scholarly journals Probing the variability in oxidation states of magnetite nanoparticles by single-particle spectroscopy

2018 ◽  
Vol 6 (4) ◽  
pp. 875-882 ◽  
Author(s):  
A. Fraile Rodríguez ◽  
C. Moya ◽  
M. Escoda-Torroella ◽  
A. Romero ◽  
A. Labarta ◽  
...  

Single-particle X-ray absorption spectroscopy reveals that the oxidation state and cation distribution of individual magnetite nanoparticles may be largely heterogeneous even when the macroscopic structural and magnetic response of the ensembles is uniform.

2021 ◽  
Vol 28 (2) ◽  
pp. 455-460
Author(s):  
Suchinda Sattayaporn ◽  
Somboonsup Rodporn ◽  
Pinit Kidkhunthod ◽  
Narong Chanlek ◽  
Chutarat Yonchai ◽  
...  

A well designed compact furnace has been designed for in situ X-ray absorption spectroscopy (XAS). It enables various heat ramps from 300 K to 1473 K. The furnace consists of heaters, a quartz tube, a circulated refrigerator and a power controller. It can generate ohmic heating via an induction process with tantalum filaments. The maximum heating rate exceeds 20 K min−1. A quartz tube with gas feedthroughs allows the mixing of gases and adjustment of the flow rate. The use of this compact furnace allows in situ XAS investigations to be carried out in transmission or fluorescence modes under controlled temperature and atmosphere. Moreover, the furnace is compact, light and well compatible to XAS. The furnace was used to study cationic oxidation states in Pr6O11 and NiO compounds under elevated temperature and reduced atmosphere using the in situ X-ray absorption near-edge structure (XANES) technique at beamline 5.2 SUT-NANOTEC-SLRI of the Synchrotron Light Research Institute, Thailand. At room temperature, Pr6O11 contains a mixture of Pr3+ and Pr4+ cations, resulting in an average oxidation state of +3.67. In situ XANES spectra of Pr (L 3-edge) show that the oxidation state of Pr4+ cations was totally reduced to +3.00 at 1273 K under H2 atmosphere. Considering NiO, Ni2+ species were present under ambient conditions. At 573 K, the reduction process of Ni2+ occurred. The Ni0/Ni2+ ratio increased linearly with respect to the heating temperature. Finally, the reduction process of Ni2+ was completely finished at 770 K.


2014 ◽  
Author(s):  
A. K. Yadav ◽  
J. Jadhav ◽  
S. Biswas ◽  
S. N. Jha ◽  
D. Bhattacharyya ◽  
...  

Author(s):  
Vitaly Mesilov ◽  
Sandra Dahlin ◽  
Susanna Liljegren Bergman ◽  
Peter Sams Hammershøi ◽  
Shibo Xi ◽  
...  

In situ Cu and S K-edge X-ray absorption spectroscopy (XAS) was used for the investigation of sulfur-poisoned and regenerated Cu-SSZ-13 selective catalytic reduction (SCR) catalysts. Sulfur in the oxidation state...


2014 ◽  
Vol 43 (37) ◽  
pp. 13852 ◽  
Author(s):  
Jeremy P. Krogman ◽  
James R. Gallagher ◽  
Guanghui Zhang ◽  
Adam S. Hock ◽  
Jeffrey T. Miller ◽  
...  

2018 ◽  
Vol 936 ◽  
pp. 93-97 ◽  
Author(s):  
Irfanita Resky ◽  
Putu Eka Dharma Putra ◽  
Triono Bambang ◽  
Saiyasombat Chatree ◽  
Kamonsuangkasem Krongthong ◽  
...  

This research is aimed to examine oxidation state of Copper (Cu) in both as-synthesized and reduced T’-Pr2-xCexCuO4 (T’-PCCO) with x = 0, 0.10, and 0.15 using Cu K-edge x-ray absorption near edge structure (XANES). The T‘-PCCO nanopowders were successfully synthesized by the chemically dissolved method with HNO3 as a dissolving agent continued by calcination at 1000°C for 15 h. The reduced T’-PCCO nanopowders were obtained by reduction annealing process at 700°C for 5 h under Ar gas atmosphere. The analyses of XANES spectra show that oxidation states of the Cu ions in all of the T'-PCCO nanopowders have values between +1 and +2. This indicates the existence of electron doping in the CuO2 planes, even in the undoped T’-structure. It is found that the oxidation states of the Cu ions change after reduction annealing depending on the existence of apical oxygen in the T'-structure. Based on the XANES analyses, it is revealed that the change of oxidation state is influenced by the presence of both electron and hole carriers in the two-carrier model of T’-structure.


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