磷酸八钙/聚多巴胺涂层在钛表面的构筑及生物相容性检测

刘梦玉; 魏祥; 林丹; 李尧; 徐纯峰; 魏凌飞; 于德栋

doi:10.16490/j.cnki.issn.1001-3660.2025.18.020

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表面技术 ›› 2025, Vol. 54 ›› Issue (18) : 200-208. DOI: 10.16490/j.cnki.issn.1001-3660.2025.18.020

表面功能化

磷酸八钙/聚多巴胺涂层在钛表面的构筑及生物相容性检测

刘梦玉^1,2,3,4,5, 魏祥^1,2,3,4,5, 林丹⁶, 李尧⁷, 徐纯峰^2,3,4,5, 魏凌飞^8,*, 于德栋^2,3,4,5,9,*

作者信息 +

Fabrication and Biocompatibility Evaluation of Octacalcium Phosphate/ Polydopamine Coating on the Surface of Titanium

LIU Mengyu^1,2,3,4,5, WEI Xiang^1,2,3,4,5, LIN Dan⁶, LI Yao⁷, XU Chunfeng^2,3,4,5, WEI Lingfei^8,*, YU Dedong^2,3,4,5,9,*

Author information +

文章历史 +

摘要

目的为提高钛合金的生物活性及其促进骨再生的能力,利用聚多巴胺（PDA）的黏附特性,在3D打印钛片（3D-PT）表面制备了一种磷酸八钙（OCP）陶瓷涂层（OCP/PDA/3D-PT）。方法通过多巴胺氧化自聚合和仿生矿化工艺在3D-PT表面制备OCP/PDA涂层。采用扫描电子显微镜（SEM）、能量色散光谱（EDS）、拉曼光谱、X射线衍射（XRD）、透射电镜（TEM）、选区电子衍射（SAED）、接触角测试和黏附强度实验对涂层的理化特性及亲水性进行检测。同时,将材料与大鼠骨髓间充质干细胞（BMSCs）直接共培养,通过细胞骨架免疫荧光染色观察附着细胞的形态,以及利用CCK-8实验评估细胞增殖活性进而评估所制备涂层的生物相容性。结果 XRD、TEM和SAED结果证实OCP/PDA涂层在3D-PT表面成功制备且与3D-PT牢固结合。接触角测试表明,与3D-PT组相比,OCP/PDA/3D-PT组的亲水性显著提高。黏附强度实验显示,OCP/PDA涂层的附着力达到GB/T9286标准1级。细胞骨架染色和CCK-8实验进一步证明该复合涂层具有良好的生物相容性。结论成功构建了OCP陶瓷涂层与3D-PT基体的强结合界面,并且显著提高了3D-PT表面的亲水性和生物相容性,为其在骨修复领域的进一步应用提供了实验依据。

Abstract

Due to the excellent mechanical properties and biocompatibility, titanium (Ti) and titanium alloys have been extensively utilized in dental implantology for maintaining space where new bone tissue will grow in guided bone generation surgery. However, the limited biological activity of titanium alloys restricts their application in certain clinical settings. To enhance the bioactivity and pro-osteogenic effects of Ti alloys, an octacalcium phosphate (OCP) coating was deposited to the surface of 3D-printed titanium sheets (3D-PTs) with polydopamine (PDA) as an adhesive. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Raman spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), selective area electron diffraction (SAED), and contact angle analysis were employed to evaluate the physicochemical properties and wettability of fabricated coatings. Meanwhile, the interface bonding strength between the OCP/PDA coating and 3D-PTs was evaluated via adhesion strength tests. Additionally, the biocompatibility of the OCP/PDA coating was investigated by culturing rat bone marrow mesenchymal stem cells (BMSCs) on the coating directly, followed by cytoskeleton immunofluorescence staining and CCK-8 assays.
The surface modification protocol initiated with meticulous substrate preparation, involving sequential ultrasonication in acetone, ethanol, and deionized water to eliminate organic contaminants and oxidation layers. Subsequently, the 3D-PTs were immersed in a 2 g/L dopamine solution (pH 8.5) and gently shaken at 57 ℃ for 6 hours to induce spontaneous polymerization, forming a conformal PDA film that served dual purposes as both molecular anchor and mineralization template. Transitioning to the biomimetic phase, the PDA-coated 3D-PTs were immersed in a supersaturated calcium phosphate solution at 37 ℃ for 48 hours for the OCP layer, during which the action of Catechol functional groups directed the epitaxial growth of OCP crystallites. Post-processing protocols ensured material stability through ambient drying and steam sterilization, preparing specimens for comprehensive physicochemical evaluation and biological validation.
Advanced characterization techniques demonstrated successful fabrication of the OCP/PDA coating with robust adhesion to 3D-PTs. Following the preparation of the PDA coating, spherical PDA polymer particles were observed on the 3D-PT surface via SEM. EDS revealed an increased nitrogen (N) peak, and Raman spectroscopy displayed characteristic peaks at 1 350 cm^-1 and 1 580 cm^-1, confirming the successful deposition of PDA on the 3D-PT surface. After the OCP/ PDA coating was prepared, SEM images revealed rhomboid plate-like crystals. EDS analysis indicated new calcium (Ca) and phosphorus (P) peaks with a Ca/P ratio of 1.43. XRD, TEM, and SAED results further demonstrated characteristic peaks corresponding to the (0-10), (002), and (420) crystal planes, collectively confirming the successful formation of OCP. Additionally, contact angle measurements indicated that the OCP/PDA/3D-PT group exhibited significantly enhanced hydrophilicity compared to the 3D-PT group. The adhesion strength of the OCP/PDA coating was classified as level 1 according to the GB/T9286 standard. Furthermore, biological validation experiments substantiated the clinical relevance of these surface modifications. Cytoskeleton immunofluorescence staining and CCK-8 assays demonstrated that the composite coating exhibited excellent biocompatibility. These findings highlight the potentially expanded application of this coating in dental practice, particularly in severe bone defect repair cases. Further investigations will focus on the molecular biological mechanisms of the ceramic composite coating to promote bone regeneration.

导出引用

刘梦玉, 魏祥, 林丹, 李尧, 徐纯峰, 魏凌飞, 于德栋. 磷酸八钙/聚多巴胺涂层在钛表面的构筑及生物相容性检测[J]. 表面技术. 2025, 54(18): 200-208 https://doi.org/10.16490/j.cnki.issn.1001-3660.2025.18.020

LIU Mengyu, WEI Xiang, LIN Dan, LI Yao, XU Chunfeng, WEI Lingfei, YU Dedong. Fabrication and Biocompatibility Evaluation of Octacalcium Phosphate/ Polydopamine Coating on the Surface of Titanium[J]. Surface Technology. 2025, 54(18): 200-208 https://doi.org/10.16490/j.cnki.issn.1001-3660.2025.18.020

中图分类号： TB34

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