纪振冰,万熠,赵梓贺,于明志,王宏卫,范世缘.水热温度和时间对3D打印Ti-6Al-4V植入体表面理化性能的影响[J].表面技术,2022,51(9):288-299.
JI Zhen-bing,WAN Yi,ZHAO Zi-he,YU Ming-zhi,WANG Hong-wei,FAN Shi-yuan.#$NPEffects of Hydrothermal Temperature and Time on Surface Physical and Chemical Properties of 3D Printed Ti-6Al-4V Implants[J].Surface Technology,2022,51(9):288-299 |
| 水热温度和时间对3D打印Ti-6Al-4V植入体表面理化性能的影响 |
| #$NPEffects of Hydrothermal Temperature and Time on Surface Physical and Chemical Properties of 3D Printed Ti-6Al-4V Implants |
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| DOI：10.16490/j.cnki.issn.1001-3660.2022.09.030 |
| 中文关键词: 3D打印 钛合金 植入体 水热处理 微纳结构 聚多巴胺涂层 |
| 英文关键词:3D printing titanium alloy implant hydrothermal treatment micro-nano structure polydopamine coating |
| 基金项目:国家自然科学基金(51975336);山东省重点研发计划(2020JMRH0202);山东省新旧动能转换重大产业攻关项目(2021-13);济宁市重点研发计划项目(2021DZP005);山东大学教育教学改革研究项目(2022Y133，2022Y124，2022Y312) |
| 作者 | 单位 |
| 纪振冰 | 山东大学 高效洁净机械制造教育部重点实验室 机械工程学院，济南 250061 |
| 万熠 | 山东大学 高效洁净机械制造教育部重点实验室 机械工程学院，济南 250061 |
| 赵梓贺 | 山东大学 高效洁净机械制造教育部重点实验室 机械工程学院，济南 250061 |
| 于明志 | 山东大学 高效洁净机械制造教育部重点实验室 机械工程学院，济南 250061 |
| 王宏卫 | 山东大学齐鲁医院 急诊科 山东大学急危重症临床医学研究中心，济南 250012 |
| 范世缘 | 山东大学 高效洁净机械制造教育部重点实验室 机械工程学院，济南 250061 |
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| Author | Institution |
| JI Zhen-bing | Key Laboratory of Ministry of Education for High-efficiency and Clean Mechanical Manufacture,School of Mechanical Engineering, Shandong University, Jinan 250061, China |
| WAN Yi | Key Laboratory of Ministry of Education for High-efficiency and Clean Mechanical Manufacture,School of Mechanical Engineering, Shandong University, Jinan 250061, China |
| ZHAO Zi-he | Key Laboratory of Ministry of Education for High-efficiency and Clean Mechanical Manufacture,School of Mechanical Engineering, Shandong University, Jinan 250061, China |
| YU Ming-zhi | Key Laboratory of Ministry of Education for High-efficiency and Clean Mechanical Manufacture,School of Mechanical Engineering, Shandong University, Jinan 250061, China |
| WANG Hong-wei | Department of Emergency Medicine, Shandong University Emergency and Critical Care Clinical Medicine Research Center, Qilu Hospital of Shandong University, Jinan 250012, China |
| FAN Shi-yuan | Key Laboratory of Ministry of Education for High-efficiency and Clean Mechanical Manufacture,School of Mechanical Engineering, Shandong University, Jinan 250061, China |
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| 中文摘要: |
| 目的 研究在具有微纳米双级结构的3D打印钛合金植入体表面制备聚多巴胺涂层的最佳工艺及参数。方法 对酸蚀和阳极氧化处理后的3D打印Ti-6Al-4V样品进行水热处理，通过水热法将聚多巴胺添加到样品表面，并分析不同水热温度和时间的处理效果。使用扫描电子显微镜、三维共聚焦激光显微镜、X射线光电子能谱仪、接触角测量仪、电化学工作站对各组样品的表面形貌、粗糙度、元素组成、表面润湿性、耐腐蚀性等进行表征。结果 经过酸蚀和阳极氧化处理后，在3D打印钛合金植入体表面成功制备了微纳米双级结构，表面纳米管的管径为80 nm左右，水热处理后各组表面均可以观察到有涂层附着。样品表面元素分析结果表明，各组样品表面的N/C值均与理论值0.125接近，证明水热处理成功在微纳米结构表面添加了聚多巴胺涂层。随着水热处理温度的升高和时间的延长，纳米管的管径逐渐减小，由80 nm减小至40 nm左右。随着反应时间的延长，样品表面粗糙度逐渐降低，各组粗糙度均保持在4~5 μm，且接触角逐渐减小，酸蚀后的表面接触角为52.1°，阳极氧化后，接触角降低至42.9°。经过水热处理，各组接触角均小于35°，表现出较好的亲水性。相比于酸蚀组和阳极氧化组，水热处理后的各组的耐腐蚀性均得到增强。结论 在基本保留原有微纳米双级结构的前提下，37 ℃的反应温度和24 h的反应时间适用于聚多巴胺在钛合金植入体表面的沉积。研究结果为聚多巴胺在钛合金植入体表面自聚合的工艺参数优化提供了参考。 |
| 英文摘要: |
| This study aims to explore the optimal process and parameters for preparing polydopamine coating on the surface of 3D printed Ti-6Al-4V implants with micro-nano structure. 3D printing is a promising method for preparing Ti-6Al-4V implants. However, the biological inertness of 3D-printed titanium alloys limits their ability to bind to bone tissue. The micro-nano structure on the surface of titanium alloy implants can promote cell adhesion, proliferation and bone integration. In addition, polydopamine has been shown to promote cell proliferation and reduce cytotoxicity. Therefore, hydrothermal treatment was performed on the 3D printed Ti-6Al-4V implants treated by acid etching and anodic oxidation, and polydopamine was coated on the surface of samples by hydrothermal treatment. The effects of different hydrothermal treatment temperatures and time were analyzed. Moreover, the surface morphology, roughness, elemental composition, surface wettability and corrosion resistance of each sample were characterized by scanning electron microscope, three-dimensional confocal laser microscope, X-ray photoelectron spectroscopy, contact angle measurement instrument and electrochemical workstation. The results showed that a micron-scale pit structure was constructed on the surface by acid etching. Through anodic oxidation, an ordered array of TiO2 nanotubes with a diameter of about 80 nm was constructed on the basis of the original micron-scale structure. Micro-nano structures were successfully prepared on the surface of the implant. With the increase of hydrothermal treatment temperature and time, the diameter of nanotubes gradually decreased from 80 nm to about 40 nm, and even blocked. The three-dimensional topography indicated that the traces of laser scanning during the printing process could be observed on the surface of samples. Through anodic oxidation, the edges and corners became smoother than the surface after acid etching. Going forward, the results of surface element analysis suggested that the N/C value of each sample was close to the theoretical value of 0.125, indicating that the hydrothermal treatment successfully coated polydopamine on the surface based on remaining the micro-nano structure. The carbon and nitrogen elements on the surface of samples after hydrothermal treatment were subjected to peak fitting processing. In addition, the carbon elements were composed of C==O/O—C==O and C—C/C==C, and the nitrogen elements were composed of pyrrolic N, further demonstrating that the hydrothermal treatment successfully added polydopamine to the sample surface. With the increase of reaction time, the surface roughness and contact angle gradually decreased, and the roughness of each group remained between 4-5 μm. The surface contact angle after acid etching was 52.1°. After anodic oxidation, the contact angle decreased to 42.9°. Through hydrothermal treatment, the contact angle was less than 35°, showing excellent hydrophilicity. Compared with the samples after acid etching and anodic oxidation, the corrosion resistance was enhanced through hydrothermal treatment. In addition, the principles of anodic oxidation and dopamine polymerization were discussed in depth. In conclusion, the reaction temperature of 37 ℃ and the reaction time of 24 hours were suitable for the deposition of polydopamine on the surface of titanium alloy implants under the premise that the original micro-nano structure was basically retained. Furthermore, the results of this study provide a reference for the optimization of process parameters of polydopamine self-polymerization on the surface of titanium alloy implants. |
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