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CHARACTERISATION OF IRON OXIDE DEPOSITS ON NICKEL-BASED ALLOY TUBES

机译:镍基合金管氧化铁沉积物的表征

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In nuclear pressurised water reactors (PWRs), steam generators (SGs) which are composed of thousands of tubes are used as heat exchangers between the primary (inside the tubes) and secondary (outside the tubes) circuits. On the SG secondary side, a fouling phenomenon occurs due to the deposition of corrosion products (mainly composed of iron oxides) at the surface of the tubes. In the long term, this effect could degrade thermal performances and may enhance risks of SG tube cracking. Several studies have been made on the characterisation of these deposits [1], on their formation mechanisms [2], and on their impact on the thermal transfer [3-5]. However, the relation between the deposit morphology and composition, the fouling mechanisms and their effect on the heat transfer efficiency in SG needs further investigations. The aim of this study is to get a detailed characterisation of the morphology, chemistry and crystallography of the deposits formed at the surface of SG tubes. Since PWR SG tube extraction is very difficult, experimental loops have been used to form fouling deposits on Ni-Cr based alloy (Inconel 600) tubes using representative secondary side thermodynamic conditions. As in a SG, two types of deposit conditions are considered: monophasic liquid and biphasic liquid-steam. In the present work, focus was made on morphological multi-scale characterisations. The observation of the surface of various sections of tubes using a FEI Nova NanoSEM 450 SEM and chemical analyses using a Bruker SDD EDS revealed that the deposits consist of geometrically-shaped crystallites containing Fe and O (Fig. 1) and allowed coverage estimations of about 82 %. Those observations were completed with u-Raman mappings to determine the molecular species present in the deposit. Deposit thickness measurements of various sections of tubes were also made from SEM observations in cross-sections to get statistical results giving a mean thickness of 0.97 ± 0.44 nm. As deposits are brittle and sensitive to oxidation, a water-free methodology has been developed for the metallographic preparation of samples, from cutting to polishing step including nickel-plating and cold resin-coating. Then, 3D electron tomography using a FEI Helios 660 dual column scanning electron microscope associated with a focussed ion beam (SEM/FIB) was used to get 3D reconstructions of the deposits over cubic micrometre volumes (Fig. 2). These reconstructions allowed the quantification of porosity, thickness distribution and coverage rate at the local scale.
机译:在核加压水反应器(PWR)中,由数千管组成的蒸汽发生器(SGS)用作初级(管)和次级(管道外部)电路之间的热交换器。在SG二次侧,由于在管的表面上沉积腐蚀产物(主要由氧化铁组成)而发生污垢现象。从长期来看,这种效果可能降低热性能,并且可以增强SG管裂化的风险。在它们的形成机制[2]上对这些沉积物[1]的表征进行了几项研究,以及它们对热转印的影响[3​​-5]。然而,沉积形态与组成之间的关系,污垢机制及其对SG中传热效率的影响需要进一步研究。本研究的目的是在SG管表面上形成的沉积物的形态,化学和晶体的详细表征。由于PWR SG管提取非常困难,因此使用代表性二次侧热力学条件,已经使用实验环在Ni-Cr基合金(Inconel 600)管上形成污垢沉积物。如在SG中,考虑两种类型的沉积条件:单表液体和双相液 - 蒸汽。在目前的工作中,重点是在形态的多标识上进行。使用Fei Nova纳米肌450SEM和使用Bruker SDD ED的化学分析观察管的各个部分表面的观察显示,沉积物由含Fe和O的几何形状的微晶组成,并允许覆盖约估计82%。这些观察结果用U形拉曼映射完成,以确定沉积物中存在的分子物种。还通过横截面的SEM观察沉积物沉积厚度测量,以获得统计结果,其平均厚度为0.97±0.44nm。由于沉积物是脆性并且对氧化敏感,因此已经开发了一种无水方法,用于样品的金相制备,从切割到包括镍镀和冷树脂涂层的抛光步骤。然后,使用与聚焦离子束(SEM / FIB)相关联的FEI Helios 660双柱扫描电子显微镜的3D电子断层扫描用于在立方微米体积上获取沉积物的3D重建(图2)。这些重建允许在本地规模上定量孔隙率,厚度分布和覆盖率。

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