Photoelectron spectroscopy instrumentation

All components of the photoelectron spectroscopy instrumentation have continued to evolve over the last decade. New commercial sources for XPS with the anode at high positive potential have an order of magnitude improvement in photon flux over the older grounded anode designs. Analyzers with electron lens prefocusing are far superior to unmodified hemispherical, parallel plate, or cylindrical... 

Wang, X.B. Wang, L.S. Development of a low-temperature photoelectron spectroscopy instrument using an electrospray ion source and a cryogenically controlled ion trap. Rev. Set Instrum. 2008, 79, 173108. 

Ratner, B. D., and Castner, D. G., Advances in x-ray photoelectron spectroscopy instrumentation and methodology instrument evaluation and new techniques with special reference to biomedical. studies. Colloids Surfaces B Biointerfaces, 2, 343-346 (1994). 

X-ray Photoelectron Spectroscopy analysis of the samples was performed with a Surface Science Instruments spectrometer (SSI 100) with a resolution (FWHM Au 4f7/2) of 1.0 eV. The X-ray beam was a monochromatised AlKa radiation (1486.6 eV). A charge neutraliser (flood gun) was adjusted at an energy of 6 eV. As the Cls spectra of these compounds were very complex, the binding energies were referenced to the binding energy of Ols, considered experimentally to be at 531.8 eV [8). 

For probing the nature of the acid sites by X-ray photoelectron spectroscopy (XFS), the samples were evacuated before gaseous pyridine was adsorbed. Excess pyridine was desorbed at 1S0°C, and then samples were pressed onto a sample stub imder Nj and loaded into the SCIENTA ESCA-300 instrument without exposure to air. Sample charging was minimized by using a Qood gun while acquiring the experimental data. 

The work of Siegbahn s group who, in the 1950s, improved the energy resolution of electron spectrometers and combined it with X-ray sources. This led to a technique called electron spectroscopy for chemical analysis (ESCA), nowadays more commonly referred to as X-ray photoelectron spectroscopy (XPS) [6]. Siegbahn received the Nobel Prize for his work in 1981. Commercial instruments have been available since the early seventies. 

X-ray photoelectron spectroscopy is indeed quite informative, but requires the use of expensive instrumentation. Also, the detection of photoelectrons requires the use of ultrahigh vacuum, and therefore can mostly be used for ex situ characterization of catalytic samples (although new designs are now available for in situ studies [146,147]). Finally, XPS probes the upper 10 to 100 A of the solid sample, and is only sensitive to the outer surfaces of the catalysts. This may yield misleading results when analyzing porous materials. 

Surface characterization studies by X-ray photoelectron spectroscopy (XPS) were conducted using DuPont 650 and Perkin Elmer 5300 instruments. Samples were prepared by placing solid material on double stick adhesive tape, or by allowing solvent to evaporate from an acetone dispersion of a suspension placed on a stainless steel probe. A magnesium anode was used as the X-ray source (hv 1253.6 eV). The temperature of samples during the analysis was approximately 30-40°C and the vacuum in the analysis chamber was about 10 torr. Potential... 

Some instrumental methods have been used for the investigation of sulphide mineral-thio-collector system such as infra-red (IR) spectroscopy (Mielezarski and Yoon, 1989 Leppinen et al., 1989 Persson et al, 1991 Laajalehto et al, 1993 Zhang., et al., 2004a) and X-ray photoelectron spectroscopy (XPS) (Pillai et al, 1983 Page and Hazell, 1989 Grano et al, 1990 Laajalechto et al, 1991). These surface sensitive spectroscopic techniques can be applied for the direct determination of the surface composition at the conditions related to flotation. 

The experiments were performed in stainless steel UHV chambers which were equipped with the instrumentation necessary to perform Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), UV Photoelectron Spectroscopy (UPS), Low Energy Electron Diffraction (LEED), work function measurements (A( )), High Resolution Electron Energy Loss Spectroscopy (HREELS), and Temperature Programmed Desorption (TPD). The Au(lll) crystal was heated resist vely and cooled by direct contact of the crystal mounting block with a liquid nitrogen reservoir. The temperature of the Au(lll) crystal was monitored directly by means of a... 

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. 

Photoelectron Spectroscopy. As a subdivision of electron spectroscopy, photoelectron or photoemission spectroscopy (PES) includes those instruments that use a photon source to eject electrons from surface atoms. The techniques of x-ray photoelectron spectroscopy (XPS) and uv photoelectron spectroscopy (UPS) are the principles in this group. Auger electrons are emitted also because of x-ray bombardment, but this combination is used infrequent-... 

Solid metal hydrides specifically have been reviewed here, but XPS and UPS can serve as tools to study vapors or volatile liquids. Much of the original work with these two methods involved organic molecules only later were solid surfaces studied. Therefore, they should always be considered as helpful analytical instruments for examining the bonding chemistry of organometallic compounds. This symposium covered mainly organometallic hydrides, and they are prime candidates for photoelectron spectroscopy study. 

We begin with the most routine characterization methods—electrochemical methods. We then discuss various instrumental methods of analysis. Such instrumental methods can be divided into two groups ex situ methods and in situ methods. In situ means that the film on the electrode surface can be analyzed while the film is emersed in an electrolyte solution and while electrochemical reactions are occurring on/in the film. Ex situ means that the film-coated electrode must be removed from the electrolyte solution before the analysis. This is because most ex situ methods are ultra-high-vacuum techniques. Examples include x-ray photoelectron spectroscopy [37], secondary-ion mass spectrometry [38,39], and scanning or transmission electron microscopies [40]. Because ex situ methods are now part of the classical electrochemical literature, we review only in situ methods here. 

The X-ray photoelectron spectroscopy (XPS) experiments were performed in an ultra-high vacuum (UHV) chamber coupled to an atmospheric pressure reaction cell. All XPS results were obtained from samples treated in situ in the reaction cell and transferred into UHV without exposure to air. Detailed sample mounting procedures and instrument details are described elsewhere.16 Ar+ bombardment was done with 3 KeV Ar+ ions at a current density of 0.8 pA/cm2 for 1 h in an attempt to remove the carbon overlayer and expose the underlying carbide phase. 

X-ray Photoelectron Spectroscopy. X-ray photoelectron spectroscopy (xps) and Auger electron spectroscopy (aes) are related techniques (19) that are initiated with the same fundamental event, the stimulated ejection of an electron from a surface. The fundamental aspects of these techniques will be discussed separately, but since the instrumental needs required to perform such methods are similar, xps and aes instrumentation will be discussed together. 

The numerous applications in various fields of chemistry and physics have clearly demonstrated the potential of X-ray photoelectron spectroscopy. A number of interesting experimental projects will be completed in the near future and papers with new and more reliable reference data will appear in the literature. Further refinement of the theoretical models will add to the fundamental understanding of the obtained results. And last, but not least new developments in instrumentation will keep pace with the practical and theoretical experience and open up new areas, which so far could not be penetrated because of resolution, sensitivity or sample handling problems. 

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