Electronic spectroscopy, surface analysis

AUGER Auger Electron Spectroscopy Surface analysis and high resolution depth profiling Auger electrons from near surface atoms 0.1-1 at% <20A >i,oooA... 

FE AUGER Field Emission Auger Electron Spectroscopy Surface analysis, microanalysis, microarea depth profiling Auger electrons firom near surface atoms 0.01-1 at% 20-ti0A <150A... 

A first parameter to be studied is the applied potential difference between anode and cathode. This potential is not necessarily equal to the actual potential difference between the electrodes because ohmic drop contributions decrease the tension applied between the electrodes. Examples are anode polarisation, tension failure, IR-drop or ohmic-drop effects of the electrolyte solution and the specific electrical resistance of the fibres and yarns. This means that relatively high potential differences should be applied (a few volts) in order to obtain an optimal potential difference over the anode and cathode. Figure 11.6 shows the evolution of the measured electrical current between anode and cathode as a function of time for several applied potential differences in three electrolyte solutions. It can be seen that for applied potential differences of less than 6V, an increase in the electrical current is detected for potentials great than 6-8 V, first an increase, followed by a decrease, is observed. The increase in current at low applied potentials (<6V) is caused by the electrodeposition of Ni(II) at the fibre surface, resulting in an increase of its conductive properties therefore more electrical current can pass the cable per time unit. After approximately 15 min, it reaches a constant value at that moment, the surface is fully covered (confirmed with X-ray photo/electron spectroscopy (XPS) analysis) with Ni. Further deposition continues but no longer affects the conductive properties of the deposited layer. 

It is evident from the above discussion that catalyst characterization is an activity important for scientific understanding, design, and troubleshooting of catalyzed processes. There is no universal recipe as to which characterization methods are more expedient than others. In the opinion of the writer, we will see continued good use of diffraction methods and electron microscopy, surface analysis, IR spectroscopy, and chemisorption methods, increased use of combined EM and ESCA analyses for determining the dopant dispersion, increased use of MAS-NMR and Raman spectroscopies for understanding of solid state chemistry of catalysts, and perhaps an increased use of methods that probe into the electronic structure of catalysts, including theory. 

A series of solid solutions (50 mole % each) was prepared from seven class I and two class II spinels. Each solid solution did stabilize catalytic activity and surface area (cf. Tables IV, I, and II). Furthermore, x-ray diffraction patterns revealed that class I spinels which did not easily form pure spinel phases readily formed a single spinel phase solid solution, e.g. the CuO Fe203 NiO A1203 system. Electron spectroscopy chemical analysis (ESCA) did not indicate any significant... 

Another theory claims that a protective complex between the metal and the CP is formed in the metal-polymer interface. Kinlen et al. [73] found by electron spectroscopy chemical analysis (ESCA) that an iron-PANl complex in the intermediate layer between the steel surface and the polymer coating is formed. By isolating the complex, it was found that the complex has an oxidation potential 250 mV more positive than PANI. According to Kinlen et al. [73], this complex more readily reduces oxygen and produces a more efficient electrocatalyst. 

Inductively Coupled Plasma. Mass Spectrometry Archaeological Applications. Microscopy Techniques Scanning Electron Microscopy. Surface Analysis X-Ray Photoelectron Spectroscopy Particle-Induced X-Ray Emission Auger Electron Spectroscopy. X-Ray Absorption and Diffraction X-Ray Diffraction - Powder. X-Ray Fluorescence and Emission X-Ray Fluorescence Theory. 

See also-. Infrared Spectroscopy Oven/iew Photother-mal. Mass Spectrometry Oven/iew Time-of-Flight. Microscopy Techniques Electron Microscopy. Surface Analysis Oven/iew. 

The application of AFM and other techniques has been discussed in general terms by several workers [350-353]. Other complementary techniques covered in these papers include FT-IR spectroscopy, Raman spectroscopy, NMR spectroscopy, surface analysis by spectroscopy, GC-MS, scanning tunnelling microscopy, electron crystallography, X-ray studies using synchrotron radiation, neutron scattering techniques, mixed crystal infrared spectroscopy, SIMS, and XPS. Applications of atomic force spectroscopy to the characterisation of the following polymers have been reported polythiophene [354], nitrile rubbers [355], perfluoro copolymers of cyclic polyisocyanurates of hexamethylene diisocyanate and isophorone diisocyanate [356], perfluorosulfonate [357], vinyl polymers... 

The Structure of the Metal-Vacuum Interface The Study of Simple Consecutive Processes in Electrochemical Reactions Surface Analysis by Electron Spectroscopy Surface-Enhanced Raman Scattering (SERS Surface Potential at Liquid Interfaces Surface States on Semiconductors... 

Madey and co-workers followed the reduction of titanium with XPS during the deposition of metal overlayers on TiOi [87]. This shows the reduction of surface TiOj molecules on adsorption of reactive metals. Film growth is readily monitored by the disappearance of the XPS signal from the underlying surface [88, 89]. This approach can be applied to polymer surfaces [90] and to determine the thickness of polymer layers on metals [91]. Because it is often used for chemical analysis, the method is sometimes referred to as electron spectroscopy for chemical analysis (ESCA). Since x-rays are very penetrating, a grazing incidence angle is often used to emphasize the contribution from the surface atoms. 

P. Echlin, ed., Analysis of Organic and Biological Surfaces, Wiley, New York, 1984. C. S. Fadley, in Electron Spectroscopy, Theory, Techniques, and Applications, Vol. 2, C. R. Brundle and A. D. Baker, eds., Pergamon, New York, 1978. 

Photoelectron spectroscopy provides a direct measure of the filled density of states of a solid. The kinetic energy distribution of the electrons that are emitted via the photoelectric effect when a sample is exposed to a monocluomatic ultraviolet (UV) or x-ray beam yields a photoelectron spectrum. Photoelectron spectroscopy not only provides the atomic composition, but also infonnation conceming the chemical enviromnent of the atoms in the near-surface region. Thus, it is probably the most popular and usefiil surface analysis teclmique. There are a number of fonus of photoelectron spectroscopy in conuuon use. 

X-ray photoelectron spectroscopy (XPS), also called electron spectroscopy for chemical analysis (ESCA), is described in section Bl.25,2.1. The most connnonly employed x-rays are the Mg Ka (1253.6 eV) and the A1 Ka (1486.6 eV) lines, which are produced from a standard x-ray tube. Peaks are seen in XPS spectra that correspond to the bound core-level electrons in the material. The intensity of each peak is proportional to the abundance of the emitting atoms in the near-surface region, while the precise binding energy of each peak depends on the chemical oxidation state and local enviromnent of the emitting atoms. The Perkin-Elmer XPS handbook contains sample spectra of each element and bindmg energies for certain compounds [58]. 

Other techniques in which incident photons excite the surface to produce detected electrons are also Hsted in Table 1. X-ray photoelectron Spectroscopy (xps), which is also known as electron spectroscopy for chemical analysis (esca), is based on the use of x-rays which stimulate atomic core level electron ejection for elemental composition information. Ultraviolet photoelectron spectroscopy (ups) is similar but uses ultraviolet photons instead of x-rays to probe atomic valence level electrons. Photons are used to stimulate desorption of ions in photon stimulated ion angular distribution (psd). Inverse photoemission (ip) occurs when electrons incident on a surface result in photon emission which is then detected. 

Analysis of Surface Elemental Composition. A very important class of surface analysis methods derives from the desire to understand what elements reside at the surface or in the near-surface region of a material. The most common techniques used for deterrnination of elemental composition are the electron spectroscopies in which electrons or x-rays are used to stimulate either electron or x-ray emission from the atoms in the surface (or near-surface region) of the sample. These electrons or x-rays are emitted with energies characteristic of the energy levels of the atoms from which they came, and therefore, contain elemental information about the surface. Only the most important electron spectroscopies will be discussed here, although an array of techniques based on either the excitation of surfaces with or the collection of electrons from the surface have been developed for the elucidation of specific information about surfaces and interfaces. 

One other very important attribute of photoemitted electrons is the dependence of their kinetic energy on chemical environment of the atom from which they originate. This feature of the photoemission process is called the chemical shift of and is the basis for chemical information about the sample. In fact, this feature of the xps experiment, first observed by Siegbahn in 1958 for a copper oxide ovedayer on a copper surface, led to his original nomenclature for this technique of electron spectroscopy for chemical analysis or esca. 

For a review of how defects manifest themselves in a LEED experiment, see M. Henzler. In Electron Spectroscopy for Surface Analysis. (H. I. Ibach, ed.) Springer, Berlin, 1977. 

Auger electron spectroscopy (AES) is a technique used to identify the elemental composition, and in many cases, the chemical bonding of the atoms in the surface region of solid samples. It can be combined with ion-beam sputtering to remove material from the surface and to continue to monitor the composition and chemistry of the remaining surface as this surface moves into the sample. It uses an electron beam as a probe of the sample surface and its output is the energy distribution of the secondary electrons released by the probe beam from the sample, although only the Ai er electron component of the secondaries is used in the analysis. 

Auger electron spectroscopy is the most frequently used surface, thin-film, or interface compositional analysis technique. This is because of its very versatile combination of attributes. It has surface specificity—a sampling depth that varies... 

PIXE detection limits for surface layers on bulk specimens are sufficiendy low to permit calibradon of true surfe.ce analysis techniques (e.g., Auger electron spectroscopy). 

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