A double-focusing electrostatic electron spectrometer has been used to measure the K—LL Auger spectra resulting from electron impact for each of the elements in the gaseous molecules N2, O2, CO, NO, H2O, and CO2. An energy resolution of 0.09% full width half-maximum was normally employed. A method for analyzing these complex spectra is described. It involves the identification of normal and satellite lines. The former are defined as arising from single electron ionization from the K shell without additional excitation followed by an Auger process in which one electron fills the vacancy while a second goes into the continuum, and where all the other electrons remain in their same orbitals. Satellite lines result when extra excitation occurs either in the initial formation of the K vacancy or in the subsequent Auger process. To aid in the identification of these satellite lines, auxiliary experiments have been performed such as the study of discrete energy losses in photoionization due to electron shake-up, and the comparison of Auger spectra produced by monoenergetic x rays. As a consequence of the analyses of the Auger spectra, information has been obtained on (1) the nature of initial excitation processes such as the transition of a K electron into excited discrete states and monopole excitation and (2) the identification of the energy and nature of the ground and excited states of the doubly charged molecular ions. The second ionization potential was obtained for each of the molecules, and in one case, N2, the third ionization potential was estimated. Finally, a brief discussion is made of the possible use of high resolution electron spectroscopy in molecular as well as elemental analysis.
The energies of the 3da/, and 3da/, levels have been determined for palladium and 13 of its compounds. The measured energies are related t o electronegativity differences between the palladium and the ligand donor atoms except in those cases where the ligand is a ?r acceptor. Ligands which are K acceptors cause greater energy level shifts since they permit greater depletion of electronic charge from the palladium. The energies of the K(2s) and P(2p) levels measured for several complexes were found to be nearly constant. The energy of the Br(3ps/,) level was lowered somewhat when the bromine occupied a bridging position in PdBrZ. The observed shifts can be "explained" by a combination of electronegativity and ?r-bonding effects. T h e cobalt(II1) complex L' = [Co( (C~H~)ZP(CHZ)ZP(C~H;)Z}Z(CN)Z] + acts as positively charged ligand giving compounds of the stoichiometry M(L+)XI, where M = Mn(II), F e ( I I ) , Co(II), N i ( I I ) , or Zn(I1) and X = halogen or pseudohalogen.On the basis of their electronic and vibrational spectra, magnetic susceptibilities, and X-ray diffraction patterns, these compounds zre formulated as pseudotetrahedral zwitterion complexes in which the cobalt(II1) cation is bound to MX3moieties through the nitrogen atom of one cyanide group.
An electron spectrometer which employs double focusing electrostatic plates is described. The photoelectron spectra obtained by bombarding methane, silane, germane, methyl fluoride, difluoromethane, and trifluoromethane with 21.22-eV photons are presented. The experimental ionization energies are compared with theoretical and other experimental data, and molecular-orbital assignments are made for the energy values obtained. Broad double maximum bands were observed in the case of methane, silane, and germane and are discussed in terms of Jahn–Teller distortion for the positive ions. Possible correlation of the methane spectrum with interstellar space data is also discussed.
Mound Laboratories has been investigating pyrotechnic materials for several years. Prior studies on the mechanism of ignition have been performed on Ti/KCIO, and Ti/ZB mixtures. Tbese studies have shown the importance of the surface oxides of these materials in determining the mechanism of ignition. In the present study, XPS spectra of fused metal, oxidized fused boron and boron metal powder have been recorded. The spectra are interpeted by including the presence of a continuous boron suboxide layer. The results presented here are different from those previously reported, which suggests that the formation of boron oxide occurs in islets. The predominant suboxide will be shown to be B,O,, where x/y = 3. This oxide was found to be present independent of the degree of oxidation. Including this oxide in thickness calculations shows the oxidation of powders to be five layers or so thick, and also aids in understanding Ti/ZB ignition.
Titanium-boron pyrotechnic reactions are essentially gasless, are very exothermic, and are known to initiate only at extremely high temperatures. The reactants are stable in normal laboratory environments and require no special sample handling, such as inert storage. These factors make the titaniundboron mixture ideal for one-shot thermal heat source applications. Mound has been investigating energetic material ignition properties for a number of years. Pyrotechnic mixtures of TiH,/KCIO, have revealed that the surface composition of the titanium fuel was TiO, and its presence on the fuel's surface controls the TiH, + KCIO, reaction. In the present study the surface chemistry of titanium and of boron have been examined before ignition. To understand the effect of temperature on the reactants and the mixture, titanium powder, boron powder, and blends were analyzed at ambient and elevated temperatures. XPS, TG and DTA results presented will show that the oxide on boron is the controlling factor in the ignition mechanism of the titanium-boron pyrotechnic reaction.
Palladium metal powders used for hydrogen isotope pumping were studied for their bulk and surface chemistry changes during cleaning with hydrogen gas at 150 O C . Cleaning is necessary to promote rapid hydriding and dehydriding and to prevent contaminant ingrowth in the process gas during use. These studies show that heating the powders in vacuum at moderate temperatures (15OOC) in a reducing environment removes surface oxide, leaves a predominately palladium metal surface which presents no significant barrier to hydrogen absorption or desorption, and shows no loss in surface area and pourability. A surface model of PdO is given and XPS results show that the water-forming reaction is the mode of PdO reduction. Thermodynamic data are discussed which support the above results.
Rksumk. -Utilisant comme exemple le spectre Auger du neon, il est montre que le spectre Auger renferme des informations precises sur I'interaction du rayonnement, ou des particules, avec les electrons du cortege klectronique et sur les mCcanisrnes d'interaction electron-electron dans I'atorne ionise dans ses couches internes. On peut differencier les processus d'ionisation simple, d'ionisation double, d'ionisation-excitation, etc. Environ 90 lignes du spectre du neon sont classifrees d'aprks ces processus fondamentaux. Les energies et les intensites relatives des lignes appartenant aux diffkrents processus sont presentees et cornparks avec la theorie et des resultats d'autres experiences. La dkpendance du spectre au mode d'excitation est discutee.Abstract. -Using the neon Auger spectrum as an example, Auger spectra are shown to yield W, m.Article published online by EDP Sciences and available at http://dx.
DiscussionThe chemistry and structural data for oxygencarrying (p-peroxo) cobalt-histidine complexes and related substances have been previously summarized. lo In the present work, we have characterized the first known p-superoxo-dicobalt ion containing histidine as ligands. The presence of this bridge is clearly indicated by both the optical spectrum (678-nm peak) and the epr characteristics.1°
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