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Adhesion and cohesion properties of diamond-like-carbon coatings deposited on biomaterials by saddle field neutral fast atom beam source: measurement and modelling

机译:鞍场中性快原子束源沉积在生物材料上的类金刚石碳涂层的附着力和内聚力特性:测量和建模

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摘要

Diamond-like-carbon (DLC) has been shown to be strategically important in respect to biomedical applications due to its biocompatibility. Despite decades of work on film deposition there is an insufficient understanding in respect of the film’s adhesion characteristics, particularly on biomaterial substrates. The central aim of this study is two pronged. A programme of work has been undertaken to set-up, study, understand and optimise the production technique for DLC deposition, while on the other hand diamond like carbon films have been characterised to investigate the strength of adhesion and cohesive strength with particular reference to biomedical applications.ududDLC films have been deposited on to substrates of 316L stainless steel, cobalt chrome (CoCr) and Ti6AI4V alloy using a saddle field neutral beam deposition system (Microvac 1200DB, Ion Tech Ltd) with acetylene and acetyleneargon mixture as the process gas. It is noted that numerous parameters influence coating adhesion including the stress in the film, contamination and chemical bonding between the film and the substrate, and the physical properties and roughness of the substrate. Discharge current vs. discharge voltage characteristics were investigated with different pressure and process gas. Uv absorption spectra were used to measure the photon energy and optical band gap of the films. The optical band gap was found in the range of -0.85 and 0.85 -0.97 eV for lower and higher deposition current respectively. The adhesion of the films has been measured as a function of the duration of in-situ etching by a neutral argon beam and also as a function of source current, system pressure and process gas (pure C2H2 and C2H2+Ar gas mixture). The studies were performed on DLC films with thickness -0 .4 |im. The adhesion of the film was measured using pull-off and Rockwell C tests whereas four point bend (FPB) test was used to measure the cohesive strength of the films. Argon pre etching for 15 minutes is recommended to guarantee an optimal adhesion. The etching process also influenced the film structure in terms of the sp3/sp2 ratio and stress. It was also found that this optimisation of the adhesion is correlated with a change in the structure and thickness of the native oxide layer on the steel surface of the substrates. Substrate surface temperature during etching and deposition also influenced film structure and adhesion. Correlation between the residual stress and the adhesion of the films has also been established which helped to identify optimum process parameters for substrate-film adhesion properties. No significant change with deposition pressure has been observed but high anode currents may lead to higher sp3 content. The adhesion strength has been found to be inversely proportional to residual stress and to increase at low deposition pressures. At source anode current of 0.6A, the adhesion is a monotonic function of pressure in the range examined where as with 1.0A source current the behaviour is more complex. The relationship between the stress and the sp3 content of the films measured by analysis of Raman signature has also been investigated.ududThe experimental work of FPB has been used to support and develop a numerical (Finite Element) model for the determination and prediction of the film's cohesive strength. The model takes into account the film hardness, Young’s modulus and thickness and has been shown to be capable of predicting the film’s cohesive strength when combined with a theoretical formulation for brittle fracture. It has been observed that maximum stress developed at the outer surface of film during the bend test, which influenced the initiation of cracks at the outer surface of the film and their propagation through the film-substrate interface. This result has only been valid for films with higher Young's modulus compared with the substrate.
机译:由于其生物相容性,类金刚石碳(DLC)在生物医学应用方面已显示出战略重要性。尽管在薄膜沉积方面进行了数十年的研究,但对于薄膜的粘附特性,尤其是在生物材料基材上的粘附特性,人们仍缺乏足够的了解。这项研究的主要目标是两个方面。已经进行了一项工作计划,以建立,研究,理解和优化DLC沉积的生产技术,另一方面,已对类似金刚石的碳膜进行了表征,以研究粘附强度和内聚强度,特别是针对生物医学 ud udDLC薄膜已使用鞍场中性束沉积系统(Microvac 1200DB,Ion Tech Ltd)以乙炔和乙酰乙二酮混合物为工艺沉积到316L不锈钢,钴铬(CoCr)和Ti6Al4V合金的基底上加油站。应当指出,许多参数影响涂层的粘附性,包括膜中的应力,膜与基底之间的污染和化学键以及基底的物理性质和粗糙度。研究了在不同压力和工艺气体下的放电电流与放电电压的关系。紫外吸收光谱用于测量薄膜的光子能量和光学带隙。对于较低和较高的沉积电流,发现光学带隙分别在-0.85和0.85 -0.97 eV的范围内。薄膜的附着力已根据中性氩束进行原位蚀刻的持续时间以及源电流,系统压力和工艺气体(纯C2H2和C2H2 + Ar气体混合物)的功能进行了测量。研究是在厚度为-0 .4 | im的DLC膜上进行的。薄膜的粘附力使用拉拔和洛氏C测试进行测量,而四点弯曲(FPB)测试用于测量薄膜的内聚强度。建议使用氩气预蚀刻15分钟以确保最佳附着力。蚀刻工艺还从sp3 / sp2比和应力方面影响了膜结构。还发现粘附力的这种优化与基底的钢表面上的天然氧化物层的结构和厚度的变化相关。蚀刻和沉积过程中的基板表面温度也会影响膜的结构和附着力。还建立了残余应力与薄膜粘附力之间的相关性,这有助于确定基材薄膜粘附性的最佳工艺参数。没有观察到沉积压力的显着变化,但是高阳极电流可能导致较高的sp3含量。已经发现粘附强度与残余应力成反比,并在低沉积压力下增加。当源阳极电流为0.6A时,粘附力是所检查范围内压力的单调函数,而对于1.0A源电流,其行为更为复杂。还研究了通过拉曼特征分析测量的应力与薄膜中sp3含量之间的关系。 ud udFPB的实验工作已被用于支持和建立用于确定和预测的数值(有限元)模型薄膜的内聚强度。该模型考虑了膜的硬度,杨氏模量和厚度,并已证明能够与脆性断裂的理论公式结合起来预测膜的内聚强度。已经观察到,在弯曲试验期间在膜的外表面上产生了最大的应力,这影响了在膜的外表面处的裂纹的起始以及它们通过膜-基底界面的传播。该结果仅对与基材相比具有更高杨氏模量的薄膜有效。

著录项

  • 作者

    Morshed Muhammad Monjur;

  • 作者单位
  • 年度 2003
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  • 原文格式 PDF
  • 正文语种 en
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