NanoSIMS analysis of hydrogen and deuterium in metallic alloys: Artefacts and best practice

NanoSIMS analysis of hydrogen and deuterium in metallic alloys: Artefacts and best practice
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金属合金中氢和氘的 NanoSIMS 分析:人工制品和最佳实践

DOI:
10.1016/j.apsusc.2021.149736
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发表时间:
2021
影响因子:
6.7
通讯作者:
Aboura Y
Aboura Y
中科院分区:
材料科学1区
文献类型:
--
作者:
Aboura Y

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氢脆可导致高强度合金的灾难性失效,但确定微观结构中的局部氢在分析上具有挑战性。NanoSIMS是少数几种可以在微观结构相关长度尺度上映射金属样品中的氢和氘的技术之一。因此,必须了解伪影并确定可靠检测的最佳方法。已经建立了用于氘(作为氢的代理)的NanoSIMS分析的实验方法/协议,揭示了未报告的伪影,并且提出了一种新的方法来最小化在映射合金中的氢和氘中的这些伪影。这种方法被用来映射氘在电化学充电的奥氏体不锈钢和沉淀硬化镍基合金的分布。在分析室中检测到残留的氘污染,这是由于样品中的氘脱气,并且通过一系列NanoSIMS实验评估了这种氘污染的影响。开发了一种新的分析协议,涉及映射被动氧化层中的氘,从而减轻束损伤效应,当表面高度氘化时,束损伤效应可能会阻止局部氘信号的检测。
Hydrogen embrittlement can cause catastrophic failure of high strength alloys, yet determining localised hydrogen in the microstructure is analytically challenging. NanoSIMS is one of the few techniques that can map hydrogen and deuterium in metal samples at microstructurally relevant length scales. Therefore it is essential to understand the artefacts and determine the optimum methodology for its reliable detection. An experimental methodology/protocol for NanoSIMS analysis of deuterium (as a proxy for hydrogen) has been established uncovering unreported artefacts and a new approach is presented to minimise these artefacts in mapping hydrogen and deuterium in alloys. This method was used to map deuterium distributions in electrochemically charged austenitic stainless steel and precipitation hardened nickel-based alloys. Residual deuterium contamination was detected in the analysis chamber as a result of deuterium outgassing from the samples, and the impact of this deuterium contamination was assessed by a series of NanoSIMS experiments. A new analysis protocol was developed that involves mapping deuterium in the passive oxide layer thus mitigating beam damage effects that may prevent the detection of localised deuterium signals when the surface is highly deuterated.
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