scholarly journals Aging and Charge Compensation Effects of the Rechargeable Aqueous Zinc/Copper Hexacyanoferrate Battery Elucidated Using In Situ X-ray Techniques

2021 ◽  
Author(s):  
Mikaela Görlin ◽  
Dickson O. Ojwang ◽  
Ming-Tao Lee ◽  
Viktor Renman ◽  
Cheuk-Wai Tai ◽  
...  
Keyword(s):  
Charge Compensation ◽  
Copper Hexacyanoferrate ◽  
X Ray

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

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
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.

In Situ X-Ray Absorption Studies of the Electrochemical Reduction of Hydroxocobalamin

1997 ◽  
Vol 7 (C2) ◽  
pp. C2-619-C2-620 ◽  
Author(s):  
M. Giorgett ◽  
I. Ascone ◽  
M. Berrettoni ◽  
S. Zamponi ◽  
R. Marassi
Keyword(s):  
Electrochemical Reduction ◽  
X Ray ◽  
Absorption Studies ◽  
X Ray Absorption

A Revised O2 Reduction Model in Li-O2 Batteries as Revealed by in Situ Small Angle X-Ray Scattering

2019 ◽  
Author(s):  
Christian Prehal ◽  
Aleksej Samojlov ◽  
Manfred Nachtnebel ◽  
Manfred Kriechbaum ◽  
Heinz Amenitsch ◽  
...  
Keyword(s):  
Small Angle ◽  
Wide Angle ◽  
Reduction Mechanism ◽  
Reduction Model ◽  
X Ray ◽  
X Ray Scattering ◽  
O2 Reduction ◽  
Ray Scattering

<b>Here we use in situ small and wide angle X-ray scattering to elucidate unexpected mechanistic insights of the O2 reduction mechanism in Li-O2 batteries.<br></b>

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Anionic and Cationic Redox Processes in β-Li2IrO3 and Their Structural Implications on Electrochemical Cycling in Li-Ion Cell

2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  
Keyword(s):  
Analytical Techniques ◽  
Charge Compensation ◽  
Coupling Mechanism ◽  
Redox Processes ◽  
Positive Electrodes ◽  
X Ray ◽  
Electrochemical Cycling ◽  
Li Ion ◽  
Electrochemical Instability ◽  
High Degree

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>

Anionic and Cationic Redox Processes in β-Li2IrO3 and Their Structural Implications on Electrochemical Cycling in Li-Ion Cell

2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  
Keyword(s):  
Analytical Techniques ◽  
Charge Compensation ◽  
Coupling Mechanism ◽  
Redox Processes ◽  
Positive Electrodes ◽  
X Ray ◽  
Electrochemical Cycling ◽  
Li Ion ◽  
Electrochemical Instability ◽  
High Degree

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>

Monitoring Polymer-Assisted Mechanochemical Cocrystallisation Through in Situ X-Ray Powder Diffraction

2020 ◽  
Author(s):  
Luzia S. Germann ◽  
Sebastian T. Emmerling ◽  
Manuel Wilke ◽  
Robert E. Dinnebier ◽  
Mariarosa Moneghini ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Powder Diffraction ◽  
Reaction Rate ◽  
Polymer Additives ◽  
Time Resolved ◽  
X Ray

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the monitoring of polymer-assisted grinding reactions using <i>in situ</i> X-ray powder diffraction, revealing that reaction rate is almost double compared to neat grinding and independent of the molecular weight and amount of used polymer additives.<br>

Atomic Layer Deposition of LiF and Lithium Ion Conducting (AlF3)(LiF)x Alloys Using Trimethylaluminum, Lithium Hexamethyldisilazide and Hydrogen Fluoride

2017 ◽  
Author(s):  
Younghee Lee ◽  
Daniela M. Piper ◽  
Andrew S. Cavanagh ◽  
Matthias J. Young ◽  
Se-Hee Lee ◽  
...  
Keyword(s):  
Lithium Ion ◽  
Atomic Layer ◽  
Mass Gain ◽  
Alloy Film ◽  
Ex Situ ◽  
X Ray ◽  
Layer Deposition ◽  
Ion Conducting ◽  
Good Agreement

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH<sub>3</sub>)<sub>3</sub> as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF<sub>3</sub> and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF<sub>3</sub>)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film was measured as σ = 7.5 × 10<sup>-6</sup> S/cm.</div>

In situ Time-Resolved Small-Angle X-ray Scattering Reveals the Formation Kinetics of Polyelectrolyte Complex Micelles

2019 ◽  
Author(s):  
Hao Wu ◽  
Jeffrey Ting ◽  
Siqi Meng ◽  
Matthew Tirrell
Keyword(s):  
Small Angle ◽  
Self Assembly ◽  
Electrostatic Interactions ◽  
Polyelectrolyte Complex ◽  
Time Resolved ◽  
X Ray ◽  
X Ray Scattering ◽  
Kinetics Of ◽  
Ray Scattering

We have directly observed the <i>in situ</i> self-assembly kinetics of polyelectrolyte complex (PEC) micelles by synchrotron time-resolved small-angle X-ray scattering, equipped with a stopped-flow device that provides millisecond temporal resolution. This work has elucidated one general kinetic pathway for the process of PEC micelle formation, which provides useful physical insights for increasing our fundamental understanding of complexation and self-assembly dynamics driven by electrostatic interactions that occur on ultrafast timescales.

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