Eliasson S T, Tibballs J, Dahl J E
Oper Dent. 2014 Sep-Oct;39(5):E206-16. doi: 10.2341/12-429-L. Epub 2014 May 7.
To evaluate the effect of surface treatments and bonding systems on the repair bond strength between composite materials after one and 12 months of storage, using an improved microtensile test method.
A total of 72 composite cylinders (Tetric Evo Ceram, Ivoclar) were fabricated, stored in distilled water for two weeks followed by thermal cycling (5000 times between 5°C and 55°C), and served as substrate. The cylinders were mechanically roughened using 320-grit silicon carbide sandpaper, etched with 37% phosphoric acid gel, rinsed with water, and divided equally into three experimental groups: group 1, unchanged surface; group 2, sandblasting of the surface (CoJet tribochemical silica sand, 3M ESPE; Microetcher II, Danville Engineering Inc); and group 3, surface silane coating (Bis-Silane, BISCO Inc). Eight control cylinders were prepared and underwent similar aging as the substrate. Each experimental group was divided into subgroups that received the following bonding systems: one-step self-etching adhesive (AdheSE One, Ivoclar Vivadent), two-step self-etching adhesive (Clearfil SE, Kuraray America), and three-step etch-and-rinse adhesive (Adper Scotchbond Multi-Purpose, 3M ESPE). Fresh composite (Tetric Evo Ceram, Ivoclar) was placed and cured on top of the prepared substrate cylinders. The specimens were placed in distilled water for a week and thermocycled the same way as before. Eight composite control cylinders were also stored and thermocycled for the same period of time. Half of the cylinders in each test group were tested at one month and the second half at 12 months. The cylinders were serially sectioned in an automatic cutting machine, producing 10 to 20 1.1 × 1.1-mm test specimen beam from each cylinder. Specimens were prepared for microtensile testing and the tensile strength calculated based on the force at fracture and specimen dimension. The fracture surfaces were examined under a stereomicroscope and the type of fracture noted.
The mean tensile strength of composite control was 54.5 ± 6.0 MPa at one month and 49.6 ± 5.1 MPa at 12 months. The mean tensile strength for the repaired groups ranged from 26.4 ± 6.8 MPa to 49.9 ± 10.4 MPa at one month and 21.2 ± 9.9 to 41.3 ± 7.5 at 12 months. There was a statistical difference between all groups (p<0.05) at one month. This difference was less pronounced at 12 months. The highest repair strength was obtained in the group having a silane-coated surface and Clearfil, the two-step self-etching adhesive. Clearfil also had the highest repair strength within each surface treatment group. There was a tendency for lower tensile strength at 12 months compared with one month. Most fractures were of the adhesive type; the highest number of cohesive fractures, 16% at one month and 12% at 12 months, were in groups with the highest tensile strength.
The best repair bond strength was achieved by using freshly mixed silane solution on the substrate in addition to an adhesive, rendering a thin bonding layer.
采用改进的微拉伸试验方法,评估表面处理和粘结系统对复合材料在储存1个月和12个月后的修复粘结强度的影响。
共制备72个复合圆柱体(Tetric Evo Ceram,义获嘉),在蒸馏水中储存两周,然后进行热循环(在5°C至55°C之间循环5000次),作为基底。使用320目碳化硅砂纸对圆柱体进行机械粗化处理,用37%磷酸凝胶蚀刻,用水冲洗,然后平均分为三个实验组:第1组,表面不变;第2组,表面喷砂处理(CoJet摩擦化学硅砂,3M ESPE;Microetcher II,丹维尔工程公司);第3组,表面硅烷涂层(双硅烷,BISCO公司)。制备8个对照圆柱体,并与基底进行类似的老化处理。每个实验组再分为接受以下粘结系统的亚组:一步自酸蚀粘结剂(AdheSE One,义获嘉威瓦登特)、两步自酸蚀粘结剂(Clearfil SE,可乐丽美国公司)和三步酸蚀冲洗粘结剂(Adper Scotchbond多功能粘结剂,3M ESPE)。将新鲜的复合材料(Tetric Evo Ceram,义获嘉)放置在制备好的基底圆柱体上并固化。将标本置于蒸馏水中一周,并以与之前相同的方式进行热循环。还制备8个复合对照圆柱体,并在相同时间段内进行储存和热循环。每个测试组的一半圆柱体在1个月时进行测试,另一半在12个月时进行测试。在自动切割机中将圆柱体依次切片,每个圆柱体产生10至20个尺寸为1.×1.1毫米的测试标本梁。制备标本进行微拉伸测试,并根据断裂时的力和标本尺寸计算拉伸强度。在立体显微镜下检查断裂表面并记录断裂类型。
复合对照组在1个月时的平均拉伸强度为54.5±6.0兆帕,在12个月时为49.6±5.1兆帕。修复组在1个月时的平均拉伸强度范围为26.4±6.8兆帕至49.9±10.4兆帕,在12个月时为21.2±9.9至41.3±7.5兆帕。1个月时所有组之间存在统计学差异(p<0.05)。这种差异在12个月时不太明显。在具有硅烷涂层表面并使用两步自酸蚀粘结剂Clearfil的组中获得了最高的修复强度。Clearfil在每个表面处理组中也具有最高的修复强度。与1个月相比,12个月时的拉伸强度有降低的趋势。大多数断裂为粘结型;在拉伸强度最高的组中,粘结断裂的数量最多,1个月时为16%,12个月时为12%。
除了使用粘结剂外,在基底上使用新鲜混合的硅烷溶液可获得最佳的修复粘结强度,形成薄的粘结层。