Erratum: “Dual analyzer system for surface analysis dedicated for angle-resolved photoelectron spectroscopy at liquid surfaces and interfaces” [Rev. Sci. Instrum. 87, 045105 (2016)]

Niedermaier, Inga; Kolbeck, Claudia; Steinrück, Hans‐Peter; Maier, Florian

doi:10.1063/1.4983571

Cited by 9 publications

(26 citation statements)

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“…Angle‐resolved X‐ray photoelectron spectroscopy (ARXPS): The ARXPS experiments were performed in our DASSA (Dual Analyzer System for Surface Analysis) setup, for details see Ref. . Simultaneous acquisition of ARXP spectra at two fixed emission angles of ϑ =0° (normal emission) and 80° (grazing emission) with respect to the surface normal of a horizontally mounted sample was achieved by two hemispherical energy analyzers (ARGUS‐type).…”

Section: Methodsmentioning

confidence: 99%

“…At 80°, it decreases to 1.0 to 1.5 nm, making the measurement very surface sensitive: ≈80 % of the signal originates from the topmost molecular layer. Each set of 80° spectra was scaled up by an individual geometry factor to compensate for lower intensity compared to 0° spectra . After this normalization, intensity differences between 80° and 0° emission angle directly reflect a higher/lower concentration of the respective species at the surface than in the bulk.…”

Section: Methodsmentioning

confidence: 99%

“…For the quantitative analysis of the spectra, we used atomic sensitivity factors (ASFs) . As the C 1s signal from the CF 3 group of the [PFBMIm] + cation overlaps with the shake‐up of the aromatic system of the cation, the intensity of this peak is set equal to that of the CF 2 peak.…”

Section: Methodsmentioning

confidence: 99%

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Temperature‐Dependent Surface Enrichment Effects in Binary Mixtures of Fluorinated and Non‐Fluorinated Ionic Liquids

Heller

Lexow

Greco

et al. 2020

Chemistry A European J

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Using angle-resolved X-ray photoelectron spectroscopy (ARXPS), we investigate the topmost nanometers of various binary ionic liquid (IL) mixtures at differentt emperatures in the liquid state. The mixtures consist of ILs with the same [PF 6 ] À anion but two different cations, namely 3methyl-1- (3,3,4,4,4-pentafluorobutyl)imidazoliumh exafluorophosphate, [PFBMIm][PF 6 ], and 1-butyl-3-methylimidazolium hexafluorophosphate, [C 4 C 1 Im][PF 6 ], with 10, 25, 50 and 75 mol %c ontento f[ PFBMIm][PF 6 ]. We observe ap referential enrichmento ft he fluorinated chain in the topmostl ayer, relative to the bulk composition, which is mostp ronounced for the lowest content of [PFBMIm][PF 6 ]. Upon cooling the mixtures stepwise from 95 8Cu ntil surfacec harging effects in XPS indicate solidification,w eo bserve ap ronouncedi ncreasei ns urfacee nrichmento ft he fluorinated chain with decreasing temperature in the liquid state. In contrast to the mixtures with lower[ PFBMIm] [PF 6 ]c ontents, cooling the 75 mol %m ixture additionallys hows an abrupt decrease of the fluorinated chain signal before complete solidification occurs, whichisa ssigned to partial precipitation effects.[a] B.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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Temperature‐Dependent Surface Enrichment Effects in Binary Mixtures of Fluorinated and Non‐Fluorinated Ionic Liquids

Heller

Lexow

Greco

et al. 2020

Chemistry A European J

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“…[43] As experimental method, we use ARXPS for probing the surface layer of the IL samples. Our Dual Analyzer System for Surface Analysis (DASSA) [44] setup allows for simultaneously recording spectra in a surface sensitive and a bulk sensitive mode, which directly permits to identify surface enrichment or depletion effects of all atoms (apart from hydrogen) being present in the ions. Compared to LEIS and TOF-SIMS (and to a lower extent also RBS), XPS has the disadvantage that it is sensitive not only to the topmost layer, but depending on the emission angle, the signals stem from the first 7-9 nm (10-15 IL layers; at 08 emission) or from the first 1-1.5 nm (1-2 IL layers; at 808 emission).…”

Section: Introductionmentioning

confidence: 99%

Surface Enrichment in Equimolar Mixtures of Non‐Functionalized and Functionalized Imidazolium‐Based Ionic Liquids

et al. 2018

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For equimolar mixtures of ionic liquids with imidazolium‐based cations of very different electronic structure, we observe very pronounced surface enrichment effects by angle‐resolved X‐ray photoelectron spectroscopy (XPS). For a mixture with the same anion, that is, 1‐methyl‐3‐octylimidazolium hexafluorophosphate+1,3‐di(methoxy)imidazolium hexafluorophosphate ([C8C1Im][PF6]+[(MeO)2Im][PF6]), we find a strong enrichment of the octyl chain‐containing [C8C1Im]+ cation and a corresponding depletion of the [(MeO)2Im]+ cation in the topmost layer. For a mixture with different cations and anions, that is, [C8C1Im][Tf2N]+[(MeO)2Im][PF6], we find both surface enrichment of the [C8C1Im]+ cation and the [Tf2N]− (bis[(trifluoromethyl)sulfonyl]imide) anion, while [(MeO)2Im]+ and [PF6]− are depleted from the surface. We propose that the observed behavior in these mixtures is due to a lowering of the surface tension by the enriched components. Interestingly, we observe pronounced differences in the chemical shifts of the imidazolium ring signals of the [(MeO)2Im]+ cations as compared to the non‐functionalized cations. Calculations of the electronic structure and the intramolecular partial charge distribution of the cations contribute to interpreting these shifts for the two different cations.

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“…60 This setup is the first of its kind and is equipped with two electron analyzers for detection at 0 • and 80 • . It enables simultaneously studying the bulk and the surface of the IL, by angle-resolved XPS, without the need of rotating the liquid sample.…”

Section: Discussionmentioning

confidence: 99%

Perspective: Chemical reactions in ionic liquids monitored through the gas (vacuum)/liquid interface

Maier

Niedermaier

Steinrück

2017

The Journal of Chemical Physics

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This perspective analyzes the potential of X-ray photoelectron spectroscopy under ultrahigh vacuum (UHV) conditions to follow chemical reactions in ionic liquids in situ. Traditionally, only reactions occurring on solid surfaces were investigated by X-ray photoelectron spectroscopy (XPS) in situ. This was due to the high vapor pressures of common liquids or solvents, which are not compatible with the required UHV conditions. It was only recently realized that the situation is very different when studying reactions in Ionic Liquids (ILs), which have an inherently low vapor pressure, and first studies have been performed within the last years. Compared to classical spectroscopy techniques used to monitor chemical reactions, the advantage of XPS is that through the analysis of their core levels all relevant elements can be quantified and their chemical state can be analyzed under well-defined (ultraclean) conditions. In this perspective, we cover six very different reactions which occur in the IL, with the IL, or at an IL/support interface, demonstrating the outstanding potential of in situ XPS to gain insights into liquid phase reactions in the near-surface region.

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Erratum: “Dual analyzer system for surface analysis dedicated for angle-resolved photoelectron spectroscopy at liquid surfaces and interfaces” [Rev. Sci. Instrum. 87, 045105 (2016)]

Abstract: Erratum: "Dual analyzer system for surface analysis dedicated for angle-resolved photoelectron spectroscopy at liquid surfaces and interfaces" [Rev. Sci. Instrum. 87, 045105 (2016)]Cite as: Rev. Sci. Instrum. 88, 059902 (2017); https://doi

Cited by 9 publications

References 1 publication

Temperature‐Dependent Surface Enrichment Effects in Binary Mixtures of Fluorinated and Non‐Fluorinated Ionic Liquids

Temperature‐Dependent Surface Enrichment Effects in Binary Mixtures of Fluorinated and Non‐Fluorinated Ionic Liquids

Surface Enrichment in Equimolar Mixtures of Non‐Functionalized and Functionalized Imidazolium‐Based Ionic Liquids

Perspective: Chemical reactions in ionic liquids monitored through the gas (vacuum)/liquid interface

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