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Powder manipulation, microstructure, mechanical properties and bio-corrosion performance of titanium and titanium alloys additively manufactured by selective electron beam melting

机译:通过选择性电子束熔融添加制造的钛和钛合金的粉末操作,微观结构,机械性能和生物腐蚀性能

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摘要

Additive manufacturing (AM), defined as a process of joining materials to make parts from three dimensional (3D) model data, usually layer upon layer, as opposed to subtractive and formative manufacturing methodologies, has been recognized globally as a group of revolutionary near-net-shape or net-shape fabrication technologies. AM offers advantages of more freedom in design, lower buy-to-fly ratio and shorter lead times. Selective electron beam melting (SEBM) is a powder-bed-fusion-based AM process, developed by Arcam AB in Sweden in 2002, which offers high energy efficiency and power density, rapid scan speed and unique capability of manufacturing high reactive metals such as titanium (Ti) due to the vacuum build chamber involved. Although much research has been devoted to the SEBM of Ti alloys, particularly Ti-6Al-4V, current understanding of the mechanical performance of SEBM-fabricated Ti components is still limited in a number of aspects. This thesis aims at enhancing the current understanding of the AM process of Ti and Ti alloys by SEBM in the following four aspects. 1. Manipulation and characterization of a novel Ti powder precursor for SEBM applications A low-cost novel Ti powder precursor (sponge Ti particles) has been manipulated using a proprietary powder manipulation technology (PMT) in order to produce a low-cost, nearly spherical Ti powder for SEBM applications. Research has shown that the PMT is capable of producing more than 50 wt.% of nearly spherical Ti powder in the size range of 45–106 μm (usable for SEBM) and about 30 wt.% of less than 45 μm of nearly spherical powder (usable for AM by cold spray processes). PMT-processed Ti powder with a size range of 75–106 μm exhibited similar flowability and spreadability to those of recycled Arcam Ti-6Al-4V powder when assessed in an external Arcam powder bed evaluation system. Cubic samples were built with the PMT-processed Ti powder using an Arcam A1 SEBM system under different SEBM parameters. The resulting density, surface conditions and microstructures of the as-built samples were investigated. It was concluded that through appropriate modification of the SEBM parameters in conjunction with the use of suitable melt strategies, it is feasible to produce quality samples with the newly developed low-cost nearly spherical Ti powder. This research demonstrates the potential of developing low-cost feedstock powder for AM by SEBM. 2. Positional dependence of microstructure and tensile properties of a thick Ti-6Al-4V block additively manufactured by SEBM Limited information exists in the open literature about the microstructure and mechanical properties of SEBM-fabricated thick-section (≥25.4 mm) Ti-6Al-4V samples or parts, while thick sections are involved in many components for structural applications. A systematic study has been made of the positional dependence of the microstructure and tensile properties of a 34mm-thick Ti-6Al-4V block additively manufactured by SEBM. Marginally graded microstructures were observed along the build direction and from the side surface to the centre. Abnormally coarse α laths, thick and tortuous grain boundary α phase, and massive α phase transformation products were observed. To assess the tensile properties, a total of 27 tensile samples were prepared from nine different heights of the block sample, and all samples satisfied the minimum requirements for mill-annealed Ti-6Al-4V, irrespective of their positions in the thick block. This conclusion demonstrates the capabilities of SEBM in producing quality thick-section Ti-6Al-4V components. A range of other revealing observations were documented and discussed. 3. The influence of as-built surface conditions and hot isostatic pressing (HIP) on tensile and fatigue properties of SEBM Ti-6Al-4V Achieving a high surface finish is a major challenge for most current metal AM processes. A quantitative study has been made of the influence of as-built surface conditions on the tensile and fatigue properties of Ti-6Al-4V produced by SEBM as compared to acid-etched and machined conditions. The experimental results indicate that chemical etching can double tensile elongation and noticeably improve tensile strengths due to improved surface finish. However, the fatigue strength remained to be much inferior to that of mill-annealed Ti-6Al-4V due to residual surface defects. Consequently, it remains challenging to modify the as-built surfaces of SEBM-fabricated components for fatigue-critical structural applications, particularly for those components which contain deep and narrow internal channels and complex concave and convex surfaces. HIP was employed to enhance the fatigue properties of SEBM-fabricated Ti-6Al-4V. Samples with different surface conditions (as-built, etched, machined and insufficiently machined) were subjected to HIP and their fatigue properties were evaluated under uniaxial tensile loading conditions. Although HIP can effectively improve the fatigue performance by healing most internal defects (i.e. pores and lack-of-fusion defects), it was found that surface defects played a more decisive role than internal defects in determining the fatigue properties of HIP-processed SEBM Ti-6Al-4V samples. It is expected that the fatigue properties of additively manufactured Ti-6Al-4V will continue to be a subject of considerable research in the near future. 4. The electrochemical responses of Ti-6Al-4V alloy manufactured by seven different processes including SEBM in Hank’s solution at 37oC Considering the increasing applications of additively manufactured Ti-6Al-4V implants, an in-depth understanding of the bio-corrosion performance of additively manufactured Ti-6Al-4V is necessary. For this reasons, samples of Ti-6Al-4V were manufactured by seven different processes, including SEBM, SEBM + HIP, selective laser beam melting (SLM), SLM + HIP, casting, mill-annealing, and spark plasma sintering (SPS). A comparative study was then made of the corrosion characteristics of these samples via the potentiodynamic polarization tests in Hank’s solution at 37oC. The microstructural features of each group of samples were characterized prior to corrosion. The corroded surfaces including the corrosion products were analysed. Owing to different microstructures, Ti-6Al-4V samples manufactured by different processes showed distinctly different polarization responses. The order of corrosion resistance was found to be: SLM & mill-annealed & SLM + HIP & SEBM & SEBM + HIP Cast SPS. The point defect model was used to interpret the different corrosion responses. The findings of this research provide a different perspective for the selection of manufacturing process for Ti-6Al-4V for bone implant applications.
机译:增材制造(AM)是指一种将材料连接起来以从三维(3D)模型数据中制造零件的过程,通常是逐层的,这与减法和形成性制造方法相反,已被全球公认是一组革命性的近距离制造方法。净形或净形制造技术。 AM提供了更多的设计自由度,更低的购买率和更短的交货时间。选择性电子束熔化(SEBM)是基于粉末床融合的AM工艺,由瑞典Arcam AB于2002年开发,具有高能效和功率密度,快速扫描速度以及独特的制造高活性金属的能力,例如钛(Ti)由于涉及真空成型腔。尽管已经对Ti合金,特别是Ti-6Al-4V的SEBM进行了大量研究,但是,目前对SEBM加工的Ti部件的机械性能的理解仍然在许多方面受到限制。本文旨在从以下四个方面增强当前对SEBM对Ti和Ti合金AM加工的理解。 1.用于SEBM应用的新型Ti粉末前体的处理和表征为了生产低成本,接近球形的新型Ti粉末前体(海绵Ti颗粒),已使用专有的粉末处理技术(PMT)对其进行了处理。用于SEBM应用的钛粉。研究表明,PMT能够生产尺寸范围为45至106μm(可用于SEBM)的接近球形的Ti粉末,占重量的50%以上,小于45μm的约为重量的30%。接近球形的粉末(可通过冷喷涂工艺用于增材制造)。当在外部Arcam粉末床评估系统中评估时,PMT处理的尺寸为75-106μm的Ti粉末表现出与回收的Arcam Ti-6Al-4V粉末相似的流动性和铺展性。使用Arcam A1 SEBM系统,在不同的SEBM参数下,使用PMT处理的钛粉构建立方样品。研究了所生成样品的密度,表面条件和微观结构。结论是,通过适当修改SEBM参数以及使用适当的熔融策略,使用新开发的低成本近球形Ti粉生产高质量样品是可行的。这项研究证明了通过SEBM开发低成本AM原料粉末的潜力。 2.由SEBM增材制造的厚Ti-6Al-4V块的微观结构和拉伸性能的位置依赖性在公开文献中存在关于SEBM加工的厚截面(≤25.4mm)Ti-的微观组织和力学性能的有限信息。 6Al-4V样品或零件,而厚的部分涉及结构应用的许多组件。对由SEBM增材制造的34mm厚Ti-6Al-4V块的微观结构和拉伸性能的位置依赖性进行了系统的研究。沿构建方向以及从侧面到中心观察到边缘渐变的微观结构。异常粗糙α条,厚而曲折的晶界α阶段和大规模α观察到相变产物。为了评估拉伸性能,从九个不同高度的块状样品制备了总共27个拉伸样品,并且所有样品均满足工厂退火的Ti-6Al-4V的最低要求,无论它们在厚块中的位置如何。该结论证明了SEBM在生产优质厚截面Ti-6Al-4V零件中的能力。记录和讨论了一系列其他揭示性观察。 3.竣工的表面条件和热等静压(HIP)对SEBM Ti-6Al-4V的拉伸和疲劳性能的影响对于大多数当前的金属增材制造工艺而言,实现高表面光洁度是一项重大挑战。与酸蚀和机械加工条件相比,已建成的表面条件对SEBM生产的Ti-6Al-4V的拉伸和疲劳性能的影响进行了定量研究。实验结果表明,由于改善了表面光洁度,化学蚀刻可以使拉伸伸长率增加一倍,并显着提高拉伸强度。但是,由于残留的表面缺陷,其疲劳强度仍远低于经铣削退火的Ti-6Al-4V。因此,为疲劳关键型结构应用,特别是对于那些包含深而窄的内部通道以及复杂的凹凸表面的组件,修改SEBM制造的组件的已建表面仍然具有挑战性。 HIP用于增强SEBM制造的Ti-6Al-4V的疲劳性能。具有不同表面条件的样品(竣工,蚀刻,机械加工和机械加工不足)进行HIP,并在单轴拉伸载荷条件下评估其疲劳性能。尽管HIP可以通过修复大多数内部缺陷(例如,孔隙和熔合缺陷)有效地改善疲劳性能,但是发现在确定HIP处理的SEBM Ti的疲劳性能方面,表面缺陷比内部缺陷起着决定性的作用。 -6Al-4V样品。预期在不久的将来,添加制造的Ti-6Al-4V的疲劳性能将继续成为大量研究的主题。 4.通过包括SEBM在37℃的Hank溶液中的7种不同工艺制造的Ti-6Al-4V合金的电化学响应考虑到增材制造的Ti-6Al-4V植入物的日益广泛的应用,对生物腐蚀有深入的了解增材制造的Ti-6Al-4V的性能是必要的。因此,通过SEBM,SEBM + HIP,选择性激光束熔化(SLM),SLM + HIP,铸造,铣削退火和火花等离子体烧结(SPS)等七种不同工艺来制造Ti-6Al-4V样品。然后通过在Hank溶液中在37oC下进行的电位动力学极化试验对这些样品的腐蚀特性进行了比较研究。在腐蚀之前表征每组样品的微观结构特征。分析了包括腐蚀产物的腐蚀表面。由于不同的微观结构,通过不同工艺制造的Ti-6Al-4V样品显示出明显不同的极化响应。发现耐蚀性的顺序为:SLM& 1。研磨退火& SLM + HIP& SEBM& SEBM + HIP Cast SPS。使用点缺陷模型来解释不同的腐蚀响应。这项研究的发现为选择用于骨植入应用的Ti-6Al-4V的制造工艺提供了不同的视角。

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