Lai Szu-Yu, Lin Szu-I, Chang Chia-Wei, Shen Yi-Rou, Mine Yuichi, Lin Zih-Chan, Fang Mei-Ling, Sung Chia-Chih, Tseng Chien-Fu, Peng Tzu-Yu, Lee Chiang-Wen
School of Dentistry, College of Oral Medicine, Taipei Medical University, Taipei 11031, Taiwan.
Department of Dentistry, Taoyuan General Hospital, Ministry of Health and Welfare, Taoyuan 33004, Taiwan.
Polymers (Basel). 2025 May 23;17(11):1448. doi: 10.3390/polym17111448.
Polyaryletherketone (PAEK) materials, including polyetheretherketone (PEEK) and polyetherketoneketone (PEKK), possess excellent mechanical properties and biocompatibility; however, their inherently low surface energy limits effective bonding with resin cements. This study investigated the effects of hydrofluoric acid (HF) etching and handheld nonthermal plasma (HNP) treatment on enhancing the adhesive performance of PAEK surfaces. Disk-shaped PEEK (BP) and PEKK (PK) specimens were divided into four groups: APA (airborne-particle abrasion), PLA (nonthermal plasma treatment), LHF (5.0% HF), and HHF (9.5% HF). Surface characterization was performed using a thermal field emission scanning electron microscope (FE-SEM). Surface wettability was evaluated using contact angle goniometry. Cytotoxicity was evaluated using HGF-1 cells exposed to conditioned media and analyzed via PrestoBlue assays. Shear bond strength (SBS) was measured after three aging conditions-NT (no aging), TC (thermocycling), and HA (highly accelerated aging)-using a light-curing resin cement. Failure modes were categorized, and statistical analysis was performed using one-way and two-way ANOVA with Tukey's HSD test (α = 0.05). Different surface treatments did not affect surface characterization. PLA treatment significantly improved surface wettability, resulting in the lowest contact angles among all groups, followed by HF etching (HHF > LHF), while APA showed the poorest hydrophilicity. Across all treatments, PK exhibited better wettability than BP. Cytotoxicity results confirmed that all surface treatments were nontoxic to HGF-1 cells, indicating favorable biocompatibility. SBS testing demonstrated that PLA-treated specimens achieved the highest and most stable bond strength across all aging conditions. Although HF-treated groups exhibited lower bond strength overall, BP samples treated with HF showed relatively less reduction following aging. Failure mode analysis revealed a shift from mixture and cohesive failures in the NT aging condition to predominantly adhesive failures after TC and HA aging conditions. Notably, the PLA-treated groups retained mixture failure patterns even after aging, suggesting improved interfacial durability. Among the tested methods, PLA treatment was the most effective strategy, enhancing surface wettability, bond strength, and aging resistance without compromising biocompatibility. In summary, the PLA demonstrated the greatest clinical potential for improving the adhesive performance of PAEK when used with light-curing resin cements.
聚芳醚酮（PAEK）材料，包括聚醚醚酮（PEEK）和聚醚酮酮（PEKK），具有优异的机械性能和生物相容性；然而，其固有的低表面能限制了与树脂水门汀的有效粘结。本研究调查了氢氟酸（HF）蚀刻和手持式非热等离子体（HNP）处理对提高PAEK表面粘结性能的影响。将圆盘状的PEEK（BP）和PEKK（PK）试样分为四组：APA（空气颗粒研磨）、PLA（非热等离子体处理）、LHF（5.0%HF）和HHF（9.5%HF）。使用热场发射扫描电子显微镜（FE-SEM）进行表面表征。使用接触角测量法评估表面润湿性。使用暴露于条件培养基中的HGF-1细胞评估细胞毒性，并通过PrestoBlue测定法进行分析。使用光固化树脂水门汀在三种老化条件下——NT（未老化）、TC（热循环）和HA（高度加速老化）——测量剪切粘结强度（SBS）。对失效模式进行分类，并使用单因素和双因素方差分析以及Tukey's HSD检验（α=0.05）进行统计分析。不同的表面处理对表面表征没有影响。PLA处理显著改善了表面润湿性，导致所有组中接触角最小，其次是HF蚀刻（HHF>LHF），而APA的亲水性最差。在所有处理中，PK的润湿性均优于BP。细胞毒性结果证实，所有表面处理对HGF-1细胞均无毒，表明具有良好的生物相容性。SBS测试表明，PLA处理的试样在所有老化条件下均获得了最高且最稳定的粘结强度。尽管HF处理组的粘结强度总体较低，但HF处理的BP试样在老化后的强度下降相对较小。失效模式分析表明，在NT老化条件下，失效模式从混合和内聚失效转变为TC和HA老化条件后的主要粘结失效。值得注意的是，即使在老化后，PLA处理组仍保持混合失效模式，表明界面耐久性得到改善。在测试的方法中，PLA处理是最有效的策略，可提高表面润湿性、粘结强度和抗老化性，且不影响生物相容性。总之，当与光固化树脂水门汀一起使用时，PLA在改善PAEK粘结性能方面显示出最大的临床潜力。
