X-Ray Photoelectron Spectroscopy

The interaction of photon and the electron goes back to the early part of 19th century emanating from the photo-electric effect depicted by none other than Albert Einstein (Ref 1) described in 1905, and the redistribution of kinetic energy resulting from the interaction of x-ray and solids reported during early part of the century (Ref.2). The spectrum resolutions obtained at that time was not sufficient to observe distinct peaks in spectra for materials. Thus, these phenomena hardly attracted any attention for many years following these discoveries. The modern X-ray Photoelectron Spectroscopy (XPS) has been possible by the extensive and significant contribution from Kai Siegbahn and others (Ref.3, 4) of Uppsala University. Siegbahn developed and employed a high-resolution electron spectrometer that revealed electron peaks in a spectrum emerging from the interaction of x-rays and solids. Eventually, Kai Siegbahn received Nobel Prize in 1981 for his contributions to XPS. Around 1958, shifts in elemental peaks were realized in compounds when the same elements are bound to other but different elements. This discovery resulted in the chemical state identification in various chemicals as well as the oxidation states of atoms in compounds. Because of these useful physical effects, the Uppsala group named XPS with a synonymous name of ESCA (Electron Spectroscopy for Chemical Analysis) used widely today and will be used here alternatively. Therefore, XPS or ESCA not only identifies the element, but also the compound these elements form, from their chemical shifts. Compared to other micro-analytical techniques such as Energy Dispersive (EDS) or Wavelength Dispersive (WDS) techniques, XPS analyzes only few atomic layers present on the surface. This was discovered early in 1966 (Ref. 5). While this has awarded a merit to the analytical technique to analyze very thin layers such as films and coatings, it often analyzes the adsorbed superficial gases and contaminations on a sample introduced to its analytical chamber. This necessitates the surface is cleaned and the underlying material, material of interest, is exposed in a clean environment such that the material of interest is analyzed. The cleaning is accomplished by a scanning ion gun within the analytical chamber of the instrument. Ion gun uses an argon gas and is commonly attached in most modern machines. Reliable and efficient vacuum systems employed in modern machines does not allow adsorbed layers to rebuild after the surface is cleaned. Development of efficient and reliable vacuum pumps over these developmental years is yet another important step in the commercialization of XPS machines. Vacuum levels of better than 10-7 torr are essential to increase the mean free path of electrons released from the sample surface. Thus, modern machines are equipped with high capacity ion, turbo or cryogenic pumps in their analytical chambers. Today, XPS has advanced from an applied physics laboratory to industry for use in quality control as well as analysis of contaminants and has taken a dominant role in microanalysis. Its uniqueness arises from the fact that it is considered non-destructive compared to other common micro-analytical techniques using the electron and ion excitation sources. Polymers and plastics could be analyzed since the binding energies of saturated and unsaturated bonds in atoms could be separated. Extremely thin layers could be analyzed including materials with layered structures. The technique, though did not advance for many years, has now opened a new window for research as well as applications in industry due to its ability to separate and measure the chemical shifts in bound elements. Principle

Investigation of work function and chemical composition of thin films of borides and nitrides

Thin films of various borides, nitrides, and barium fluorides were tentatively deposited by pulsed laser deposition and by magnetron sputtering in order to develop the components of thermionic-photovoltaic devices for the high-temperature thermal to electrical conversion by solid state. To improve the device performance, the materials characterized by a low work function were selected. In the present work, the chemical composition and work function of obtained films were investigated by X-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy techniques. The values of work function were determined from the cut-off in the He I valence band spectra. Different films were compared and estimated on the basis of X-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy results

Surface properties of SmB6 from x-ray photoelectron spectroscopy

We have investigated the properties of cleaved SmB$_6$ single crystals by x-ray photoelectron spectroscopy. At low temperatures and freshly cleaved samples a surface core level shift is observed which vanishes when the temperature is increased. A Sm valence between 2.5 - 2.6 is derived from the relative intensities of the Sm$^{2+}$ and Sm$^{3+}$ multiplets. The B/Sm intensity ratio obtained from the core levels is always larger than the stoichiometric value. Possible reasons for this deviation are discussed. The B $1s$ signal shows an unexpected complexity: an anomalous low energy component appears with increasing temperature and is assigned to the formation of a suboxide at the surface. While several interesting intrinsic and extrinsic properties of the SmB$_6$ surface are elucidated in this manuscript no clear indication of a trivial mechanism for the prominent surface conductivity is found

Valence band offset of InN/AlN heterojunctions measured by X-ray photoelectron spectroscopy

The valence band offset of wurtzite-InN/AlN (0001) heterojunctions is determined by x-ray photoelectron spectroscopy to be 1.52±0.17 eV. Together with the resulting conduction band offset of 4.0±0.2 eV, a type-I heterojunction forms between InN and AlN in the straddling arrangement

Fortran Program for X-Ray Photoelectron Spectroscopy Data Reformatting

A FORTRAN program has been written for use on an IBM PC/XT or AT or compatible microcomputer (personal computer, PC) that converts a column of ASCII-format numbers into a binary-format file suitable for interactive analysis on a Digital Equipment Corporation (DEC) computer running the VGS-5000 Enhanced Data Processing (EDP) software package. The incompatible floating-point number representations of the two computers were compared, and a subroutine was created to correctly store floating-point numbers on the IBM PC, which can be directly read by the DEC computer. Any file transfer protocol having provision for binary data can be used to transmit the resulting file from the PC to the DEC machine. The data file header required by the EDP programs for an x ray photoelectron spectrum is also written to the file. The user is prompted for the relevant experimental parameters, which are then properly coded into the format used internally by all of the VGS-5000 series EDP packages

Thin films of AlCrFeCoNiCu high-entropy alloy by pulsed laser deposition

Pulsed laser deposition has been used to prepare thin films of the high entropy alloy AlCrFeCoNiCu. The 35 nm films were deposited in ultra-high vacuum onto glass at room temperature and above and analysed using X-ray diffraction and X-ray photoelectron spectroscopy. Films deposited at room temperature exhibit a mix of FCC and BCC reflections, the FCC crystallites having size similar to the film thickness, but the BCC crystallites are larger. The intensity of the reflections from both crystal structures reduce with increasing deposition temperature, the fall in BCC commencing at lower temperature than the FCC associated with a reduction of the content of Al and Cu. X-ray photoelectron spectroscopy shows that the films deposited at room temperature are closer to stoichiometry than those at higher temperatures. An important feature of the X-ray photoelectron spectroscopy depth profiles is surface segregation, the outer 3 nm of the high entropy alloy films has higher concentration of Al and, to a lesser extent, Cr

Synthesis and structure of the inclusion complex {NdQ[5]K@Q[10](H₂O)4}·4NO₃·20H₂O

Heating a mixture of Nd(NO₃)₃·6H₂O, KCl, Q[10] and Q[5] in HCl for 10 min affords the inclusion complex {NdQ[5]K@Q[10](H₂O)₄}·4NO₃·20H₂O. The structure of the inclusion complex has been investigated by single crystal X-ray diffraction and by X-ray Photoelectron spectroscopy (XPS)