Department of Bone and Joint Surgery, the Second Affiliated Hospital of Xi'an Jiaotong University, Xi'an, China.
State Key Laboratory for Mechanical Behavior of Materials, School of Materials Science and Engineering, Xi'an Jiaotong University, Xi'an, China.
J Biomater Appl. 2020 Sep;35(3):342-352. doi: 10.1177/0885328220935008. Epub 2020 Jun 17.
Polyetheretherketone (PEEK) has been becoming a popular implant material in orthopaedic applications. The lack of bioactivity affects PEEK's long-term lifetime, and appropriate surface modification is an effective way to enhance its bioactivity. Sulfonation of PEEK can endow PEEK with a 3 D porous network surface and improve its bioactivity. This study is aimed at exploring an optimal sulfonation time and a post-treatment method of PEEK sulfonation. PEEK was immersed into concentrated sulfuric acid for different sulfonation times and experienced different post-treatment methods to turn into sulfonated PEEK (SPEEK). The immersion times were 0.5 min (SPEEK0.5), 1 min (SPEEK1), 3 min (SPEEK3), 5 min (SPEEK5) and 7 min (SPEEK7), and the post-treatment methods were acetone rinsing (SPEEK-T1), hydrothermal treatment (SPEEK-T2) and NaOH immersion (SPEEK-T3). Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy, hydrophilic property, ion release and cell viability evaluations were performed to optimize the sulfonation time, and the SEM, EDS, ion release and cell viability were analysed to optimize the post-treatment method. The results showed a porous network structure was formed on all samples of SPEEK, and the porous structure became more obvious and the S concentration increased with increasing sulfonation time. However, too long of an immersion time (SPEEK7) tended to damage the superficial porous structure and left a higher content of sulfuric acid, which could inhibit the growth of MC3T3E1 cells on its surface. In addition, the surface morphology, residual sulfuric acid and cytocompatibility of SPEEK-T1, SPEEK-T2 and SPEEK-T3 were not distinctly different. In conclusion, a 5-min sulfonation time was considered to be the optimal selection, and acetone rinsing, hydrothermal treatment and NaOH immersion showed the same effect in removing the residual sulfuric acid. The understanding of optimal sulfonation time and post-treatment method can provide a theoretical basis in preparing SPEEK for orthopaedic applications.
聚醚醚酮（PEEK）已成为骨科应用中一种流行的植入材料。缺乏生物活性会影响 PEEK 的长期寿命，而适当的表面改性是提高其生物活性的有效方法。PEEK 的磺化可以赋予 PEEK 三维多孔网络表面，并提高其生物活性。本研究旨在探索 PEEK 磺化的最佳磺化时间和后处理方法。将 PEEK 浸入浓硫酸中不同的磺化时间，并经历不同的后处理方法，转化为磺化聚醚醚酮（SPEEK）。浸入时间分别为 0.5 分钟（SPEEK0.5）、1 分钟（SPEEK1）、3 分钟（SPEEK3）、5 分钟（SPEEK5）和 7 分钟（SPEEK7），后处理方法分别为丙酮冲洗（SPEEK-T1）、水热处理（SPEEK-T2）和 NaOH 浸泡（SPEEK-T3）。通过扫描电子显微镜（SEM）、能谱（EDS）、傅里叶变换红外光谱、亲水性能、离子释放和细胞活力评估来优化磺化时间，并通过 SEM、EDS、离子释放和细胞活力分析来优化后处理方法。结果表明，所有 SPEEK 样品均形成了多孔网络结构，随着磺化时间的增加，多孔结构变得更加明显，S 浓度增加。然而，过长的浸入时间（SPEEK7）容易破坏表面多孔结构，并留下更高含量的硫酸，这可能会抑制 MC3T3E1 细胞在其表面的生长。此外，SPEEK-T1、SPEEK-T2 和 SPEEK-T3 的表面形貌、残留硫酸和细胞相容性没有明显差异。总之，5 分钟的磺化时间被认为是最佳选择，而丙酮冲洗、水热处理和 NaOH 浸泡在去除残留硫酸方面效果相同。对最佳磺化时间和后处理方法的理解可为制备用于骨科应用的 SPEEK 提供理论基础。
