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Full depth profile of passive films on 316L stainless steel based on high resolution HAXPES in combination with ARXPS
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
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2012 (English)In: Applied Surface Science, ISSN 0169-4332, E-ISSN 1873-5584, Vol. 258, no 15, 5790-5797 p.Article in journal (Refereed) Published
Abstract [en]

Depth profiles of the passive films on stainless steel were based on analysis with the non-destructive hard X-ray photoelectron spectroscopy (HAXPES) technique in combination with the angular resolved X-ray photoelectron spectroscopy (ARXPS). The analysis depth with ARXPS is within the passive film thickness, while the HAXPES technique uses higher excitation energies (between 2 and 12 keV) also non-destructively probing the chemical content underneath the film. Depth profiles were done within and underneath the passive film of 316L polarized in acidic solution. The passive film thickness was estimated to 2.6 nm for a sample that was polarized at 0.6 V and the main component in the passive film is, as expected, chromium. From the high resolution HAXPES spectra we suggest chromium in three different oxidation states present. Also for iron three oxides were detected. Gradients of chromium and iron concentrations and oxidation states within the film and an enrichment of nickel within a 0.5 nm layer directly underneath the passive film are some of the results discussed. 

Place, publisher, year, edition, pages
2012. Vol. 258, no 15, 5790-5797 p.
Keyword [en]
Stainless steel, XPS, HAXPES, Passive film
National Category
Inorganic Chemistry
Research subject
Chemistry with specialization in Inorganic Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-173615DOI: 10.1016/j.apsusc.2012.02.099ISI: 000302135700044OAI: oai:DiVA.org:uu-173615DiVA: diva2:525780
Funder
StandUp
Available from: 2012-05-09 Created: 2012-05-02 Last updated: 2017-12-07Bibliographically approved
In thesis
1. Depth Profiling of the Passive Layer on Stainless Steel using Photoelectron Spectroscopy
Open this publication in new window or tab >>Depth Profiling of the Passive Layer on Stainless Steel using Photoelectron Spectroscopy
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The physical properties of the protective passive films formed on the surface of stainless steels under electrochemical polarization in different electrolytes were studied. The structure of these films was analyzed as a function of depth using photoelectron spectroscopy (PES).

Depth profiling (using PES) of the surface layer was achieved by either changing the angle of incidence to achieve different analysis depths (ARXPS), by argon ion etching, or by varying the energy of the incoming x-rays by the use of synchrotron radiation. The use of hard x-rays with high resolution (HAXPES) provided novel quantified information about the nickel content underneath the passive films.

A complex environment was found in these surface layers composed of an outermost monolayer of iron on top of a layer of chromium hydroxides covering an underlayer of chromium oxides. Molybdenum was enriched in the interface between the metal and oxide. Nickel is enriched underneath the passive film and therefore nickeloxides are only present in the surface layer in low concentrations.

A comparison was performed on austenitic and duplex stainless prepared by hot isostatically pressed (HIP) or cast and forged processes. HIP stainless steel was produced using the burgeoning technique of pressing gas atomized powders together. The structure of these steels is far more homogenous with a lower porosity than that of the conventionally prepared equivalents. It was shown that hot HIP austenitic steel had better pitting corrosion resistance than its conventional counterpart.

Finally, the duplex steel was cycled in a Li-ion battery to explore its potential application as a current collector. It was shown that the passive film formed in the organic solvents is similar in composition and thickness to the films formed in aqueous solutions. However, it is doubtful if steel could be used as current collector in batteries due to its high reactivity with lithium.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2012. 69 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 955
Keyword
depth profile, stainless steel, passive film, XPS, HAXPES, corrosion, powder metallurgical
National Category
Materials Chemistry
Research subject
Chemistry with specialization in Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-179399 (URN)978-91-554-8430-9 (ISBN)
Public defence
2012-09-28, Å2005, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 13:15 (English)
Opponent
Supervisors
Available from: 2012-09-05 Created: 2012-08-14 Last updated: 2013-01-22
2. Insights into Li-ion Battery and Stainless Steel Interfaces Using Refined Photoelectron Spectroscopy Methodology
Open this publication in new window or tab >>Insights into Li-ion Battery and Stainless Steel Interfaces Using Refined Photoelectron Spectroscopy Methodology
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

If sacrificing some of its material to form a passivating layer at the surface, materials may expand the range of environments where they can be used and further material degradation can decrease. This thesis aims to contribute with insights into passivating layers on especially Li-ion battery anodes (solid electrolyte interphase, SEI) but also on stainless steels, as well as the non-passivating Li-ion battery cathode/electrolyte interface layers (solid permeable interface, SPI). The studies have been performed using new possibilities offered by photoelectron spectroscopy techniques.

Depth gradients in the SEI and SPI layers were studied by combining synchrotron-based hard and soft X-ray photoelectron spectroscopy (HAXPES and SOXPES), which was further developed for Li-ion battery investigations. Stainless steel depth profiles were acquired combining HAXPES with angle resolved X-ray photoelectron spectroscopy (ARXPS).

In the Li-ion battery, organic species were more common in the outermost SEI, while some inorganic compounds were only detected in the more bulk sensitive measurements. No depth gradients were observed in the SPI. The interface between the graphite and the SEI was studied for the first time indicating lithium enrichment at the graphite surface. Furthermore, the influence of the film-forming additive propargyl methanesulphonate (PMS) on the electrode/electrolyte interfaces was studies, and cells cycled to end of life at 22°C and 55°C were compared.

For stainless steels, the thicknesses of the oxide film as well as the nickel enriched metal layer underneath the oxide were determined. A similar methodology was applied to estimate the Li-ion battery SEI thickness.

Finally, experiences from PES methodology work on the Li-ion battery systems are discussed aiming to facilitate further studies of the experimentally challenging electrochemically modified samples.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2013. 69 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1031
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-197153 (URN)978-91-554-8624-2 (ISBN)
Public defence
2013-05-03, Häggsalen, Ångströmslaboratoriet, Lägerhyddsvägen 1, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2013-04-12 Created: 2013-03-18 Last updated: 2013-08-30Bibliographically approved

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Fredriksson, WendyMalmgren, SaraGustafsson, TorbjörnEdström, Kristina

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