2000
DOI: 10.1149/1.1394043
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X-Ray Photoelectron Spectroscopy and Morphological Studies of Polycrystalline Nickel Surfaces Exposed to Anhydrous HF

Abstract: The Simons electrochemical fluorination (ECF) process is an important method for the electrosynthesis of a variety of perfluorinated organic compounds of commercial interest. 1 The electron/ atom-transfer reactions associated with this complex process are believed to occur on sites on, or within a film formed on Ni anodes polarized at very high potentials, ca. 5-6 V vs. a hydrogen-evolving Ni counter electrode, in solutions of the organic precursors in liquid anhydrous HF (AHF). Although the film undoubtedly c… Show more

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Cited by 11 publications
(10 citation statements)
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“…Initial formation of a passivation layer on the freshly prepared Ni anode occurs upon application of an oxidizing potential . It is known that when metallic Ni is exposed to gaseous or liquid HF, the formation of NiF 2 is exergonic . NiF 2 as an electrical insulator is consistent with its proposed role in the passivation of the anode …”
Section: Resultsmentioning
confidence: 66%
“…Initial formation of a passivation layer on the freshly prepared Ni anode occurs upon application of an oxidizing potential . It is known that when metallic Ni is exposed to gaseous or liquid HF, the formation of NiF 2 is exergonic . NiF 2 as an electrical insulator is consistent with its proposed role in the passivation of the anode …”
Section: Resultsmentioning
confidence: 66%
“…All aspects of the cleaning and transfer of Ni foils between the main and auxiliary chambers, as well as those regarding XPS analysis have been described previously. 2 Polarization of clean Ni foil electrodes ͑Alfa Aesar, 99 ϩ %, 0.127 mm thick, 0.25 cm 2 active area͒ was performed using an EG&G PAR model 173 potentiostat with a model 176 current-to-voltage converter and an EG&G PAR model 175 universal programmer. A second Ni foil, cut from the same piece as the working electrode ͑WE͒ and of an area ten times larger than the WE, was used both as a counter and reference electrode, Ni͓C/R͔.…”
Section: Methodsmentioning
confidence: 99%
“…Recently, novel procedures were developed and implemented at Case Western Reserve University ͑CWRU͒, that allow specimens to be exposed to AHF environments in an auxiliary ultrahigh vacuum ͑UHV͒ compatible chamber. 2 These specimens can subsequently be transferred to a UHV chamber ͑herein denoted as main͒, equipped with an X-ray photoelectron spectrometer ͑XPS͒. The transfer is performed using a portable UHV-compatible arm, which prevents exposure of specimens to the ambient atmosphere, thereby avoiding complications in the interpretation of data derived from contamination.…”
mentioning
confidence: 99%
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“…The sample soaked in TiCl 4 was not pretreated with NH 3 . The peak position of nickel fluoride (NiF 2 ) is 685.3 eV for F 1s [12] and 858 eV for Ni 2p [13]. The peak positions of nickel oxidesNi 2 O 3 and NiO-are 855.8 and 854.5 eV for Ni 2p [14].…”
Section: Deoxidization Mechanism By Nh 3 Soak Treatmentmentioning
confidence: 99%