<strong>Ti6Al4V</strong>表面微纳结构的制备及生物活性

doi:10.11900/0412.1961.2021.00410

金属学报

2023, Vol. 59

Issue (11): 1466-1474 DOI: 10.11900/0412.1961.2021.00410

本期目录 | 过刊浏览

Ti6Al4V表面微纳结构的制备及生物活性

高晗¹^,²(

), 刘力¹^,², 周笑宇¹^,², 周心怡¹^,², 蔡汶君¹^,², 周泓伶¹^,²

^1.山东大学材料液固结构演变与加工教育部重点实验室济南 250061
^2.山东大学材料科学与工程学院济南 250061

Preparation and Bioactivity of Micro-Nano Structure on Ti6Al4V Surface

GAO Han¹^,²(

), LIU Li¹^,², ZHOU Xiaoyu¹^,², ZHOU Xinyi¹^,², CAI Wenjun¹^,², ZHOU Hongling¹^,²

^1.Key Laboratory for Liquid-Solid Structural Evolution and Processing of Materials, Ministry of Education, Shandong University, Jinan 250061, China
^2.School of Materials Science and Engineering, Shandong University, Jinan 250061, China

引用本文:

高晗, 刘力, 周笑宇, 周心怡, 蔡汶君, 周泓伶. Ti6Al4V表面微纳结构的制备及生物活性[J]. 金属学报, 2023, 59(11): 1466-1474.
Han GAO, Li LIU, Xiaoyu ZHOU, Xinyi ZHOU, Wenjun CAI, Hongling ZHOU. Preparation and Bioactivity of Micro-Nano Structure on Ti6Al4V Surface[J]. Acta Metall Sin, 2023, 59(11): 1466-1474.

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摘要:

基于喷砂酸蚀技术，分别采用(36%~38%)HCl (质量分数)和20%HCl∶30%H₂SO₄ = 1∶1 (体积比)混合酸，同时施加超声场，研究了酸蚀试剂、酸蚀时间和超声场等不同工艺参数对Ti6Al4V合金表面酸洗结构和形貌的影响规律。通过喷砂酸洗+感应加热的复合工艺，实现了Ti6Al4V合金表面微纳米多级结构的制备。结果表明，在一定时间内随酸洗时间的延长，微孔内壁的阶梯结构更加明显，超声可以加速酸蚀；在喷砂酸蚀的表面进行800℃感应加热后，表面得到了微米复合孔+纳米氧化物的多级结构，模拟体液浸泡实验表明得到的微纳米多级结构具有较高的生物活性。

关键词 ： Ti, 表面改性, 酸蚀, 感应加热, 微纳结构

Abstract：

Titanium (Ti) and its alloys have been widely used in the medical field for dental and orthopedic surgeries owing to their excellent mechanical and biological properties. However, much effort has been devoted to the surface modification on Ti-based implants for better biological response in medical applications. Bioactive layers with micro- and nano-scale structures and morphologies can increase the specific surface area of the implants and facilitate rapid osseointegration, which has shown good biological behaviors both in the laboratory and clinical setting. Sandblasting and acid-etching (SLA) technology has become one of the most commonly used surface modification processes for currently marketed dental implants, since it can be easily operated and is efficient. However, studies on etching behavior are still limited. In this study, concentrated hydrochloric acid ((36%-38%)HCl, mass fraction) and mixed diluted acid (20%HCl : 30%H₂SO₄ = 1 : 1, volume fraction) were used to etch Ti6Al4V, and an ultrasonic field was applied to the acid etching treatment. The influence of different etching parameters on the surface structure and morphology of Ti6Al4V was discussed, including the acid etching reagent, acid etching time, and ultrasonic field. Moreover, through the combination of SLA and induction heating treatment (IHT) oxidation, the micro- and nano-scale hierarchical structure was prepared on the surface of Ti6Al4V. The evolution of surface topography, chemistry, roughness, wettability, and bioactivity of the hierarchical structure was discussed. The micro-scale composite pores combing dozens of micron pores and several micron pores were obtained by SLA. Within a certain etching time range, with the prolonging of the etching time, the step structure on the inner wall of the micro-pores becomes more obvious, and ultrasound can accelerate the acid etching. After the IHT at 800^oC, the micro- and nano-scale hierarchical surface with micro-scale composite pores and nanoscale oxide was obtained. Compared with the SLA surface, there was a decrease in surface roughness and an increase in wettability. Furthermore, after soaking in simulated body fluid (SBF) for 14 d, a homogeneous hydroxyapatite (HA) layer was formed on the micro- and nano-scale structured Ti6Al4V surface, suggesting high biological activity of the fabricated structure.

Key words： Ti surface modification acid etching induction heating treatment (IHT) micro- and nano-scale structure

收稿日期: 2021-09-26

ZTFLH:

TG178

基金资助:国家级大学生创新创业训练计划项目(S202010422074)

通讯作者: 高晗，201713597@mail.sdu.edu.cn，主要从事生物医用钛及钛合金表面改性研究

Corresponding author: GAO Han, Tel: 15194105516, E-mail: 201713597@mail.sdu.edu.cn

作者简介: 高晗，女，1995年生，博士生

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图1 Ti6Al4V经喷砂 + (36%~38%)HCl酸洗10、20和30 min后的表面SEM像

图2 Ti6Al4V经喷砂 + 20%HCl∶30%H2SO4 = 1∶1 (体积比)混合酸酸洗60 min后的表面SEM像

图3 Ti6Al4V经SLA + IHT得到的多级结构在模拟体液浸泡14 d前后的XRD谱

图4 Ti6Al4V经SLA + IHT得到的多级结构在模拟体液浸泡14 d前后的SEM像和EDS结果

图5 Ti6Al4V经喷砂+超声酸洗+感应加热后的表面三维形貌及粗糙度定量检测结果

图6 Ti6Al4V经喷砂+超声酸洗+感应加热后的表面水滴形貌图及润湿角

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