Department of Endodontics, Jiangsu Key Laboratory of Oral Diseases, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing, China.
Department of Prosthodontics, Jiangsu Key Laboratory of Oral Diseases, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing, China.
J Mech Behav Biomed Mater. 2019 Feb;90:417-425. doi: 10.1016/j.jmbbm.2018.10.034. Epub 2018 Nov 2.
Nanocomposite ceramics have been widely used in clinical practice; however, a standard, recommended bonding protocol has not been determined yet. The present study aimed to evaluate application of tribochemical silica coating or multipurpose products on bonding performance of a CAD/CAM resin-based material (known as nanocomposite ceramic).
Nanocomposite ceramic specimens were fabricated and assigned into 11 groups to build bonded specimens (n = 15) according to surface treatments (none; air particle abrasion with 50-μm alumina followed by application of a silane coupling agent or a universal adhesive; tribochemical silica coating followed by application of a silane coupling agent or a universal adhesive) and resin luting cements (conventional resin cement, RelyX Veneer; self-adhesive resin cement RelyX Unicem) used. Micro-shear bond strength (μ-SBS) was measured after 24-h water storage or ageing with 10,000 thermocycles plus additional 90-d water storage. Surface roughness after alumina air abrasion and tribochemical silica coating were determined using a profilometer. Surface morphology and element variation were observed by using a scanning electron microscope (SEM)/energy dispersion spectrum (EDS). X-ray photoelectron spectroscopy (XPS) was used to characterize nanocomposite ceramic powders conditioned with silane coupling agent or the universal adhesive used in the μ-SBS test. The nanocomposite ceramic plates received alumina air abrasion, tribochemical silica coating, or without, were determined using X-ray diffraction (XRD).
Nanocomposite ceramic treated with alumina air abrasion achieved the highest surface roughness, followed by those treated with tribochemical silica coating. Newly formed Si-O-Si bonds on the nanocomposite ceramic surface were detected by XPS after treatment with silane coupling agent or universal adhesive, and a Zr-O-P bond was detected after treating with universal adhesive. μ-SBS was significantly affected by bond strategies and ageing. Ageing by thermocycling and water storage significantly decreased μ-SBS. μ-SBS values derived by use of a universal adhesive or self-adhesive resin cement alone were no lower than the values derived by use of a silane coupling agent alone. Pre-silanization further enhanced the bonding improvement of universal adhesive or self-adhesive resin cement. However, tribochemical silica coating failed to provide higher μ-SBS compared with alumina air abrasion. XRD detected no monoclinic zirconia phase after alumina air abrasion or tribochemical silica coating, suggesting that these two roughening methods did not lead to phase transformation of zirconia fillers.
Combination of presilanization and universal adhesives improve resin bonding of nanocomposite ceramics. Tribochemical silica coating is not superior to alumina air abrasion for pretreated nanocomposite ceramics.
纳米复合陶瓷已广泛应用于临床实践中,但尚未确定标准的推荐粘接方案。本研究旨在评估在 CAD/CAM 树脂基材料(纳米复合陶瓷)的粘接性能上应用化学机械硅涂层或多用途产品。
制作纳米复合陶瓷标本,并根据表面处理(无处理;用 50-μm 氧化铝进行空气粒子喷砂处理,然后应用硅烷偶联剂或通用胶粘剂;化学机械硅涂层处理,然后应用硅烷偶联剂或通用胶粘剂)和使用的树脂水门汀(传统树脂水门汀 RelyX Veneer;自粘接树脂水门汀 RelyX Unicem)将纳米复合陶瓷标本分为 11 组,以制作粘结标本(n=15)。在 24 小时水储存或 10000 次热循环加 90 天水储存后的老化后,测量微剪切结合强度(μ-SBS)。使用轮廓仪测定氧化铝空气喷砂和化学机械硅涂层后的表面粗糙度。使用扫描电子显微镜(SEM)/能谱(EDS)观察表面形貌和元素变化。使用 X 射线光电子能谱(XPS)对硅烷偶联剂或用于 μ-SBS 测试的通用胶粘剂处理的纳米复合陶瓷粉末进行特性分析。使用 X 射线衍射(XRD)对纳米复合陶瓷板进行氧化铝空气喷砂、化学机械硅涂层处理或无处理的检测。
经过氧化铝空气喷砂处理的纳米复合陶瓷的表面粗糙度最高,其次是经过化学机械硅涂层处理的纳米复合陶瓷。经过硅烷偶联剂或通用胶粘剂处理后,XPS 检测到纳米复合陶瓷表面形成了新的 Si-O-Si 键,而经过通用胶粘剂处理后则检测到 Zr-O-P 键。粘结策略和老化对 μ-SBS 有显著影响。热循环和水储存老化显著降低了 μ-SBS。单独使用通用胶粘剂或自粘接树脂水门汀获得的 μ-SBS 值不低于单独使用硅烷偶联剂获得的 μ-SBS 值。预硅烷化进一步增强了通用胶粘剂或自粘接树脂水门汀的粘结改善效果。然而,化学机械硅涂层与氧化铝空气喷砂相比,未能提供更高的 μ-SBS。XRD 检测到氧化铝空气喷砂或化学机械硅涂层后没有发现单斜氧化锆相,表明这两种粗糙化方法不会导致氧化锆填料的相转变。
预硅烷化和通用胶粘剂的组合可改善纳米复合陶瓷的树脂粘结性能。化学机械硅涂层预处理纳米复合陶瓷的效果不如氧化铝空气喷砂。