silane + bonding agent. Brackets were bonded to the conditioned ceramic specimens with a light-polymerized resin composite. All specimens were stored in water for 1 week at 37 degrees C and then thermocycled (1000 cycles, 5 degrees C to 55 degrees C, 30 seconds). The shear bond strength values were measured on a universal testing machine at a crosshead speed of 1 mm/min. Brackets treated with silica coating with silanization had significantly greater bond strength values (13.6 MPa, P =.01) than brackets treated with orthophosphoric acid (8.5 MPa). There was no significant difference (P =.97) between the bond strengths obtained after airborne abrasion with aluminium trioxide particles followed by silanization (12 MPa) and hydrofluoric acid application (11.2 MPa) (ANOVA and Tukey test). Although brackets conditioned with orthophosphoric acid exhibited only adhesive failures of the luting cement from the ceramic surface, other conditioning methods showed mixed types of failures. Airborne particle abrasion with aluminium trioxide or silica coating followed by silanization gave the most favorable bond strengths. The types of failures observed after debonding indicated that the critical parameter was the strength of the adhesive joint of the luting cement to both the bracket and the ceramic.