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自酸蚀粘结剂的界面结构与粘结强度分析

Analysis of interfacial structure and bond strength of self-etch adhesives.

作者信息

Pinzon Lilliam M, Watanabe Larry G, Reis Andre F, Powers John M, Marshall Sally J, Marshall Grayson W

出版信息

Am J Dent. 2013 Dec;26(6):335-40.

Abstract

PURPOSE

To determine the bond strength, nanoleakage and interfacial morphology of four self-etch adhesives bonded to superficial dentin.

METHODS

Microtensile (MT) (n= 15) and single plane shear (SP) (n= 8) bond tests were performed using human dentin polished through 320-grit SiC paper. Clearfil Protect Bond (PB), Clearfil S3 Bond (S3), Prompt L-Pop (PLP) and G-Bond (GB) were used according to their manufacturers' instructions. Composite was applied as cylinders with a thickness of 4 mm with a 1 mm diameter and stored in water at 370C for 24 hours. Specimens were debonded with a testing machine at a cross-head speed of 1 mm/minute. Means and standard deviations of bond strength were calculated. Data were analyzed using ANOVA. Fisher's PLSD intervals were calculated at the 0.05 level of significance. Failure modes were determined at x100. The hybrid layer was revealed by treatment with 5N HC1/5% NaOCl or fractured perpendicular to the interface and sputter coated with gold. Specimens were viewed at x1,000, x2,500, and x5,000 in a field emission SEM at 15 kV. Teeth (n=2) sectioned into 0.9 mm-thick slabs were immersed in ammoniacal silver nitrate solution for 24 hours, rinsed and immersed in photo-developing solution for 8 hours. Specimens were sectioned (90 nm-thick) and observed under TEM.

RESULTS

Means ranged from 25.0 to 73.1 MPa for MT and from 15.5 to 56.4 MPa for SP. MT values were greater than SP, but were highly correlated (R2 = 0.99, P= 0.003) and provided the same order for the systems studied. Fisher's PLSD intervals (P< 0.05) for bond strength techniques and adhesives results were 1.7 and 2.3 MPa, respectively. Failures sites were mixed. TEM showed that hybrid layers were -0.5 pm for PB, GB and S3 and approximately 5 microm for PLP. SEM showed morphologic differences among adhesives. Silver nitrate deposits were observed within the interfaces for all adhesive systems.

摘要

目的

测定四种自酸蚀粘结剂与表层牙本质粘结的粘结强度、纳米渗漏及界面形态。

方法

使用经320目碳化硅砂纸打磨的人牙本质进行微拉伸(MT)(n = 15)和单平面剪切(SP)(n = 8)粘结试验。根据制造商说明使用Clearfil Protect Bond(PB)、Clearfil S3 Bond(S3)、Prompt L-Pop(PLP)和G-Bond(GB)。将复合材料制成厚度为4 mm、直径为1 mm的圆柱体,在37℃水中储存24小时。用试验机以1 mm/分钟的十字头速度使试件脱粘。计算粘结强度的平均值和标准差。数据采用方差分析进行分析。在0.05显著性水平计算Fisher's PLSD区间。在100倍下确定失效模式。用5N HCl/5%次氯酸钠处理或垂直于界面断裂并溅射镀金来显示混合层。在15 kV的场发射扫描电子显微镜下以1000倍、2500倍和5000倍观察试件。将切成0.9 mm厚薄片的牙齿(n = 2)浸入氨硝酸银溶液中24小时,冲洗后浸入显影液中8小时。将试件切片(90 nm厚)并在透射电子显微镜下观察。

结果

MT的平均值范围为25.0至73.1 MPa, SP的平均值范围为15.5至56.4 MPa。MT值大于SP值,但高度相关(R2 = 0.99,P = 0.003),且为所研究的体系提供了相同的顺序。粘结强度技术和粘结剂结果的Fisher's PLSD区间(P < 0.05)分别为1.7和2.3 MPa。失效部位为混合型。透射电子显微镜显示,PB、GB和S3的混合层约为0.5μm,PLP的混合层约为5μm。扫描电子显微镜显示粘结剂之间存在形态差异。在所有粘结剂体系的界面内均观察到硝酸银沉积。

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