Synchrotron photoelectron spectroscopy

Ultraviolet photoelectron spectroscopy (UPS) is a variety of photoelectron spectroscopy that is aimed at measuring the valence band, as described in sectionBl.25.2.3. Valence band spectroscopy is best perfonned with photon energies in the range of 20-50 eV. A He discharge lamp, which can produce 21.2 or 40.8 eV photons, is commonly used as the excitation source m the laboratory, or UPS can be perfonned with synchrotron radiation. Note that UPS is sometimes just referred to as photoelectron spectroscopy (PES), or simply valence band photoemission. 

Smith N V and Himpsel F J 1983 Photoelectron spectroscopy Handbook on Synchrotron Radiation ed E E Koch (Amsterdam North-Holland)... 

Eland, J. H. D. (1983) Photoelectron Spectroscopy. 2nd edn, Butterworth-Heinemann, London. Huffier, S. (2001) Photoelectron Spectroscopy Principles and Applications. 3rd edn. Springer, Berlin. Prince, K. C. (1995) Photoelectron Spectroscopy of Solids and Suifaces Synchrotron Radiation Techniques and Applications, World Scientific Publishing, Singapore. 

Other techniques utilize various types of radiation for the investigation of polymer surfaces (Fig. 2). X-ray photoelectron spectroscopy (XPS) has been known in surface analysis for approximately 23 years and is widely applied for the analysis of the chemical composition of polymer surfaces. It is more commonly referred to as electron spectroscopy for chemical analysis (ESCA) [22]. It is a very widespread technique for surface analysis since a wide range of information can be obtained. The surface is exposed to monochromatic X-rays from e.g. a rotating anode generator or a synchrotron source and the energy spectrum of electrons emitted... 

Extensive discussion on the ionization potentials of 1,2,5-thiadiazole and its derivatives can be found in CHEC(1984) and CHEC-II(1996) <1984CHEC(6)513, 1996CHEC-II(4)355>. Hel photoelectron spectroscopy, inner-shell electron energy loss spectroscopy involving the S2p, S2s, Cls and Nls edges, and Sis synchrotron radiation photoabsorption spectroscopy were used to probe the occupied and unoccupied valence levels of benzothiadiazole 2 <1991MI165>. 

An ozone treatment (10 minutes at room temperature) of the HF-etched SiC surface before the metallization step was introduced as a very convenient processing step to produce Schottky diode gas sensors with an increased stability and reproducibility. The use of spectroscopic ellipsometry analysis and also photoelectron spectroscopy using synchrotron radiation showed that an oxide, 1-nm in thickness, was formed by the ozone exposure [74, 75]. The oxide was also found to be close to stochiometric SiO in composition. This thin oxide increased the stability of the SiC Schottky diodes considerably, without the need for any further interfacial layer such as Ta or TaSi which have been frequently used. Schottky diodes employing a porous Pt gate electrode and the ozone-produced interfacial layer have been successfully operated in both diesel exhausts and flue gases [76, 77]. 

As we have seen, the most advanced photoelectron techniques, especially those which necessitate the use of synchrotron radiation sources, have been applied until now only to U and Th systems. Application on Pu and Am systems as well as to heavier actinides is to be expected in the future. The same development is likely to occur as for neutron experiments, where more and more these hazardous actinides are investigated at high levels of instrumental sophistication. Difficulties arising from handling and protection problems are, of course, much greater for photoelectron spectroscopy. 

Hollinger et al (1985) have studied bronzes NaxW03 and Na2TayW1 y03 near the metal-insulator transition using photoelectron spectroscopy with synchrotron radiation. The results show that the transition is due to localization in an impurity band in a pseudogap. 

Nesbitt, H.W., Schaufu/3, A., Sciani, M. et al. (2003) Monitoring fundamental reactions at NiAsS surfaces by synchrotron radiation X-ray photoelectron spectroscopy As and S air oxidation by consecutive reaction schemes. Geochimica et Cosmochimica Acta, 67(5), 845-58. 

XRD and LEED are laboratory techniques, although synchrotrons offer advantages for XRD. XAFS, on the other hand, is conducted almost exclusively at synchrotrons. This - and the fact that EXAFS data analysis is complicated and not always without ambiguity - has inhibited the widespread use of the technique in catalysis. XANES, however, is becoming increasingly popular, as it may routinely yield similar information as X-ray photoelectron spectroscopy (XPS), but under in-situ conditions. 

There has been substantial progress in experimental and theoretical surface analytical methods over the last years. Methods based on X-rays and UV light for diffraction, absorption, or photoelectron spectroscopies benefit from new generation synchrotron light sources. To name a few, surface experimental methods include XPS, AES and SIMS for investigating the surface chemistry A

adsorption energetics and kinetics as well as XPD, RAIRS, HREELS, LEED and STM for molecular and surface structure... 

Synchrotron radiation (SR) sources provided a welcome boost to photoelectron spectroscopy in the late 80s. In fact, the switch from conventional discharge sources to SR induced a major revolution. Consequently, we now provide a brief description of the advantages and disadvantages of synchrotron radiation sources. Should the reader be interested in further details, a number of excellent reviews12-14 are available. 

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