李浩,张皓,申孝龙,李栋梁,杨成.医用镁合金表面阳极氧化/茶多酚复合转化层耐腐蚀性能研究[J].表面技术,2023,52(1):196-205.
LI Hao,ZHANG Hao,SHEN Xiao-long,LI Dong-liang,YANG Cheng.Corrosion Resistance of Anodic Oxidation/Polyphenol Conversion Composite Coating on Biomedical Magnesium Alloy[J].Surface Technology,2023,52(1):196-205
医用镁合金表面阳极氧化/茶多酚复合转化层耐腐蚀性能研究
Corrosion Resistance of Anodic Oxidation/Polyphenol Conversion Composite Coating on Biomedical Magnesium Alloy
  
DOI:10.16490/j.cnki.issn.1001-3660.2023.01.020
中文关键词:  镁合金  医用材料  阳极氧化  EGCG  耐腐蚀能力
英文关键词:magnesium alloy  biomedical material  anodic oxidation  EGCG  corrosion resistance
基金项目:国家自然科学基金(52101286);四川省自然科学基金项目(2022NSFSC2011);国家级大学生创新创业训练计划项目(202011360001)
作者单位
李浩 攀枝花学院 钒钛学院 沈阳 110043 
张皓 攀枝花学院 钒钛学院 沈阳 110043 
申孝龙 攀枝花学院 生物与化工学院,四川 攀枝花 610000 
李栋梁 攀枝花学院 钒钛学院 沈阳 110043 
杨成 攀枝花学院 钒钛学院 沈阳 110043 
AuthorInstitution
LI Hao College of Vanadium and Titanium,Sichuan Panzhihua 610000, China 
ZHANG Hao College of Vanadium and Titanium,Sichuan Panzhihua 610000, China 
SHEN Xiao-long College of Biology and Chemical Engineering, Panzhihua University, Sichuan Panzhihua 610000, China 
LI Dong-liang College of Vanadium and Titanium,Sichuan Panzhihua 610000, China 
YANG Cheng College of Vanadium and Titanium,Sichuan Panzhihua 610000, China 
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中文摘要:
      目的 在AZ31镁合金表面制备阳极氧化/茶多酚复合转化层,解决医用镁合金在植入环境中降解过快、易导致炎症等问题。方法 使用阳极氧化法在镁合金表面构建阳极氧化(Anodization)层,之后在阳极氧化层上通过浸泡法制备多酚转化层,得到复合转化层,多酚选择表没食子儿茶素没食子酸酯(EGCG)。通过SEM、EDS、XRD、FTIR和XPS对转化层的表面形貌、成分结构进行分析,利用极化曲线、电化学阻抗谱、长期浸泡试验评价转化层的耐腐蚀行为。结果 阳极氧化层内层致密,外层多孔,主要成分为MgO和MgSiO3。在阳极氧化层表面构建EGCG转化层形成复合层后,外层孔洞被填补,且FTIR图谱中出现了EGCG的特征峰。电化学评价结果显示,与AZ31相比,复合转化层的自腐蚀电流密度降低了约2个数量级,高频容抗弧半径显著增大,等效电路模拟后所得极化电阻(Rp)为179.425 kΩ.cm2,远大于裸材。长期浸泡试验结果显示,复合层可明显控制浸泡过程中溶液pH值的增加,且明显低于其他对照组。浸泡160 h后,表面腐蚀产物最少,具有良好的耐腐蚀性能。结论 采用阳极氧化法和浸泡法在AZ31镁合金表面成功制备了阳极氧化/茶多酚复合层,明显提高了镁基底的耐蚀性能。选用的EGCG来源绿色、价格低廉,且具有抗氧化、抗炎等多重功效,为医用镁合金表面改性提供了一种新方案。
英文摘要:
      Magnesium and its alloys are widely regarded as potentially revolutionary orthopaedic implant materials due to their biodegradability, good biocompatibility and ideal Young's modulus close to that of natural cortical bone. However, the clinical application of magnesium implants is limited by their high reactivity in the physiological environment. Rapid degradation of magnesium alloys in physiological environments can lead to rapid loss of implant mechanical integrity, large amounts of hydrogen, localized alkaline environments, and enrichment of corrosion products. To address these issues and develop clinically viable magnesium-based bone implants, slowing and controlling the biodegradation rate of magnesium- based bone implants is critical. The work aims to prepare an anodic oxidation/polyphenol conversion composite coating on AZ31 Mg alloy surface to solve the problems such as fast degradation and easy to cause inflammation of medical magnesium alloy in implantation environment. In this work, an anodic oxidation/polyphenol conversion composite coating was prepared on AZ31 alloy, and its corrosion resistance and was evaluated. Anodic oxidation (OA) coating was prepared by anodization method, then a polyphenol conversion coating was prepared on the OA coating by immersing in EGCG (epigallocatechin gallate) solution, and finally the OA-EGCG composite conversion coating was obtained. The surface morphology and composition structure of the coating were analyzed by SEM, EDS, XRD, FTIR and XPS. The polarization curve, electrochemical impedance spectroscopy, and long-term immersion test were used to evaluate the corrosion resistance of the composite coating. The results showed that the main components of anodic oxide coating were MgO and MgSiO3. After the EGCG conversion coating constructed, the porous morphology of the AO coating was filled. The characteristic peaks of EGCG appeared in the FTIR spectrum, indicating the successful construction of the OA-EGCG composite coating. The fitting results of XPS high-resolution images of Mg and O elements on the AZ31-AO-EGCG showed that the EGCG was combined on the AZ31-AO surface by conversion to form an AO-EGCG composite coating. The anodic oxide coating acts as an intermediate layer, which can effectively improve the binding force of the EGCG conversion coating to the substrate. Electrochemical evaluation results showed that the corrosion current density of OA-EGCG coating was reduced about 2 orders of magnitude compared with AZ31. The arc radius of the high-frequency capacitive reactance was significantly increased, and the polarization resistance (Rp) obtained after the equivalent circuit simulation was 179.425 kΩ.cm2, which was much larger than that of the AZ31. After immersion for 160 h, the OA-EGCG composite coating could obviously control the increase of pH value of the solution, and significantly lower than other controls. The corrosion products formed on the AZ31-OA-EGCG was the least. The hydrogen evolution results showed that the AZ31 released about 14 mL/cm2 of hydrogen within 160 hours, and the AZ31-AO and AZ31-AO-EGCG sample groups released about 11 mL/cm2 and 6 mL/cm2 of hydrogen, respectively. This result corresponded to the immersion changes in pH. By combining the anodization and the polyphenol conversion coating, the corrosion resistance of the single anodized coating was improved, and the bonding force of the single polyphenol coating was improved.
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