X‐ray photoelectron spectroscopy on radioactive materials using a McPherson ESCA‐36 equipped with an SSL position‐sensitive detector

Abstract

A McPherson ESCA-36 instrument has been upgraded extensively to achieve greatly enhanced x-ray photoelectron spectroscopy (XPS) performance. An SSL position-sensitive detector (PSD) has been retrofitted to the spectrometer in place of the standard exit slit and channel electron multiplier. A DEC LSI-11/73 computer and a Tektronix colour-graphics terminal with ink-jet plotter have been substituted for the o r i g i~l PDP 8/e computer and peripherals. The system vacuum quality also has been significantly improved by installation of modern cryosorption and turbomolecular pumps. A self-contained software package, based on interactive program modules, has been developed for XPS surface analysis, comprising instrument control, data acquisition and data processing. Photoelectron spectra are recorded in the non-retardation scanning mode, utilizing the output from the central 200 channels of the 256-channel PSD. High spectrometer resolution has been maintained by accounting for energy dispersion to second order. Calibration of the spectrometer energy scale and intensity-energy response function is discussed. The suitability of the upgraded ESCA-36 for XPS studies of highly radioactive materials, such as used CANDU fuel, is illustrated.

Sample handling, preparation and mounting for XPS and other surface analytical techniques

“…There are groups that specialize in the analysis of radioactive materials, and they have instruments dedicated to this purpose. 27…”

The influence of dissolved hydrogen on the surface composition of doped uranium dioxide under aqueous corrosion conditions

“…SIMFUEL is an unirradiated analogue of used nuclear fuel, produced by doping natural UO 2 with a series of stable elements (Ba, Ce, La, Mo, Sr, Y, Rh, Pd, Ru, Nd, Zr) in proportions appropriate to replicate the chemical effects of irradiation of UO 2 fuel in a CANDU reactor to various burn-ups [13,14]. As a consequence of this doping procedure, holes are injected into the 5f band, due to the substitution of trivalent rare-earth species (e.g.…”

Electrochemical, SECM, and XPS Studies of the Influence of H2 on UO2 Nuclear Fuel Corrosion

“…%, or 6 at. % burn-up [11,12]. The noble metal elements (Mo, Ru, Rh, Pd), insoluble in the oxide lattice, congregate in metallic ε-particles, consisting of small, spherical precipitates (0.5 -1.5 µm diameter) uniformly distributed in the UO 2 matrix [11].…”