Ray Photoelectron Spectroscopy

Kerkhof and Moulijn used their method for estimating crystallite sizes 

Cocco andG. Fagherazzi,Chem. Soc., Chem. Commutu, 1978, 979. 

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Finally, similar effects can be seen in miscible polymer blends where the surface tension correlates with the enrichment of the lower-energy component at the surface as monitored by x-ray photoelectron spectroscopy [104],... 

XPS X-ray photoelectron spectroscopy [131-137] Monoenergetic x-rays eject electrons from various atomic levels the electron energy spectrum is measured Surface composition, oxidation state... 

Electronic spectra of surfaces can give information about what species are present and their valence states. X-ray photoelectron spectroscopy (XPS) and its variant, ESC A, are commonly used. Figure VIII-11 shows the application to an A1 surface and Fig. XVIII-6, to the more complicated case of Mo supported on TiOi [37] Fig. XVIII-7 shows the detection of photochemically produced Br atoms on Pt(lll) [38]. Other spectroscopies that bear on the chemical state of adsorbed species include (see Table VIII-1) photoelectron spectroscopy (PES) [39-41], angle resolved PES or ARPES [42], and Auger electron spectroscopy (AES) [43-47]. Spectroscopic detection of adsorbed hydrogen is difficult, and... 

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]. 

XPS is also often perfonned employing syncln-otron radiation as the excitation source [59]. This technique is sometimes called soft x-ray photoelectron spectroscopy (SXPS) to distinguish it from laboratory XPS. The use of syncluotron radiation has two major advantages (1) a much higher spectral resolution can be achieved and (2) the photon energy of the excitation can be adjusted which, in turn, allows for a particular electron kinetic energy to be selected. 

Powell C J, Jablonski A, Tilinin I S, Tanuma S and Penn D R 1999 Surface sensitivity of Auger-electron spectroscopy and x-ray photoelectron spectroscopy J. Eiectron Spec. Reiat. Phenom. 98-9 1... 

Powell C J 1994 Inelastic interactions of electrons with surfaces applications to Auger-electron spectroscopy and x-ray photoelectron spectroscopy Surf. Sc/. 299-300 34... 

X-ray photoelectron spectroscopy (XPS) is among the most frequently used surface chemical characterization teclmiques. Several excellent books on XPS are available [1, 2, 3, 4, 5, 6 and 7], XPS is based on the photoelectric effect an atom absorbs a photon of energy hv from an x-ray source next, a core or valence electron with bindmg energy is ejected with kinetic energy (figure Bl.25.1) ... 

XPS X-ray photoelectron spectroscopy Absorption of a photon by an atom, followed by the ejection of a core or valence electron with a characteristic binding energy. Composition, oxidation state, dispersion... 

Briggs D and Seah M P (eds) 1983 Practical Surface Analysis by Auger and X-ray Photoelectron Spectroscopy (New York Wiley)... 

Wagner C D, Riggs W M, Davis L E, Moulder J F and Muilenburg G E 1979 Handbook of X-ray Photoelectron Spectroscopy (Eden Prairie, MN Perkin Elmer)... 

McFeely and co-workers used soft x-ray photoelectron spectroscopy (SXPS) to measure the changes in binding energies of Si(2p) levels after slight exposure to fluorine atoms via dissociative chemisoriDtion of XeF2 [39]. Using synclirotron radiation at 130 eV as the source enabled extreme surface sensitivity. Since this level is split into a... 

Figure 8.1 Processes occurring in (a) ultraviolet photoelectron spectroscopy (UPS), (b) X-ray photoelectron spectroscopy (XPS) and (c) Auger electron spectroscopy (AES)...

Barr, T. L. (1994) Modern ESCA The Principles and Practice of X-ray Photoelectron Spectroscopy, CRC Press, Boca Raton, FL. 

Briggs, D. (Ed.) (1994) Practical Surface Analysis Auger and X-ray Photoelectron Spectroscopy, John Wiley, Chichester. 

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. 

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 instmmental needs required to perform such methods are similar, xps and aes instmmentation will be discussed together. 

C. D. Wagner, W. M. Riggs, L. E. Davis, andj. F. Moulder, in G. E. Muilenberg, ed.. Handbook of X-Ray Photoelectron Spectroscopy, Perkin-Elmer Corporation, Eden Prairie, Minn., 1979. 

X-rays provide an important suite of methods for nondestmctive quantitative spectrochemical analysis for elements of atomic number Z > 12. Spectroscopy iavolving x-ray absorption and emission (269—273) is discussed hereia. X-ray diffraction and electron spectroscopies such as Auger and electron spectroscopy for chemical analysis (esca) or x-ray photoelectron spectroscopy are discussed elsewhere (see X-raytechnology). 

High quahty SAMs of alkyltrichlorosilane derivatives are not simple to produce, mainly because of the need to carefully control the amount of water in solution (126,143,144). Whereas incomplete monolayers are formed in the absence of water (127,128), excess water results in facile polymerization in solution and polysiloxane deposition of the surface (133). Extraction of surface moisture, followed by OTS hydrolysis and subsequent surface adsorption, may be the mechanism of SAM formation (145). A moisture quantity of 0.15 mg/100 mL solvent has been suggested as the optimum condition for the formation of closely packed monolayers. X-ray photoelectron spectroscopy (xps) studies confirm the complete surface reaction of the —SiCl groups, upon the formation of a complete SAM (146). Infrared spectroscopy has been used to provide direct evidence for the hiU hydrolysis of methylchlorosilanes to methylsdanoles at the soHd/gas interface, by surface water on a hydrated siUca (147). 

Near edge x-ray absorption fine stmcture spectroscopy (nexafs) and x-ray photoelectron spectroscopy (xps) have been used to study SAMs of OTS, octadecyltrimethoxysilane (OTMS), CH2(CH2) ySi(OCH2)3, and (17-aminoheptadecyl)-trimethoxysilane (AHTMS), H2N(CH2) ySi(OCH3)3 (149). A number of important observations have been reported. First, the chains in OTS SAMs are practicaUy perpendicular to the substrate surface (tilt angle... 

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