Ratna Sunil B, Sampath Kumar T S, Chakkingal Uday, Nandakumar V, Doble Mukesh, Devi Prasad V, Raghunath M
Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, India.
Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, India.
Mater Sci Eng C Mater Biol Appl. 2016 Feb;59:356-367. doi: 10.1016/j.msec.2015.10.028. Epub 2015 Oct 22.
The objective of the present work is to investigate the role of different grain sizes produced by equal channel angular pressing (ECAP) on the degradation behavior of magnesium alloy using in vitro and in vivo studies. Commercially available AZ31 magnesium alloy was selected and processed by ECAP at 300°C for up to four passes using route Bc. Grain refinement from a starting size of 46μm to a grain size distribution of 1-5μm was successfully achieved after the 4th pass. Wettability of ECAPed samples assessed by contact angle measurements was found to increase due to the fine grain structure. In vitro degradation and bioactivity of the samples studied by immersing in super saturated simulated body fluid (SBF 5×) showed rapid mineralization within 24h due to the increased wettability in fine grained AZ31 Mg alloy. Corrosion behavior of the samples assessed by weight loss and electrochemical tests conducted in SBF 5× clearly showed the prominent role of enhanced mineral deposition on ECAPed AZ31 Mg in controlling the abnormal degradation. Cytotoxicity studies by MTT colorimetric assay showed that all the samples are viable. Additionally, cell adhesion was excellent for ECAPed samples particularly for the 3rd and 4th pass samples. In vivo experiments conducted using New Zealand White rabbits clearly showed lower degradation rate for ECAPed sample compared with annealed AZ31 Mg alloy and all the samples showed biocompatibility and no health abnormalities were noticed in the animals after 60days of in vivo studies. These results suggest that the grain size plays an important role in degradation management of magnesium alloys and ECAP technique can be adopted to achieve fine grain structures for developing degradable magnesium alloys for biomedical applications.
本工作的目的是通过体外和体内研究,探讨等径角挤压(ECAP)产生的不同晶粒尺寸对镁合金降解行为的影响。选用市售AZ31镁合金,并在300°C下采用Bc路径通过ECAP加工多达四道次。在第四道次后,成功地将初始尺寸为46μm的晶粒细化至1-5μm的晶粒尺寸分布。通过接触角测量评估的ECAP处理样品的润湿性因细晶结构而增加。通过浸入过饱和模拟体液(SBF 5×)研究的样品的体外降解和生物活性表明,由于细晶AZ31镁合金润湿性的增加,在24小时内出现快速矿化。通过在SBF 5×中进行的失重和电化学测试评估的样品的腐蚀行为清楚地表明,增强的矿物沉积在ECAP处理的AZ31镁中对控制异常降解起着重要作用。通过MTT比色法进行的细胞毒性研究表明,所有样品都是有活力的。此外,ECAP处理的样品,特别是第三道次和第四道次的样品,细胞粘附性极佳。使用新西兰白兔进行的体内实验清楚地表明,与退火的AZ31镁合金相比,ECAP处理的样品降解速率较低,并且所有样品均具有生物相容性,在体内研究60天后,动物未发现健康异常。这些结果表明,晶粒尺寸在镁合金的降解管理中起着重要作用,并且可以采用ECAP技术来获得细晶结构,以开发用于生物医学应用的可降解镁合金。