In situelectrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

2017 ◽  
Vol 24 (4) ◽  
pp. 787-795 ◽  
Author(s):  
Matthias J. Young ◽  
Nicholas M. Bedford ◽  
Naisheng Jiang ◽  
Deqing Lin ◽  
Liming Dai
Keyword(s):  
Structural Changes ◽  
Active Material ◽  
High Energy ◽  
Distribution Functions ◽  
Atomic Scale ◽  
X Ray Diffraction ◽  
Active Materials ◽  
X Ray ◽  
Working Electrode ◽  
Electrochemically Active

The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurements and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.

Structural changes in titanium dioxide nanocrystals during plastic deformation

2005 ◽  
Vol 38 (5) ◽  
pp. 749-756 ◽  
Author(s):  
Ulrich Gesenhues
Keyword(s):  
Structural Changes ◽  
Crystal Size ◽  
Lower Layer ◽  
High Energy ◽  
Primary Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Hall Method ◽  
Means Of Transmission

The polygonization of 200 nm rutile crystals during dry ball-milling at 10gwas monitored in detail by means of transmission electron microscopy (TEM) and X-ray diffraction (XRD). The TEM results showed how to modify the Williamson–Hall method for a successful evaluation of crystal size and microstrain from XRD profiles. Macrostrain development was determined from the minute shift of the most intense reflection. In addition, changes in pycnometrical density were monitored. Accordingly, the primary crystal is disintegrated during milling into a mosaic of 12–35 nm pieces where the grain boundaries induce up to 1.2% microstrain in a lower layer of 6 nm thickness. Macrostrain in the interior of the crystals rises to 0.03%. The pycnometrical density, reflecting the packing density of atoms in the grain boundary, decreases steadily by 1.1%. The results bear relevance to our understanding of plastic flow and the mechanism of phase transitions of metal oxides during high-energy milling.

scholarly journals Structural Evolution in Wet Mechanically Alloyed Co-Fe-(Ta,W)-B Alloys

Metals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 800
Author(s):  
Vladimír Girman ◽  
Maksym Lisnichuk ◽  
Daria Yudina ◽  
Miloš Matvija ◽  
Pavol Sovák ◽  
...  
Keyword(s):  
Structural Changes ◽  
Magnetic Measurements ◽  
Structural Evolution ◽  
High Energy ◽  
Control Agent ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
X Ray ◽  
Transmission Electron ◽  
X Ray Absorption

In the present study, the effect of wet mechanical alloying (MA) on the glass-forming ability (GFA) of Co43Fe20X5.5B31.5 (X = Ta, W) alloys was studied. The structural evolution during MA was investigated using high-energy X-ray diffraction, X-ray absorption spectroscopy, high-resolution transmission electron microscopy and magnetic measurements. Pair distribution function and extended X-ray absorption fine structure spectroscopy were used to characterize local atomic structure at various stages of MA. Besides structural changes, the magnetic properties of both compositions were investigated employing a vibrating sample magnetometer and thermomagnetic measurements. It was shown that using hexane as a process control agent during wet MA resulted in the formation of fully amorphous Co-Fe-Ta-B powder material at a shorter milling time (100 h) as compared to dry MA. It has also been shown that substituting Ta with W effectively suppresses GFA. After 100 h of MA of Co-Fe-W-B mixture, a nanocomposite material consisting of amorphous and nanocrystalline bcc-W phase was synthesized.

scholarly journals Joint crystallization of KCuAl[PO4]2 and K(Al,Zn)2[(P,Si)O4]2: crystal chemistry and mechanism of formation of phosphate-silicate epitaxial heterostructure

2020 ◽  
Vol 76 (3) ◽  
pp. 483-491
Author(s):  
Olga Yakubovich ◽  
Galina Kiriukhina ◽  
Larisa Shvanskaya ◽  
Anatoliy Volkov ◽  
Olga Dimitrova
Keyword(s):  
Crystal Structures ◽  
Active Material ◽  
Structure Type ◽  
Structural Features ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electrochemically Active ◽  
Phosphate Silicate ◽  
The Stability ◽  
Small Channels

Two novel phases, potassium copper aluminium bis(phosphate), KCuAl[PO4]2 (I), and potassium zinc aluminium bis(phosphate-silicate), K(Al,Zn)2[(P,Si)O4]2 (II), were obtained in one hydrothermal synthesis experiment at 553 K. Their crystal structures have been studied using single-crystal X-ray diffraction. (I) is a new member of the A + M 2+ M 3+[PO4]2 family. Its open 3D framework built by AlO5 and PO4 polyhedra includes small channels populated by columns of CuO6 octahedra sharing edges, and large channels where K+ ions are deposited. It is assumed that the stability of this structure type is due to the pair substitution of Cu/Al with Ni/Fe, Co/Fe or Mg/Fe in different representatives of the series. From the KCuAl[PO4]2 structural features, one may suppose it is a potentially electrochemically active material and/or possible low-temperature antiferromagnet. In accordance with results obtained from X-ray diffraction data, using scanning electron microscopy, microprobe analysis and detailed crystal chemical observation, (II) is considered as a product of epitaxial intergrowth of phosphate KAlZn[PO4]2 and silicate KAlSi[SiO4]2 components having closely similar crystal structures. The assembly of `coherent intergrowth' is described in the framework of a single diffraction pattern.

Atomic-Scale Structure of Polymer-Route Si-C-O Fibers Observed by Synchrotron Radiation X-Ray Diffraction

2007 ◽  
Vol 352 ◽  
pp. 65-68 ◽  
Author(s):  
Kiyohito Okamura ◽  
Kentaro Suzuya ◽  
Shinji Kohara ◽  
Hiroshi Ichikawa ◽  
Kenji Suzuki
Keyword(s):  
Synchrotron Radiation ◽  
Network Structure ◽  
High Energy ◽  
Scale Structure ◽  
Atomic Scale ◽  
Intermediate Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atomic Scale Structure ◽  
Amorphous Sic

The atomic scale structure of amorphous Si-C-O ceramics fibers produced from the pyrolysis of a polycarbosilane precursor has been investigated by X-ray diffraction using high-energy synchrotron radiation at SPring-8. First peak in the total correlation function T(r) of the amorphous and the heat-treated fibers is analyzed to consist of two contributions: Si-C (1.89 Å) and Si-O (1.61 Å) bonds. The coordination number of C and/or O around Si is about four. This suggests that the Si-C-O fibers basically have a network structure that consists of two tetrahedral units: SiC4 and SiO4. The local chemical and structural orders vary continuously in the materials from the disordered network structure of SiC4 and SiO4 tetrahedra (mixture of amorphous SiC and SiO2) to nanocrystals of SiC and SiO2, through the ternary Si-C-O solid solution which is believed to have an intermediate structure between the amorphous and crystalline states.

Synthesis of Nanocrystalline Fe25Al57.5Ni17.5 by Mechanical Alloying

2012 ◽  
Vol 476-478 ◽  
pp. 1318-1321
Author(s):  
Qi Zhi Cao ◽  
Jing Zhang
Keyword(s):  
Thermal Analysis ◽  
Solid Solution ◽  
Differential Thermal Analysis ◽  
Mechanical Alloying ◽  
Ball Mill ◽  
Structural Changes ◽  
Early Stage ◽  
High Energy ◽  
X Ray Diffraction ◽  
X Ray

Nanostructured Fe25Al57.5Ni17.5intermetallics was prepared directly by mechanical alloying (MA) in a high-energy planetary ball-mill. The phase transformations and structural changes occurring in the studied material during mechanical alloying were investigated by X-ray diffraction (XRD). Thermal behavior of the milled powders was examined by differential thermal analysis (DTA). Disordered Al(Fe,Ni) solid solution was formed at the early stage. After 50 h of milling, Al(Fe,Ni) solid solution transformed into Al3Ni2，AlFe3，AlFe0.23Ni0.77 phase. The power annealed at temperature 500 results in forming of intermetallics AlFe3 and FeNi3 after 5h milling. The nanocrystalline intermetallic compound was obtained after 500h milling.

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