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Characterization of porous nickel-titanium alloys for medical applications.

机译:用于医疗应用的多孔镍钛合金的表征。

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摘要

The purpose of this study is to investigate the electrochemical behaviour of porous NiTi alloys provided by different sources. In order to achieve this goal, a systematic characterization of the physical and chemical properties by different techniques and new approaches were conducted. The martensite-austenite phase transition was determined by the use of the Differential scanning Calorimetry (DSC). The morphological characteristics (porosity and roughness) were measured with the Scanning Electron Microscopy (SEM). The surface chemical composition of the samples was identified by the use of X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES).;In the case of porous material the biomechanical compatibility is closely related to the porosity distribution of the sample. To describe appropriately the influence of this parameter on the properties of NiTi, four types of materials provided by different sources were analyzed. The samples were produced by Self-propagating High-temperature Synthesis (SHS) procedure. A heat treatment was applied in order to release internal stress created during forming processes, one series of specimens from each type was submitted to an annealing process during 30 min at 550°C in an air atmosphere. Its influence on the properties of the materials was also evaluated.;Our first results showed that despite the fact that all the materials present different pore size, all the samples exhibited an open and interconnected porosity that promotes a good fixation and bone ingrowth within their structure. The thermal analysis showed that the temperature of the inception of the martensite-austenite phase transition occurs at 60°C, which is greater than the body temperature by 20°C. The microscopic analysis for the samples revealed that the heat treatment did not generate any morphological changes. The XPS study indicated that the surface oxidation occurs after the heat treatment. This oxide layer has a different thickness for the materials in the range of 310--3990 A.;The evaluation of the corrosion resistance of the four porous NiTi alloys showed a correlation between the chemical composition, pore size and the electrochemical behaviour. In particular it was found that the corrosion resistance is related to the surface chemical composition of the electrodes rather than to their surface morphology. First we observed that the impact of the annealing process varies with the type of sample. The non-treated samples showed higher breakdown potentials and also bigger pores. The materials with a pore size in the range of 80-120mum showed different behaviours, one material (B) showed no visible effect while the other two (A and C) exhibited a decrease of the breakdown potential value. The material with the smallest pore size 35-50mum showed an important improvement after the heat treatment. Therefore, we can conclude, that the surface treatment used in our investigations led to an improvement of the corrosion resistance for small pores whereas a decrease was observed for bigger pores.;On the other hand the lower corrosion rates observed on treated samples are an indication of the high corrosion resistance compare to those non-treated. In this case we observed that the one material (B) exhibited the highest corrosion rate presented a difference in the chemical composition as shown by XPS analysis. Moreover, the absence of intermediate titanium oxides (Ti2+ and Ti3+) was observed. As these oxides were identified in the other materials (A, C and D) we conclude that the presence of intermediate titanium oxides on surface chemical composition of the samples results on better corrosion rates and improved corrosion resistance.;The Spectroelectrochemistry evaluation showed that solid electropolished sample and solid mechanopolished samples exhibited a better corrosion resistance than porous mechanopolished samples. However the solid mechanopolished sample exhibits a higher corrosion rate almost as high as the one showed by the porous sample. On the other hand a higher breakdown potential was measured porous samples compared to previous studies. However this sample shows a higher susceptibility for pitting and crevice corrosion. This can be explained by the porous structure of the sample. The FTIR results showed the interactions between the solution and the samples. It can be observed that each sample exhibit a particular behaviour. The porous sample as well as the solid samples showed Ti-OH interactions. Moreover both solid samples exhibited another peak corresponding to the OTi(OH)CCH interaction, which is explained by the chemical composition of the electrolyte, in this case the Hank's solution that has a certain amount of glucose. However an inversion of the peak is observed in both samples, this direction change can be attributed to the surface treatment. The electropolished sample showed a more stable behaviour mean while the mechanopolished sample exhibited a change during the reverse scan. (Abstract shortened by UMI.)
机译:这项研究的目的是研究不同来源提供的多孔NiTi合金的电化学行为。为了实现该目标,通过不同的技术和新方法对物理和化学性质进行了系统表征。通过使用差示扫描量热法(DSC)确定马氏体-奥氏体相变。用扫描电子显微镜(SEM)测量形态特征(孔隙率和粗糙度)。通过使用X射线光电子能谱(XPS)和俄歇电子能谱(AES)来识别样品的表面化学组成;在多孔材料的情况下,生物力学相容性与样品的孔隙率分布密切相关。为了恰当地描述该参数对NiTi性能的影响,分析了不同来源提供的四种材料。样品通过自蔓延高温合成(SHS)程序生产。为了消除在成型过程中产生的内部应力,进行了热处理,将每种类型的一系列试样在空气中于550°C下于30分钟内进行退火处理。我们的第一个结果表明,尽管所有材料均具有不同的孔径,但所有样品均显示出开放且互连的孔隙度,从而促进了其结构内的良好固定和骨向内生长。热分析表明,马氏体-奥氏体相变开始的温度发生在60°C,比体温高20°C。样品的显微分析表明热处理没有产生任何形态变化。 XPS研究表明,热处理后会发生表面氧化。该氧化物层在310--3990 A的范围内具有不同的材料厚度;四种多孔NiTi合金的耐蚀性评估显示出化学成分,孔径和电化学行为之间的相关性。特别地,发现耐腐蚀性与电极的表面化学组成有关,而不与电极的表面形态有关。首先,我们观察到退火过程的影响随样品类型而变化。未经处理的样品显示出更高的击穿电位和更大的孔。孔径在80-120μm范围内的材料表现出不同的行为,一种材料(B)无可见效果,而其他两种(A和C)击穿电位值降低。最小孔径为35-50μm的材料在热处理后显示出重要的改进。因此,我们可以得出结论,我们的研究中使用的表面处理导致小孔的耐蚀性提高,而大孔的耐蚀性下降;另一方面,在处理过的样品上观察到的较低的腐蚀速率表明与未经处理的相比,具有较高的耐腐蚀性。在这种情况下,我们观察到一种材料(B)表现出最高的腐蚀速率,这表明化学成分存在差异,如XPS分析所示。此外,观察到不存在中间的钛氧化物(Ti 2+和Ti 3+)。由于在其他材料(A,C和D)中发现了这些氧化物,因此我们得出结论,样品表面化学成分中存在中间氧化钛会导致更好的腐蚀速率和改善的耐腐蚀性。;光谱电化学评估表明固体电抛光样品和固态机械抛光样品比多孔机械抛光样品具有更好的耐腐蚀性。然而,固体机械抛光的样品表现出较高的腐蚀速率,几乎与多孔样品显示的腐蚀速率一样高。另一方面,与以前的研究相比,多孔样品的击穿潜力更高。然而,该样品显示出更高的点蚀和缝隙腐蚀敏感性。这可以通过样品的多孔结构来解释。 FTIR结果显示了溶液和样品之间的相互作用。可以看出,每个样本都表现出特定的行为。多孔样品和固体样品都显示出Ti-OH相互作用。此外,两个固体样品均显示出另一个对应于OTi(OH)CCH相互作用的峰,这由电解质的化学组成解释,在这种情况下,Hank's溶液具有一定量的葡萄糖。但是,在两个样品中均观察到峰反转,该方向变化可以归因于表面处理。电抛光的样品表现出更稳定的行为平均值,而机械抛光的样品在反向扫描过程中表现出变化。 (摘要由UMI缩短。)

著录项

  • 作者

    Hernandez Tenorio, Rommy.;

  • 作者单位

    Ecole Polytechnique, Montreal (Canada).;

  • 授予单位 Ecole Polytechnique, Montreal (Canada).;
  • 学科 Engineering Biomedical.;Engineering Materials Science.
  • 学位 Ph.D.
  • 年度 2008
  • 页码 131 p.
  • 总页数 131
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 生物医学工程;工程材料学;
  • 关键词

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