Combined electrochemical/surface science investigations of Pt/Cr alloy electrodes Page: 4 of 21
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Electronic grade 85% H3P04 was treated with H202 to remove oxidizable
impurities [7]. Prior to electrochemical measurements the solution wa:3 de-
gassed with ultra-high purity argon. Usually 50 cycles were made between
*0.04 V and the desired upper limit and the potential brought to +0.40 V
(double layer region) before removing from potentiostatic control. The elec-
trode was immediately removed from solution and washed eith pure water ir. an
ultrasonic cleaner. The samples were then ultrasonically cleaned in absolute
ethanol, and placed in the vacuum chamber for analysis.
X-ray photoelectron spectroscopy (XPS) was performed in a Leybold-Hereaus
apparatus described previously [8], using a Mg-Ka X-ray source. Spectra were
collected at 100 eV pass erergy, referenced to a Ag 3d5/2 peak at 367.91 eV
binding energy (B.E.) for pure Ag, with a full width at half maximum (FWHM) of
1.67 eV. All spectra were referenced to the Fermi level of the sample. Sputter
cleaning was achieved with a 3 kV Ar' ion beam.
Ill. RESULTS
111.1. Characterization of Polished PLCr Alloys
To ascertain whether the sur face of the alloys is representative of the
bulk, XP: spectra of Pt(4f) and Cr(2p) regIorns were recorrdcd for each alloy as
well as for pure Pt and Cr. Figure 1 shuws spectra for" polished samples that
have been briefly (<, min) sputterud clean with Are ions t.o remove surface'
contamination. Spectra for unsputtered samples were arlsu recur'dvd; pc+;k in-
tens 1 Li es were docr eaned duc to sur faec' contam t inat. ion (C ,0) and l i 1f1nt
amounts o1' Cr oxide were ubner ved in the Cr( 'p) YP. region. prom the areas (1)
under' the PL Jrnd Cr pc.ikn the atmic rat l of C.: r.r/Pt cou d be obtained for both
utnputtered ard c onn alloyn:
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Daube, K. A.; Paffett, M. T.; Gottesfeld, S. & Campbell, C. T. Combined electrochemical/surface science investigations of Pt/Cr alloy electrodes, article, January 1, 1985; New Mexico. (https://digital.library.unt.edu/ark:/67531/metadc1054134/m1/4/: accessed July 16, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.