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通过等径角挤压和微弧氧化工艺改善纯钛的生物学和力学性能

Improving Pure Titanium's Biological and Mechanical Characteristics through ECAP and Micro-Arc Oxidation Processes.

作者信息

Alemayehu Dawit Bogale, Todoh Masahiro, Hsieh Jang-Hsing, Li Chuan, Huang Song-Jeng

机构信息

Division of Human Mechanical Systems and Design, Graduate School of Engineering, Hokkaido University, Sapporo 060-8628, Japan.

Division of Mechanical and Aerospace Engineering, Faculty of Engineering, Hokkaido University, Sapporo 060-8628, Japan.

出版信息

Micromachines (Basel). 2023 Jul 31;14(8):1541. doi: 10.3390/mi14081541.

DOI:10.3390/mi14081541
PMID:37630077
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC10456902/
Abstract

Pure titanium is limited to be used in biomedical applications due to its lower mechanical strength compared to its alloy counterpart. To enhance its properties and improve medical implants feasibility, advancements in titanium processing technologies are necessary. One such technique is equal-channel angular pressing (ECAP) for its severe plastic deformation (SPD). This study aims to surface modify commercially pure titanium using micro-arc oxidation (MAO) or plasma electrolytic oxidation (PEO) technologies, and mineral solutions containing Ca and P. The composition, metallography, and shape of the changed surface were characterized using X-ray diffraction (XRD), digital optical microscopy (OM), and scanning electron microscope (SEM), respectively. A microhardness test is conducted to assess each sample's mechanical strength. The weight % of Ca and P in the coating was determined using energy dispersive spectroscopy (EDS), and the corrosion resistance was evaluated through potentiodynamic measurement. The behavior of human dental pulp cell and periodontal cell behavior was also studied through a biomedical experiment over a period of 1-, 3-, and 7-days using culture medium, and the cell death and viability can be inferred with the help of enzyme-linked immunosorbent assay (ELISA) since it can detect proteins or biomarkers secreted by cells undergoing apoptosis or necrosis. This study shows that the mechanical grain refinement method and surface modification might improve the mechanical and biomechanical properties of commercially pure (CP) titanium. According to the results of the corrosion loss measurements, 2PassMAO had the lowest corrosion rate, which is determined to be 0.495 mmpy. The electrode potentials for the 1-pass and 2-pass coated samples are 1.44 V and 1.47 V, respectively. This suggests that the coating is highly effective in reducing the corrosion rate of the metallic CP Ti sample. Changes in the grain size and the presence of a high number of grain boundaries have a significant impact on the corrosion resistance of CP Ti. For ECAPED and surface-modified titanium samples in a 3.6% NaCl electrolyte solution, electrochemical impedance spectroscopy (EIS) properties are similar to Nyquist and Bode plot fitting. In light of ISO 10993-5 guidelines for assessing in vitro cytotoxicity, this study contributes valuable insights into pulp and periodontal cell behavior, focusing specifically on material cytotoxicity, a critical factor determined by a 30% decrease in cell viability.

摘要

由于纯钛与钛合金相比机械强度较低,其在生物医学应用中的使用受到限制。为了提高其性能并改善医用植入物的可行性,钛加工技术的进步是必要的。等通道转角挤压(ECAP)就是这样一种因其严重塑性变形(SPD)而采用的技术。本研究旨在使用微弧氧化(MAO)或等离子体电解氧化(PEO)技术以及含Ca和P的矿物溶液对商业纯钛进行表面改性。分别使用X射线衍射(XRD)、数字光学显微镜(OM)和扫描电子显微镜(SEM)对改性表面的成分、金相组织和形状进行了表征。进行了显微硬度测试以评估每个样品的机械强度。使用能谱仪(EDS)测定涂层中Ca和P的重量百分比,并通过动电位测量评估耐腐蚀性。还通过使用培养基进行为期1天、3天和7天的生物医学实验研究了人牙髓细胞和牙周细胞的行为,并且由于酶联免疫吸附测定(ELISA)可以检测经历凋亡或坏死的细胞分泌的蛋白质或生物标志物,因此可以借助该方法推断细胞死亡和活力。本研究表明,机械晶粒细化方法和表面改性可能会改善商业纯(CP)钛的机械和生物力学性能。根据腐蚀损失测量结果,2次通过MAO的腐蚀速率最低,确定为0.495 mmpy。1次通过和2次通过涂层样品的电极电位分别为1.44 V和1.47 V。这表明该涂层在降低金属CP Ti样品的腐蚀速率方面非常有效。晶粒尺寸的变化和大量晶界的存在对CP Ti的耐腐蚀性有显著影响。对于在3.6% NaCl电解质溶液中的ECAP处理和表面改性的钛样品,电化学阻抗谱(EIS)特性类似于奈奎斯特图和博德图拟合。根据ISO 10993-5评估体外细胞毒性的指南,本研究为牙髓和牙周细胞行为提供了有价值的见解,特别关注材料细胞毒性,这是由细胞活力降低30%确定的一个关键因素。

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