Valence-to-Core X-ray Emission Spectroscopy Identification of Carbide Compounds in Nanocrystalline Cr Coatings Deposited from Cr(III) Electrolytes Containing Organic Substances

Сафонов, В. А.; Vykhodtseva, L. N.; Polukarov, Yurii M.; Safonova, Оlga V.; Smolentsev, Grigory; Sikora, Marcin; Eeckhout, S. G.; Glatzel, Pieter

doi:10.1021/jp064569j

Cited by 106 publications

(76 citation statements)

References 11 publications

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“…It should be pointed out that a low-energy component is also observed in the C1s spectra recorded for Cr coatings deposited from aqueous electrolytes [32,33], where the overall percentage of carbon generally is much higher (about 22 at.%) than that in the coating obtained from the employed IL (about 4-5 at.%). It is known [34][35][36][37], that C1s peak revealed at BE \ 285.0 eV points to the presence of coordination bonds between carbon chains and chromium atoms and the negative shift value depends on the electronic density on carbon. Analysis of the C1s spectra makes it possible to illuminate the nature of species formed on the metalelectrolyte interface.…”

Section: Resultsmentioning

confidence: 99%

Chromium electrodeposition from [BMIm][BF4] ionic liquid

Surviliene¹,

Eugénio

Vilar

2010

J Appl Electrochem

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The electrodeposition of black chromium coatings from ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate with chromium chloride, and the chemical composition of the deposits are discussed in this article. The UV-Vis spectra recorded for chromium(III) species in 1-butyl-3-methylimidazolium tetrafluoroborate suggest that along with the chromium(III) complexes containing three ligands, there are some amounts of chromium species containing four ligands in the bath employed. The cathodic process of chromium electrodeposition in the employed ionic liquid is complicated by the electrochemical reduction of water molecules, which is followed by chemical disintegration of tetrafluoroborate ions. The surface morphology of black chromium films deposited potentiostatically (-1.5 to -2.0 V) at 85°C shows nodules and microcracks increasing in size with cathodic potential. Analysis of the X-ray photoelectron spectra recorded from surface to depth of the deposit has shown that the black oxide-rich chromium coating consists of chromium in both oxide and metallic states with small impurities of other elements (fluorine, boron, carbon and nitrogen) and the surface is covered with a thin layer of organic substances. The results of this study show that 1-butyl-3-methylimidazolium tetrafluoroborate may be considered as a promising substitute of toxic Cr(VI) baths for black chromium plating.

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Section: Resultsmentioning

confidence: 99%

Chromium electrodeposition from [BMIm][BF4] ionic liquid

Surviliene¹,

Eugénio

Vilar

2010

J Appl Electrochem

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“…Besides to the chemically most sensitive valenceto-core 4,5,7,32,[89][90][91][92] , core-to-core transitions have also proved useful in physical and chemical characterization 2,3,30,38,93,94 . Using a crystal spectrometer, one can record the corresponding X-ray emission spectrum with a good resolution, as illustrated in figure 2 for the case of NaBrO 3 (the also displayed theoretical spectrum will be discussed later).…”

Section: X-ray Emission Spectroscopymentioning

confidence: 99%

On the sensitivity of hard X-ray spectroscopies to the chemical state of Br

Bordage

Pápai

Sas

et al. 2013

Phys. Chem. Chem. Phys.

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The sensitivity of the 1s X-ray emission and high-energy-resolution fluorescence-detected X-ray absorption spectroscopies (XES and HERFD-XAS) to resolve the variations of the chemical state (electronic structure and local coordination) of Br has been investigated for a selected set of compounds including NaBrO 3 , NH 4 Br and C 2 H 4 Br 2 (1,2-dibromoethane). For the Br K-edge XAS, employing the HERFD mode significantly increases the energy resolution, which demonstrates that with a crystal spectrometer used as detector the absorption technique becomes a more powerful analytical tool. In the case of XES, the experimental results as well as the density functional theory (DFT) modeling both show that the chemical sensitivity of the main 1s diagram emission lines (Kα 1,2 and Kβ 1,3 ) is rather limited. However, the valence-to-core (Kβ 2 ) region of XES displays significant shape and intensity variations, as expected for transitions having the same final states as those of photoemission spectroscopy. The spectra are in good agreement with the molecular orbital description delivered by DFT calculations. Calculations for an extended series of Br compounds confirm that valence-to-core XES can serve as a probe for chemical analysis, and, being a hard X-ray photon-in/photon-out technique, it is particularly well-suited for in situ investigations of molecular transformations, even on the ultrafast time scales down to femtosecond time resolution.

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“…[8][9][10][11] and to study core-to-core and valence-to-core transitions. [12][13][14] The high energy resolution XAS/RIXS techniques require the experimental resolution to be lower than the natural lifetime broadening of the excited state. For x-rays between 5 keV and 15 keV, the lifetime broadening of the K-shell is in the range of 1 eV-5 eV (i.e., lifetimes of 1.6-6.5 × 10 −16 s), while for the L-shell it is between 3 eV and 10 eV (0.7-2.1 × 10 −16 s).…”

Section: Introductionmentioning

confidence: 99%

A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

Szlachetko

Nachtegaal

Boni

et al. 2012

Review of Scientific Instruments

167

145

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We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

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Valence-to-Core X-ray Emission Spectroscopy Identification of Carbide Compounds in Nanocrystalline Cr Coatings Deposited from Cr(III) Electrolytes Containing Organic Substances

Cited by 106 publications

References 11 publications

Chromium electrodeposition from [BMIm][BF4] ionic liquid

Chromium electrodeposition from [BMIm][BF4] ionic liquid

On the sensitivity of hard X-ray spectroscopies to the chemical state of Br

A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

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