In situ X-ray diffraction techniques as a powerful tool to study battery electrode materials

Raman microscopy has been used to investigate the reactions between the chemical dosants in scandium metal halide discharge lamps and their silica lamp envelopes; such lamps are typically dosed with Hg, NaI, ScI3, and sometimes, additionally, excess Sc metal. Raman measurements were made both on operated lamps and dosed silica ampoules that had been furnace heat-treated. The ampoules mimic closely the dose–envelope interactions of lamps in a convenient manner while avoiding the obscuring and complicating effects in whole-lamp studies resulting from the reactions and mobility of electrode materials. In situ Raman analyses of deposits in the envelopes and ampoules, supported by an extensive database of the Raman spectra of lamp materials, and ex situ X-ray diffraction (XRD) analyses of refractory deposits to confirm independently the Raman assignments, have demonstrated that: (1) Sc metal reacts with envelope silica to produce Sc2O3 and elemental Si; (2) Sc metal in the presence of ScI3 reacts with the envelope silica to produce Sc2Si2O7; and (3) Sc metal reacts with envelope silica in the presence of NaI alone to produce Sc2O3 and not Sc2Si2O7. The results confirm and extend previous studies and demonstrate the value of Raman microscopy as a nondestructive investigative tool for lamp chemistry.

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Battery research using synchrotron powder X-ray diffraction

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s2053273314090482 ◽

2014 ◽

Vol 70 (a1) ◽

pp. C951-C951

Author(s):

Qinfen Gu ◽

Helen Brand ◽

Justin Kimpton

Keyword(s):

Structural Changes ◽

Electrode Materials ◽

Rechargeable Batteries ◽

Ex Situ ◽

Insertion Reaction ◽

Clear Understanding ◽

X Ray Diffraction ◽

X Ray ◽

User Groups

Research and development of rechargeable batteries is critical to meet the worldwide demand for clean and sustainable energy collection and storage. A vital part of this research is to get clear understanding of how the crystal structures of electrode materials affect the the resulting properties of the batteries. As structural changes in both the anode and cathode materials play an important role in overall battery performance, synchrotron powder X-ray diffraction (PXRD), with high beam flux and resolution, is an extremely useful tool for studying the battery both in-situ and ex-situ. Several simple in-situ cell designs have been designed for synchrotron PXRD measurement. The cell is available for researchers in the field of battery research. The effectiveness and simplicity of the cell design have been demonstrated at Powder Diffraction Beamline at Australian Synchrotron for several user groups. Case studies of analysis of the lithium insertion reaction for Li0.18Sr0.66Ti0.5Nb0.5O3 defect perovskite [1], crystal structure of Li4Ti5O12–xBrx electrode material [2] and LiNi1/3Mn1/3Co1/3O2 (NMC) as a new synthesized cathode material [3] will be discussed, respectively.

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Using in situ synchrotron x-ray diffraction to study lithium- and sodium-ion batteries: A case study with an unconventional battery electrode (Gd2TiO5)

Journal of Materials Research ◽

10.1557/jmr.2014.311 ◽

2014 ◽

Vol 30 (3) ◽

pp. 381-389 ◽

Cited By ~ 9

Author(s):

James C. Pramudita ◽

Robert Aughterson ◽

Wesley M. Dose ◽

Scott W. Donne ◽

Helen E. A. Brand ◽

...

Keyword(s):

Sodium Ion ◽

Sodium Ion Batteries ◽

X Ray Diffraction ◽

X Ray ◽

Battery Electrode ◽

Image Position

Abstract

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A furnace forin situX-ray diffraction studies of insertion processes in electrode materials at elevated temperatures

Journal of Applied Crystallography ◽

10.1107/s0021889801011864 ◽

2001 ◽

Vol 34 (5) ◽

pp. 654-657 ◽

Cited By ~ 1

Author(s):

T. Eriksson ◽

A. M. Andersson ◽

Ö. Bergström ◽

K. Edström ◽

T. Gustafsson ◽

...

Keyword(s):

Structural Changes ◽

Electrode Materials ◽

Elevated Temperatures ◽

Lithium Ion ◽

X Ray Diffraction ◽

X Ray ◽

Electrochemical Cycling ◽

Flat Cell ◽

And Storage

A furnace is described forin situX-ray diffraction studies, in transmission mode, of structural changes in electrode materials for Li-ion (polymer) batteries in the ambient to 300°C temperature range. The method exploits the thin flat-cell geometry of the lithium-polymer battery concept. The flat sample is able to oscillate about a horizontal axis in its own plane in the X-ray beam, to provide better averaging during the diffraction experiment. The use of the device is demonstrated in a study of lithium intercalation in graphite (a commonly used anode material in lithium-ion batteries) during electrochemical cycling and storage at 70°C.

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The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071107 ◽

1973 ◽

Vol 31 ◽

pp. 132-133 ◽

Cited By ~ 1

Author(s):

R. E. Herfert

Keyword(s):

Surface Characterization ◽

Analytical Techniques ◽

X Ray Diffraction ◽

Depth Of Penetration ◽

X Ray ◽

The Past ◽

Transmission Electron ◽

Scanning Electron

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.

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