Structure and photoinduced structural changes in nonstoichiometrica-AsxS1−x: A study by x-ray-absorption fine structure

1992 ◽  
Vol 46 (7) ◽  
pp. 3817-3825 ◽  
Author(s):  
Weiqing Zhou ◽  
M. A. Paesler ◽  
D. E. Sayers
Minerals ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 267 ◽  
Author(s):  
Tatsuya Kato ◽  
Yuki Tsunazawa ◽  
Wenying Liu ◽  
Chiharu Tokoro

Prolonged high-intensity grinding can modify the crystal structure of solid substances and/or induce chemical reaction, which is referred to as mechanochemical reaction. Such reactions can exert positive influences on hydrometallurgical processes, therefore, many researchers have applied mechanochemical reactions for metals dissolution from minerals. The mechanism of mechanochemical reaction has been investigated using solid analyses and simulations. Structural changes caused by mechanochemical reactions are not yet sufficiently clarified because the ground samples are amorphous. The objective of this study was to analyze structural changes of cerianite in weathered residual rare earth ore by mechanochemical reduction. The ore was ground by planetary ball milling for 10, 60 and 720 min. Structural change was analyzed by the X-ray absorption near-edge structure and extended x-ray absorption fine structure analysis at the cerium LIII- and K-edges. These analyses revealed that the structural change of cerianite in this ore induced by mechanochemical reduction involved oxygen vacancy production. The process of the oxygen vacancy formation was closely coupled with the quantum effect of localization–delocalization of the 4f electron of cerium.


1977 ◽  
Vol 55 (11) ◽  
pp. 1968-1974 ◽  
Author(s):  
E. D. Crozier ◽  
F. W. Lytle ◽  
D. E. Sayers ◽  
E. A. Stern

The extended fine structure in the X-ray absorption coefficient is dominated by the interference of the photoelectron scattered by atoms in the immediate neighbourhood of the atom which absorbs the X-ray photon and thus can provide structural information about ordered or disordered systems. In this paper it is demonstrated that Extended X-Ray Absorption Fine Structure (EXAFS) measurements can be made on liquid systems at high temperatures. The technique is illustrated with results for As2Se3 in the liquid and amorphous states for temperatures between 100 and 773 K. A Fourier analysis of the EXAFS data reveals that a major structural rearrangement does not occur in the nearest neighbour shell when As2Se3 is melted. However, small structural changes do occur at the melting point which, within the limitations of the present data, suggest a slight increase in the nearest neighbour As–Se distance, a decrease in the number of nearest neighbours, and a decrease in the nearest neighbour disorder term σ12.


Author(s):  
Tatsuya Kato ◽  
Yuki Tsunazawa ◽  
Wenying Liu ◽  
Chiharu Tokoro

Prolonged high-intensity grinding can modify the crystal structure of solid substances and/or induce chemical reaction, which is referred to as mechanochemical reaction. Such reactions can exert positive influences on hydrometallurgical processes, therefore, many researchers have applied mechanochemical reactions for metals dissolution from minerals. The mechanism of mechanochemical reaction has been investigated using solid analyses and simulations. Structural changes caused by mechanochemical reaction are not yet sufficiently clarified because the ground samples are amorphous. The objective of this study was to analyze structural changes of cerianite in weathered residual rare earth ore by mechanochemical reduction. Structural change was analyzed by x-ray absorption near-edge structure and extended x-ray absorption fine structure analysis at the cerium LIII- and K-edges. These analyses revealed that the structural change of cerianite in this ore induced by mechanochemical reduction involved oxygen vacancy production. The process of the oxygen vacancy formation was closely coupled with the quantum effect of localization–delocalization of the 4f electron of cerium.


2003 ◽  
Vol 251 (1-4) ◽  
pp. 408-411 ◽  
Author(s):  
Vincent Gambin ◽  
Vincenzo Lordi ◽  
Wonill Ha ◽  
Mark Wistey ◽  
Toshiyuki Takizawa ◽  
...  

1998 ◽  
Vol 05 (05) ◽  
pp. 1057-1086 ◽  
Author(s):  
P. S. Mangat ◽  
P. Soukiassian

Extended X-ray absorption fine structure (EXAFS) has been known for half a century. However, using synchrotron radiation, it has developed into a powerful tool for determining the atomic structure of a wide variety of surfaces and interfaces. The power of this technique lies in its sensitivity to the local environment of a particular element. Photoemission extended X-ray absorption fine structure (PEXAFS) is a new variation of electron detection surface EXAFS (SEXAFS) using photoemission spectroscopy in the constant initial state mode, Due to small escape depths, a very high surface sensitivity is achieved. Other major advantages of this new technique include (i) an improved signal/noise ratio allowing very short data collection times, which is an especially useful feature for short lifetime surfaces, and (ii) double-checking interatomic distances. Combined with core level and valence band photoemission spectroscopies. PEXAFS provides the exceptional ability to probe the atomic geometry and the electronic structure at the same time and for the same surface. It thus gives access to important issues, such as (i) surface reconstruction and/or relaxation, (ii) bonding nature, (iii) adsorption site and (iv) initial interface formation. Furthermore, it could be used to clarify photoemission core level shift origin by allowing one to discriminate structural changes from other causes as initial or final state effects. This article reviews the latest PEXAFS investigations for model elemental (silicon) and compound (indium phosphide) semiconductor surfaces and their interfaces with alkali metals, antimony, aluminum, bismuth and silver.


2021 ◽  
Vol 28 (1) ◽  
pp. 266-277
Author(s):  
Jonas Klaes ◽  
Patrick Rothweiler ◽  
Benjamin Bornmann ◽  
Ralph Wagner ◽  
Dirk Lützenkirchen-Hecht

Niobium metal foils were heat-treated at 900°C under different conditions and in situ investigated with time-resolved X-ray absorption fine-structure (EXAFS and XANES) measurements. The present study aims to mimic the conditions usually applied for heat treatments of Nb materials used for superconducting radiofrequency cavities, in order to better understand the evolving processes during vacuum annealing as well as for heat treatments in controlled dilute gases. Annealing in vacuum in a commercially available cell showed a substantial amount of oxidation, so that a designated new cell was designed and realized, allowing treatments under clean high-vacuum conditions as well as under well controllable gas atmospheres. The experiments performed under vacuum demonstrated that the original structure of the Nb foils is preserved, while a detailed evaluation of the X-ray absorption fine-structure data acquired during treatments in dilute air atmospheres (10−5 mbar to 10−3 mbar) revealed a linear oxidation with the time of the treatment, and an oxidation rate proportional to the oxygen (air) pressure. The structure of the oxide appears to be very similar to that of polycrystalline NbO. The cell also permits controlled exposures to other reactive gases at elevated temperatures; here the Nb foils were exposed to dilute nitrogen atmospheres after a pre-conditioning of the studied Nb material for one hour under high-vacuum conditions, in order to imitate typical conditions used for nitrogen doping of cavity materials. Clear structural changes induced by the N2 exposure were found; however, no evidence for the formation of niobium nitride could be derived from the EXAFS and XANES experiments. The presented results establish the feasibility to study the structural changes of the Nb materials in situ during heat treatments in reactive gases with temporal resolution, which are important to better understand the underlaying mechanisms and the dynamics of phase formation during those heat treatments in more detail.


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