| 1. |
- Evertsson, Jonas, et al.
(författare)
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Self-organization of porous anodic alumina films studied in situ by grazing-incidence transmission small-angle X-ray scattering
- 2018
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Ingår i: RSC Advances. - 2046-2069. ; 8:34, s. 18980-18991
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Tidskriftsartikel (refereegranskat)abstract
- Self-ordered porous anodic alumina (PAA) films are studied extensively due to a large number of possible applications in nanotechnology and low cost of production. Whereas empirical relationships between growth conditions and produced oxides have been established, fundamental aspects regarding pore formation and self-organization are still under debate. We present in situ structural studies of PAA films using grazing-incidence transmission small-angle X-ray scattering. We have considered the two most used recipes where the pores self-organize: 0.3 M H2SO4 at 25 V and 0.3 M C2H2O4 at 40 V. During anodization we have followed the evolution of the structural parameters: average interpore distance, length of ordered pores domains, and thickness of the porous oxide layer. Compared to the extensively used ex situ investigations, our approach gives an unprecedented temporal accuracy in determination of the parameters. By using of Al(100), Al(110) and Al(111) surfaces, the influence of surface orientation on the structural evolution was studied, and no significant differences in the interpore distance and domain length could be observed. However, the rate of oxide growth in 0.3 M C2H2O4 at 40 V was significantly influenced by the surface orientation, where the slowest growth occurs for Al(111). In 0.3 M H2SO4 at 25 V, the growth rates were higher, but the influence of surface orientation was not obvious. The structural evolution was also studied on pre-patterned aluminum surfaces. These studies show that although the initial structures of the oxides are governed by pre-patterning geometry, the final structures are dictated by the anodization conditions.
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| 2. |
- Linpé, Weronica, et al.
(författare)
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The State of Electrodeposited Sn Nanopillars within Porous Anodic Alumina from In-situ X-ray Observations
- 2019
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Ingår i: ACS Applied Nano Materials. - : American Chemical Society (ACS). - 2574-0970. ; 2:5, s. 3031-3038
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Tidskriftsartikel (refereegranskat)abstract
- Porous anodic alumina (PAA) can be used as a template for controlled electrodeposition and growth of nano-structures, it is also essential for long-lasting decorative coloring of aluminum. We have investigated the deposition of Sn nanopillars into PAA in-situ, with Grazing transmission small angle X-ray scattering, X-ray fluorescence and X-ray absorption near edge structure spectroscopy. An accumulation of Sn could be detected in the pores during the electrodeposition. From the X-ray absorption near edge structure spectroscopy measurements we could conclude that the deposited Sn was primarily in the metallic state. Ex-situ scanning electron microscopy cross-section measurements show Sn nanopillars inside the PAA.
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| 3. |
- Långberg, Marie, 1988-, et al.
(författare)
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Redefining passivity breakdown of super duplex stainless steel by electrochemical operando synchrotron near surface X-ray analyses
- 2019
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Ingår i: npj Materials Degradation. - Stockholm, : Springer Science and Business Media LLC. - 2397-2106. ; 3:1
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Tidskriftsartikel (refereegranskat)abstract
- Passivity determines corrosion resistance and stability of highly-alloyed stainless steels, and passivity breakdown is commonly believed to occur at a fixed potential due to formation and dissolution of Cr(VI) species. In this work, the study of a 25Cr–7Ni super duplex stainless steel in 1 M NaCl solution revealed that the passivity breakdown is a continuous degradation progress of the passive film over a potential range, associated with enhanced Fe dissolution before rapid Cr dissolution and removal of the oxide. The breakdown involves structural and compositional changes of the passive film and the underlying alloy surface layer, as well as selective metal dissolution depending on the anodic potential. The onset of passivity breakdown occurred at 1000 mV/Ag/AgCl, and Fe dissolved more on the ferrite than the austenite phase. With increasing potential, the passive film became thicker but less dense, while the underlying alloy surface layer became denser indicating Ni and Mo enrichment. Rapid Cr dissolution occurred at ≥1300 mV/Ag/AgCl.
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| 4. |
- Vinogradov, Nikolay A., et al.
(författare)
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Observation of Pore Growth and Self-Organization in Anodic Alumina by Time-Resolved X-ray Scattering
- 2018
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Ingår i: ACS Applied Nano Materials. - : American Chemical Society (ACS). - 2574-0970. ; 1:3, s. 1265-1271
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Tidskriftsartikel (refereegranskat)abstract
- The anodic oxidation of metals such as aluminum and titanium can lead to the development of self-ordering pores. These pores make excellent templates for a range of nanoscale objects with many applications in nanoscience. Theoretical studies on pore formation have proposed several models for the establishment, growth, and ordering of these pores; however, experimental verification has mostly been limited to ex situ measurements. Here we show that the lateral and vertical pore structure can be probed in situ with high precision, using grazing transmission X-ray scattering. By making use of the high flux available at modern synchrotrons and fitting only the difference between scattering patterns we show the nearly real-time evolution of the pore’s arrangement. We observe no dependence on the substrate crystallographic orientation for domain size or pore separation. We do however observe an anisotropy in the oxide growth rate for the different substrate surfaces. This experimental approach can be applied to the study of a large variety of electrochemically produced materials such as magnetic nanowires, novel solar cell designs, and catalysts.
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| 5. |
- Örnek, Cem, et al.
(författare)
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In-situ synchrotron GIXRD study of passive film evolution on duplex stainless steel in corrosive environment
- 2018
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Ingår i: Corrosion Science. - : Elsevier BV. - 0010-938X .- 1879-0496. ; 141, s. 18-21
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Tidskriftsartikel (refereegranskat)abstract
- This paper presents new findings about the passive film formed on super duplex stainless steel in ambient air and corrosive environments, studied by synchrotron grazing-incidence X-ray diffraction (GIXRD). The passive film, formed in air, was seen to be a nano-crystalline mixed-oxide. Electrochemical polarisation to the passive region in aqueous 1 M NaCl at room temperature resulted in an increase of the passive film thickness, preferential dissolution of Fe, and partial loss of crystallinity. After termination of polarization to the transpassive regime, reformation of the mixed-oxides was observed, showing a thicker, semi-crystalline, and more defective nature (more vacancies) with further new oxides/hydroxides.
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| 6. |
- Örnek, Cem, et al.
(författare)
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Influence of Surface Strain on Passive Film Formation of Duplex Stainless Steel and Its Degradation in Corrosive Environment
- 2019
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Ingår i: Journal of the Electrochemical Society. - : The Electrochemical Society. - 0013-4651 .- 1945-7111. ; 166:11, s. 3071-3080
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Tidskriftsartikel (refereegranskat)abstract
- The effect of surface strain on the passive film evolution of SAF 2507 super duplex stainless steel exposed to ambient air and 0.1 M NaCl solution with varying anodic polarization at room temperature has been investigated using in-situ grazing incidence X-ray diffraction (GIXRD) in combination with electrochemical measurements. Surface strain affected the crystallinity of the passive film as such that the surface oxides/hydroxides were predominantly amorphous, with some minor crystalline CrOOH and FeOOH present in the film. Crystalline CrOOH was seen to diminish in volume upon immersion in the NaCl solution, well-possibly becoming amorphous during anodic polarization, whereas crystalline FeOOH was seen to increase in volume during polarization to the passive potential regime. Strain relaxation, associated with metal dissolution, occurred in both austenitic and ferritic grains during immersion in the electrolyte. Anodic polarization to the transpassive regime led to maximum strain relaxation, occurring more on the austenite than the ferrite. The selective transpassive dissolution nature of the ferrite was significantly reduced due to large strains in the austenite. Passive film breakdown was reflected by enhanced dissolution of Fe, Cr, Mo and Ni occurring simultaneously around 1300 mV vs. Ag/AgCl.
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