Effects of concentrated sulfuric acid etching durations on the shear bond strength between polyether-ketone-ketone and dentin

doi:10.12016/j.issn.2096-1456.2021.03.002

Abstract

Abstract:

Objective To study the effects of different concentrated sulfuric acid etching durations on the shear bond strength between polyether-ketone-ketone (PEKK) and dentin, providing a scientific basis for the clinical bonding procedures of PEKK prosthesis. Methods Forty-four PEKK specimens were prepared and randomly divided into four groups: group A was the control group, which was only polished with abrasive papers, group B, group C and group D were experimental groups, which were etched by 98% concentrated sulfuric acid for 5 s, 30 s and 60 s, respectively. In addition, one sample was randomly selected from each group, and the profile was prepared by a slow cutting machine. The surface morphology of the profile was observed under SEM. After the four groups of specimens and dentin were bonded by resin, they were soaked in distilled water at 37 ℃ for 24 h. After the shear bonding strengths were measured, the fracture interfaces of the specimens were examined by the scanning electron microscopy and stereomicroscopy, and failure models of bonding were analyzed. Results After acid etching treatments, the cross-sectional images in group B presented uniform spongy shapes, while the cross-sectional images in group C and group D showed destructive pore structures. The shear bond strengths of group B (16.84 ± 1.84) MPa, group C (12.33 ± 1.22) MPa and group D (6.44 ± 1.18) MPa were higher than that of group A (3.99 ± 1.06) MPa (P < 0.05). The highest shear bond strength was observed in group B (16.84 ± 1.84) MPa. Conclusion The surface treatment of 98% sulfuric acid etching for 5 s manifested the best bond strength between PEKK and dentin.

Key words: polyether-ketone-ketone, surface treatment, dentin, bonding, primer, RelyX^TM Ultimate, shear bond strength, scanning electron microscope

摘要：

目的研究浓硫酸酸蚀聚醚酮酮（polyether-ketone-ketone,PEKK）不同时间对其与牙本质剪切粘接强度的影响,为临床使用PEKK修复体的粘接操作提供科学依据。方法制备PEKK试件44个,随机平均分为A、B、C、D 4组：A组为对照组,仅用水磨砂纸打磨;B组、C组、D组为实验组,分别用98%浓硫酸酸蚀经打磨试件表面5 s、30 s、60 s。另外,每组随机抽取1个试件用慢速切割机制备出剖面,在扫描电镜下观察其剖面的表面形貌。4组试件与牙本质通过树脂粘接后在37 ℃蒸馏水浸泡24 h,测量剪切粘接强度后统计分析,通过扫描电子显微镜与体视显微镜检查试件断裂界面,统计粘接失败类型。结果 B组PEKK试件酸蚀处理后剖面呈海绵状且孔隙大小均匀,C组、D组可见试件剖面有破坏状孔蚀样结构;剪切粘接强度B组（16.84 ± 1.84） MPa、C组（12.33 ± 1.22） MPa和D组（6.44 ± 1.18） MPa均大于A组（3.99 ± 1.06） MPa（P<0.05）,其中B组与牙本质的剪切粘接强度最高（16.84 ± 1.84） MPa。结论采用98%浓硫酸酸蚀PEKK表面5 s处理方法可以使PEKK与牙本质获得较好的剪切粘接强度。

关键词: 聚醚酮酮, 表面处理, 牙本质, 粘接, 底涂剂, RelyX^TM Ultimate, 剪切粘接强度, 扫描电镜

WANG Chenwei,SUN Fangfang,YANG Chuncheng,DING Ling,CHEN Xi,ZHANG Jiaqi,WU Guofeng. Effects of concentrated sulfuric acid etching durations on the shear bond strength between polyether-ketone-ketone and dentin[J]. Journal of Prevention and Treatment for Stomatological Diseases, 2021, 29(3): 151-156.

王琛玮,孙方方,杨春成,丁玲,陈晞,张嘉琪,吴国锋. 浓硫酸酸蚀聚醚酮酮的时间对其与牙本质剪切粘接强度的影响[J]. 口腔疾病防治, 2021, 29(3): 151-156.

Figures/Tables 4

Figure 1 Cross-sectional scanning electron microscopy images of PEKK after different concentrated sulfuric acid etching durations a: A group, there is no pore structure in the section, the cutting lines are clear and regular, and the whole is relatively flat; b: B group, the section has a spongy structure, and pore size is uniform; c: C group, pore size is not uniform, the number of pores decreases gradually, and a small amount of porous collapse occurs; d: D group, large amount of disintegration exists in the pore; A: control group, no etching treatment with concentrated sulfuric acid; B: etched by 98% concentrated sulfuric acid for 5 s; C: etched by 98% concentrated sulfuric acid for 30 s; D: etched by 98% concentrated sulfuric acid for 60 s; PEKK: polyether-ketone-ketone

Figure 2 Comparison of shear bond strengths between PEKK and dentin after different concentrated sulfuric acid etching durations *: vs. A group, P<0.05; A: control group, no etching treatment with concentrated sulfuric acid; B: etched by 98% concentrated sulfuric acid for 5 s; C: etched by 98% concentrated sulfuric acid for 30 s; D: etched by 98% concentrated sulfuric acid for 60 s; PEKK: polyether-ketone-ketone

Table 1 The bonding failure types after different concentrated sulfuric acid etching durations

Groups	Adhesive cement/PEKK	Cohesive in PEKK	Mixed
A	10	0	0
B	0	1	9
C	4	0	6
D	8	0	2

Figure 3 Scanning electron microscopy images of bonding failure types after different concentrated sulfuric acid etching durations a: A group, the fracture surface is relatively flat without residual attachment; b: B group, the fracture surface is protruding with a large amount of residual attachments; c: C group, the fracture surface is slightly depressed and has a large number of corrosion-like structures; d: D group, the fracture surface is slightly depressed and has a large number of corrosion-like structures, the surface has less residual attachment than that of group C; A: control group, no etching treatment with concentrated sulfuric acid; B: etched by 98% concentrated sulfuric acid for 5 s; C: etched by 98% concentrated sulfuric acid for 30 s; D: etched by 98% concentrated sulfuric acid for 60 s; PEKK: polyether-ketone-ketone

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