目的 提高聚醚醚酮（PEEK）作为骨科植入材料的骨整合能力与生物相容性。方法 采用紫外激光加工技术,在PEEK表面构建了不同中心距的正交微织构,通过对比抛光表面与四种织构参数组试样的表面粗糙度、羟基磷灰石矿化能力及成骨细胞活性,揭示了微织构形貌与生物响应之间的构效关系。结果 织构中心距对表面粗糙度（Ra）调控具有显著的规律性：随中心距从100 μm增至400 μm,表面粗糙度由8.23 μm渐降至3.05 μm,呈准线性衰减趋势。通过模拟体液浸泡实验发现,300 μm中心距组试样表面羟基磷灰石沉积能力呈现最优状态,其矿化层连续且结晶颗粒显著聚集。细胞实验显示,所有试样RGR值均>90%,毒性等级为0级,表明激光加工PEEK未引入生物危害性副产物。通过对比发现,300 μm中心距的正交织构接触角为最小值62.020°,亲水性提升最大,对成骨细胞行为的正向调控最为显著,培养72 h细胞增殖活性达到无织构表面的3.2倍,显微观察细胞伪足沿织构沟槽定向延伸,体现出典型的接触诱导生长特征。结论 激光加工的正交织构可通过调控表面形貌显著改善PEEK材料的骨整合能力与生物相容性,且中心距为300 μm的正交织表现最佳。
Abstract
Poly ether ether ketone (PEEK), a high-molecular polymer material, has an elastic modulus more similar to that of human cortical bones, which can minimize stress shielding. However, due to its inherent biological inertness, the bone integration ability and biocompatibility of PEEK need to be improved. In this study, orthogonal micro-textures with different center distances were fabricated on the surface of PEEK with ultraviolet laser processing technology to enhance the bone integration ability and biocompatibility of PEEK. After preliminary mechanical property tests, the PEEK samples were polished and ground. Orthogonal micro-textures with center distances of 100 μm, 200 μm, 300 μm, and 400 μm were fabricated on PEEK materials with dimensions of 10 mm×10 mm×10 mm by an ultraviolet laser processor with an output power of 1.4 W, a scanning speed of 80 mm/s, and a scanning frequency of 90 kHz. After successful fabrication of the orthogonal micro-textures with different center distances, the roughness before and after processing was compared. Then, the samples were immersed in simulated body fluid, maintained in a constant temperature water bath, and the simulated body fluid was replaced every 24 hours. After 14 days of immersion, the samples were taken out, dried, and immediately characterized for the deposition of hydroxyapatite on the surface. After pretreatment, XRD and scanning electron microscopy were used for phase analysis and imaging in a constant temperature and humidity environment, with a focus on medical PEEK materials. Before biocompatibility analysis, cytotoxicity tests were performed on the laser-processed PEEK materials which were then compared with the original PEEK materials. With simulated body fluid as the measurement medium, after ultrasonic cleaning and vacuum drying, the contact angle measurement instrument was set to a droplet volume of 2 μL, a droplet deposition speed of 0.2 μL/ms, and a balance time of 30 seconds. Each group was repeated three times. The PEEK materials with different center distances were prepared into 1 mm thin slices, with three samples in each group. Then, they were ultrasonically cleaned for 10 minutes, sterilized with ultraviolet light, and finally sealed and stored in anhydrous ethanol to ensure a sterile state. The frozen MC3T3-E1 cells were thawed in a 37 °C constant temperature water bath and then cultured in DMEM high-glucose medium (10% fetal bovine serum, 1% penicillin/streptomycin) in a constant temperature incubator (5% CO2, 37 °C). After digestion and centrifugation of the MC3T3-E1 cells with trypsin, they were diluted and cultured at a constant temperature. Upon the completion of the treatment, the live and dead cells were stained, and the cell adhesion was observed under an inverted fluorescence microscope to quantitatively analyze the cell proliferation. The center distance of the texture had a significant regularity in regulating the surface roughness (Ra): as the center distance increased from 100 μm to 400 μm, the surface roughness gradually decreased from 8.23 μm to 3.05 μm, showing a quasi-linear attenuation trend. Through the simulated body fluid immersion experiment, it was found that the 300 μm center distance group had the best hydroxyapatite deposition ability on the surface, with a continuous mineralization layer and significantly aggregated crystalline particles. The cell experiments showed that the RGR values of all samples were greater than 90%, and the toxicity grade was 0, indicating that the laser-processed PEEK did not introduce biologically harmful by-products. Through comparison, it was found that the contact angle of the 300 μm center distance orthogonal micro-texture was the minimum value of 62.020°, with the greatest improvement in hydrophilicity and the most significant positive regulation of osteoblast behavior. The proliferation activity of cells after 72 hours of culture reached 3.2 times that of the non-textured surface. Microscopic observation showed that the cell pseudopodia extended along the texture grooves in a directional manner, demonstrating typical contact-induced growth characteristics. The laser-processed orthogonal micro-textures can significantly improve the bone integration ability and biocompatibility of PEEK materials by regulating the surface morphology, and the 300 μm center distance orthogonal micro-texture performs the best.
关键词
聚醚醚酮（PEEK） /
生物相容性 /
激光加工 /
微织构 /
表面粗糙度 /
成骨细胞
Key words
poly ether ether ketone (PEEK) /
biocompatibility /
laser processing /
micro-texture /
surface roughness /
osteoblast
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基金
山东省自然科学基金（ZR2023ME077,ZR2023MC140）; 济南大学2024年学科交叉会聚建设项目（XKJC-202406）
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