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Application of Electrochemical Noise measurements for Stress Corrosion Cracking studies: influence of current partition and instrumental noise

机译:电化学噪声测量在应力腐蚀裂纹研究中的应用:电流分配和仪器噪声的影响

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Electrochemical Noise (EN) measurements have been increasingly implemented in Stress Corrosion Cracking (SCC) studies because of its non-intrusive characteristics and its performance for (ⅰ) crack initiation detection, (ⅱ) SCC progression monitoring and (ⅲ) quantitative evaluation of the dissolved amount of metal during discontinuous cracking by measuring the current generated by each cracking step and using the Faraday law. However, the influence of both the current partition (in the measuring circuit) and the instrument noise on the obtained results was not entirely clarified in these studies. In that context, this work is focused on the investigation of the influence of both the instrumental noise and the rise in asymmetry between the electrodes (inherent in the SCC tests when only the working electrode is stressed) on the EN data. The EN data were acquired by using two electrodes made from Inconel 600 alloy connected with a zero-resistance ammeter (ZRA) and a Saturated Calomel Electrode (SCE) as a reference electrode. Only one of the Inconel electrodes (Working Electrode - WE) was undergoing SCC in an acidified 10 mM tetrathionate solution under constant load, while the other electrode (Counter Electrode -CE) remained unstressed. The WE and CE presented the same exposed surface to the solution and underwent the same surface preparation. The studied SCC system is known to be prone to intergranular SCC and to generate a low level of EN. The results showed that the measured current did not correspond to the totality of the current released by the anodic process occurring on the stressed specimen. Actually, only a fraction of the current due to anodic dissolution occurring at the WE was recorded because of the higher impedance of the CE. On the other hand, an important contribution to the total recorded current came both from the CE due to the asymmetry of the system and from the instrumental noise of the ZRA (Gamry REF600). The instrumental noise was quantified and its effective frequency bandwidth was compared with that of the EN data related to the corrosion process. The consequences of the asymmetry of the system were evaluated in the frequency domain and it remains hazardous to go back to temporal transients. It was finally demonstrated that the contribution of the instrumentation noise can represent the major part of the EN for very weakly emissive SCC systems. In that case, the quantitative evaluation of dissolution processes from EN data appears to be therefore questionable.
机译:由于应力腐蚀开裂(SCC)研究的非侵入性特性及其在(ⅰ)裂纹萌生检测,(ⅱ)SCC进度监控和(ⅲ)定量评估应力腐蚀性能方面的性能,因此在应力腐蚀开裂(SCC)研究中已越来越多地采用电化学噪声(EN)测量。通过测量每个裂化步骤产生的电流并使用法拉第定律,在不连续裂化过程中溶解金属的量。然而,在这些研究中并没有完全弄清电流分配(在测量电路中)和仪器噪声对获得的结果的影响。在这种情况下,这项工作的重点是研究仪器噪声和电极之间不对称性上升(仅在工作电极受到压力时在SCC测试中固有)对EN数据的影响。通过使用两个由Inconel 600合金制成的电极连接零电阻电流表(ZRA)和饱和甘汞电极(SCE)作为参考电极来获取EN数据。在恒定负载下,仅一个Inconel电极(工作电极-WE)在酸化的10 mM四硫代酸盐溶液中进行SCC,而另一个电极(对电极-CE)保持无应力状态。 WE和CE呈现相同的溶液暴露表面,并进行了相同的表面处理。已知研究的SCC系统倾向于晶间SCC并产生低水平的EN。结果表明,测得的电流与应力试样上发生的阳极过程释放的电流总量不符。实际上,由于CE的较高阻抗,仅记录了由于WE处发生阳极溶解而产生的电流的一小部分。另一方面,由于系统的不对称性,CE以及ZRA(Gamry REF600)的仪器噪声都对CE产生了重要的贡献。对仪器噪声进行了量化,并将其有效频率带宽与与腐蚀过程相关的EN数据进行了比较。在频域中评估了系统不对称的后果,回到时态瞬态仍然很危险。最终证明,对于非常弱的发射SCC系统,仪器噪声的贡献可以代表EN的主要部分。在那种情况下,根据EN数据对溶解过程进行定量评估似乎是有问题的。

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