scholarly journals Soft X-ray Transmission Microscopy on Lithium-Rich Layered-Oxide Cathode Materials

2021 ◽  
Vol 11 (6) ◽  
pp. 2791
Author(s):  
Andrea Sorrentino ◽  
Laura Simonelli ◽  
Arefehsadat Kazzazi ◽  
Nina Laszczynski ◽  
Agnese Birrozzi ◽  
...  

Energy-dependent full field transmission soft X-ray microscopy (TXM) is able to give a full picture at the nanometer scale of the chemical state and spatial distribution of oxygen and other elements relevant for battery materials, providing pixel-by-pixel absorption spectrum. We show different methods to localize chemical inhomogeneities in Li1.2Mn0.56Ni0.16Co0.08O2 particles with and without VOx coating extracted from electrodes at different states of charge. Considering the 3d(Mn,Ni)-2p(O) hybridization, it has been possible to discriminate the chemical state of Mn and Ni in addition to the one of O. Different oxidation states correspond to specific features in the O-K spectra. To localize sample regions with specific compositions we apply two different methods. In the first, the pixel-by-pixel ratios of images collected at different key energies clearly highlight local inhomogeneities. In the second, introduced here for the first time, we directly correlate corresponding pixels of the two images on a xy scatter plot that we call phase map, where we can visualize the distributions as function of thickness as well as absorption artifacts. We can select groups of pixels, and then map regions with similar spectral features. Core-shell distributions of composition are clearly shown in these samples. The coating appears in part to frustrate some of the usual chemical evolution. In addition, we could directly observe several further aspects, such as: distribution of conducting carbon; inhomogeneous state of charge within the electrode; molecular oxygen profiles within a particle. The latter suggests a surface loss with respect to the bulk but an accumulation layer at intermediate depth that could be assigned to retained O2.

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1229-1236
Author(s):  
Matthias Wörsching ◽  
Constantin Hoch

Abstract Cesium hydroxide, CsOH, was for the first time characterised on the basis of single-crystal data. The structure is isotypic to the one of the room-temperature modification of NaOH and can be derived from the NaCl structure type thus allowing the comparison of all alkali metal hydroxide structures. Raman spectroscopic investigations show the hydroxide anion to behave almost as a free ion as in the gas phase. The X-ray investigations indicate possible H atom positions.


2019 ◽  
Vol 10 (1) ◽  
Author(s):  
Benedikt Günther ◽  
Lorenz Hehn ◽  
Christoph Jud ◽  
Alexander Hipp ◽  
Martin Dierolf ◽  
...  

2017 ◽  
Vol 32 (2) ◽  
pp. 402-407 ◽  
Author(s):  
J. J. Leani ◽  
R. D. Pérez ◽  
J. I. Robledo ◽  
H. J. Sánchez

X-ray resonant Raman scattering was used, for the first time, in a confocal setup with the aim of determining different compounds of the same element in a copper-multilayer sample.


Author(s):  
Alexander M. Antipin ◽  
Natalia I. Sorokina ◽  
Olga A. Alekseeva ◽  
Alexandra N. Kuskova ◽  
Elena P. Kharitonova ◽  
...  

A single crystal of Nd5Mo3O16with lead partly substituting for neodymium, which has a fluorite-like structure, was studied by precision X-ray diffraction, high-resolution transmission microscopy and EDX microanalysis. The crystal structure is determined in the space group Pn\bar 3n. It was found that the Pb atoms substitute in part for Nd atoms in the structure and are located in the vicinity of Nd2 positions. Partial substitutions of Mo cations for Nd positions and of Nd for Mo positions in crystals of theLn5Mo3O16oxide family are corroborated by X-ray diffraction for the first time. The first experimental verification of the location of an additional oxygen ion in the voids abutting MoO4tetrahedra was obtained.


2015 ◽  
Vol 9 (1) ◽  
pp. 2299-2302
Author(s):  
GülÅŸah çelik gül ◽  
Figen KurtuluÅŸ

Anode materials with high storage capacity and high power density attract considerable interest because of recent advances in Li-ion battery used electronic devices. Vanadium based oxides are the one possible group. LiV2O5 was synthesized by hydrothermal method at 3 days (72 hours) and 180 ºC. Structural characterization was performed by powder X-ray diffractometer and fourier transform infrared spectroscopy. Morphology was scanned by scanning electron microscopy with energy disperse X-ray analysis. The first time synthesized material is crstallisized in orthorombic system with unit cell parameters a = 11.31, b = 9.552, c = 3.585 Å and space group Pmn21 (31). 


Molecules ◽  
2019 ◽  
Vol 24 (23) ◽  
pp. 4252 ◽  
Author(s):  
Rungthip Kunthom ◽  
Nobuhiro Takeda ◽  
Masafumi Unno

The one-pot synthesis of an unsymmetrical double-decker siloxane with a novel structure via the reaction of double-decker tetrasodiumsilanolate with 1 equiv. of dichlorotetraphenyldisiloxane in the presence of an acid is reported herein for the first time. The target compound bearing all phenyl substituents on the unsymmetrical siloxane structure was successfully obtained, as confirmed by 1H-NMR, 13C-NMR, 29Si-NMR, IR, MALDI-TOF, and X-ray crystallography analyses. Additionally, the thermal properties of the product were evaluated by TG/DTA and compared with those of other siloxane cage compounds.


Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5022
Author(s):  
Joanna Czerwik-Marcinkowska ◽  
Renata Piwowarczyk ◽  
Bohuslav Uher ◽  
Ewa Tomal ◽  
Anna Wojciechowska

The paper presents four new sites where bright green Ulva thalli were found inhabiting freshwater (a river, a ditch, the Milet Canal) and marine (on the rocky shore of the Adriatic Sea) habitats in Montenegro. The aims of this study were to determine, for the first time, whether specimens of Ulva pilifera collected in Montenegro are phylogenetically and morphologically the same species as the one occurring in Europe. Using total reflection X-ray fluorescence (TXRF) and wavelength dispersive X-ray fluorescence (WDXRF) techniques it assessed the elemental composition of their thalli and its influence to colonise new habitats. Elements: Al, As, Ba, Br, Ca, Cl, Cr, Cu, Fe, Hf, I, K, Mg, Mn, Na, Ni, P, Pb, Rb, S, Si, Sr, Ti, V, and Zn were determined. The highest elemental concentrations were found for Ca = 16.3% (using WDXRF) and for Sr = 292 ppm (using TXRF) in the Ulva thalli. Ulva pilifera analysed from Montenegro, based on classical morphological methods and molecular techniques, are closely related to the same species from inland and coastal waters throughout Europe. The analysis of trace elements showed that the metal content in Ulva thalli is correlated with the trace elements in water and sediments. Ulva pilifera fits numerous features that make it one of the bioindicators of marine pollution, thanks to its worldwide distribution and capacity to accumulate trace elements.


2012 ◽  
Vol 19 (5) ◽  
pp. 705-709 ◽  
Author(s):  
Joan Vila-Comamala ◽  
Yongsheng Pan ◽  
Jeffrey J. Lombardo ◽  
William M. Harris ◽  
Wilson K. S. Chiu ◽  
...  

2017 ◽  
Vol 359 ◽  
pp. 234-241 ◽  
Author(s):  
Mara Olivares-Marín ◽  
Andrea Sorrentino ◽  
Eva Pereiro ◽  
Dino Tonti

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