scholarly journals In Situ Study of Graphene Oxide Quantum Dot-MoSx Nanohybrids as Hydrogen Evolution Catalysts

Surfaces ◽  
2020 ◽  
Vol 3 (2) ◽  
pp. 225-236
Author(s):  
Marco Favaro ◽  
Mattia Cattelan ◽  
Stephen W. T. Price ◽  
Andrea E. Russell ◽  
Laura Calvillo ◽  
...  

Graphene quantum dots (GOQDs)-MoSx nanohybrids with different MoSx stoichiometries (x = 2 and 3) were prepared in order to investigate their chemical stability under hydrogen evolution reaction (HER) conditions. Combined photoemission/electrochemical (XPS/EC) measurements and operando X-ray absorption spectroscopy (XAS) were employed to determine the chemical changes induced on the MoSx-based materials as a function of the applied potential. This in situ characterization indicates that both MoS2 and MoS3 materials are stable under operating conditions, although sulfur terminal sites in the MoS3 nanoparticles are converted from S-dimer (S22−) to S-monomer (S2−), which constitute the first sites where the hydrogen atoms are adsorbed for their subsequent evolution. In order to complete the characterization of the GOQDs-MoSx nanohybrids, the composition and particle size were determined by X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD) and Raman spectroscopy; whereas the HER activity was studied by conventional electrochemical techniques.

Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.


2010 ◽  
Vol 663-665 ◽  
pp. 542-545 ◽  
Author(s):  
Bing Jie Zhu ◽  
Xin Wei Wang ◽  
Mei Fang Zhu ◽  
Qing Hong Zhang ◽  
Yao Gang Li ◽  
...  

The PANI/ITO conducting nanocomposites have been synthesized by in-situ polymerization. The obtained nanocomposites were characterized by X-ray diffraction pattern, scanning electron microscopy and Fourier transform infrared. Electrical conductivity measurements on the samples pressed into pellets showed that the maximum conductivity attained 2.0 ± 0.05 S/cm for PANI/ITO nanocomposites, at ITO doping concentration of 10 wt%. The results of the present work may provide a simple, rapid and efficient approach for preparing PANI/ITO nanocomposites.


2000 ◽  
Vol 15 (7) ◽  
pp. 1617-1621 ◽  
Author(s):  
Jan Schroers ◽  
Konrad Samwer ◽  
Frigyes Szuecs ◽  
William L. Johnson

The reaction of the bulk glass forming alloy Zr41Ti14Cu12Ni10Be23 (Vit 1) with W, Ta, Mo, AlN, Al2O3, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structure and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials.


2014 ◽  
Vol 2014 ◽  
pp. 1-5
Author(s):  
Daisuke Ogawa ◽  
Ryo Kitaura ◽  
Takeshi Saito ◽  
Shinobu Aoyagi ◽  
Eiji Nishibori ◽  
...  

Thermally fragile tris(η5-cyclopentadienyl)erbium (ErCp3) molecules are encapsulated in single-wall carbon nanotubes (SWCNTs) with high yield. We realized the encapsulation of ErCp3with high filling ratio by using high quality SWCNTs at an optimized temperature under higher vacuum. Structure determination based on high-resolution transmission electron microscope observations together with the image simulations reveals the presence of almost free rotation of each ErCp3molecule in SWCNTs. The encapsulation is also confirmed by X-ray diffraction. Trivalent character of Er ions (i.e., Er3+) is confirmed by X-ray absorption spectrum.


2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.


2020 ◽  
Vol 22 (20) ◽  
pp. 11713-11723 ◽  
Author(s):  
Abhijeet Gaur ◽  
Matthias Stehle ◽  
Kristian Viegaard Raun ◽  
Joachim Thrane ◽  
Anker Degn Jensen ◽  
...  

Combination of in situ multi-edge X-ray absorption spectroscopy at the Mo K- and Fe K-edges in combination with X-ray diffraction successfully uncovered structural dynamics and phase transformations of an iron molybdate catalyst during redox cycling.


Soft Matter ◽  
2019 ◽  
Vol 15 (4) ◽  
pp. 734-743 ◽  
Author(s):  
Pinzhang Chen ◽  
Jingyun Zhao ◽  
Yuanfei Lin ◽  
Jiarui Chang ◽  
Lingpu Meng ◽  
...  

The structural evolution of NR during stretching at −40 °C and in the strain–temperature space.


2000 ◽  
Vol 07 (04) ◽  
pp. 437-446 ◽  
Author(s):  
G. RENAUD

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.


2010 ◽  
Vol 25 (8) ◽  
pp. 1601-1616 ◽  
Author(s):  
Jordi Cabana ◽  
Christopher S. Johnson ◽  
Xiao-Qing Yang ◽  
Kyung-Yoon Chung ◽  
Won-Sub Yoon ◽  
...  

The complexity of layered-spinel yLi2MnO3·(1 – y)Li1+xMn2–xO4 (Li:Mn = 1.2:1; 0 ≤ x ≤ 0.33; y ≥ 0.45) composites synthesized at different temperatures has been investigated by a combination of x-ray diffraction (XRD), x-ray absorption spectroscopy (XAS), and nuclear magnetic resonance (NMR). While the layered component does not change substantially between samples, an evolution of the spinel component from a high to a low lithium excess phase has been traced with temperature by comparing with data for pure Li1+xMn2–xO4. The changes that occur to the structure of the spinel component and to the average oxidation state of the manganese ions within the composite structure as lithium is electrochemically removed in a battery have been monitored using these techniques, in some cases in situ. Our 6Li NMR results constitute the first direct observation of lithium removal from Li2MnO3 and the formation of LiMnO2 upon lithium reinsertion.


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