scholarly journals An electrochemical cell with sapphire windows foroperandosynchrotron X-ray powder diffraction and spectroscopy studies of high-power and high-voltage electrodes for metal-ion batteries

2018 ◽  
Vol 25 (2) ◽  
pp. 468-472 ◽  
Author(s):  
Oleg A. Drozhzhin ◽  
Ivan V. Tereshchenko ◽  
Hermann Emerich ◽  
Evgeny V. Antipov ◽  
Artem M. Abakumov ◽  
...  
Keyword(s):  
Cathode Material ◽  
High Voltage ◽  
High Power ◽  
Metal Ion ◽  
Electrochemical Cell ◽  
Signal To Noise Ratio ◽  
European Synchrotron Radiation Facility ◽  
X Ray ◽  
Discharge Rates ◽  
Good Signal

A new multi-purposeoperandoelectrochemical cell was designed, constructed and tested on the Swiss–Norwegian Beamlines BM01 and BM31 at the European Synchrotron Radiation Facility. Single-crystal sapphire X-ray windows provide a good signal-to-noise ratio, excellent electrochemical contact because of the constant pressure between the electrodes, and perfect electrochemical stability at high potentials due to the inert and non-conductive nature of sapphire. Examination of the phase transformations in the Li1–xFe0.5Mn0.5PO4positive electrode (cathode) material at C/2 and 10C charge and discharge rates, and a study of the valence state of the Ni cations in the Li1–xNi0.5Mn1.5O4cathode material for Li-ion batteries, revealed the applicability of this novel cell design to diffraction and spectroscopic investigations of high-power/high-voltage electrodes for metal-ion batteries.

scholarly journals Development and Investigation of a NASICON‐Type High‐Voltage Cathode Material for High‐Power Sodium‐Ion Batteries

2020 ◽  
Vol 132 (6) ◽  
pp. 2470-2477 ◽  
Author(s):  
Mingzhe Chen ◽  
Weibo Hua ◽  
Jin Xiao ◽  
David Cortie ◽  
Xiaodong Guo ◽  
...  
Keyword(s):  
Cathode Material ◽  
High Voltage ◽  
High Power ◽  
Sodium Ion ◽  
Sodium Ion Batteries ◽  
Nasicon Type

scholarly journals Development and Investigation of a NASICON‐Type High‐Voltage Cathode Material for High‐Power Sodium‐Ion Batteries

2020 ◽  
Vol 59 (6) ◽  
pp. 2449-2456 ◽  
Author(s):  
Mingzhe Chen ◽  
Weibo Hua ◽  
Jin Xiao ◽  
David Cortie ◽  
Xiaodong Guo ◽  
...  
Keyword(s):  
Cathode Material ◽  
High Voltage ◽  
High Power ◽  
Sodium Ion ◽  
Sodium Ion Batteries ◽  
Nasicon Type

Time-resolved XAFS measurement using quick-scanning techniques at BSRF

2017 ◽  
Vol 24 (3) ◽  
pp. 674-678 ◽  
Author(s):  
Shengqi Chu ◽  
Lirong Zheng ◽  
Pengfei An ◽  
Hui Gong ◽  
Tiandou Hu ◽  
...  
Keyword(s):  
Signal To Noise Ratio ◽  
High Energy ◽  
High Energy Resolution ◽  
Double Crystal ◽  
Time Resolved ◽  
Edge Structure ◽  
X Ray ◽  
Double Crystal Monochromator ◽  
Good Signal ◽  
X Ray Absorption

A new quick-scanning X-ray absorption fine-structure (QXAFS) system has been established on beamline 1W1B at the Beijing Synchrotron Radiation Facility. As an independent device, the QXAFS system can be employed by other beamlines equipped with a double-crystal monochromator to carry out quick energy scans and data acquisition. Both continuous-scan and trapezoidal-scan modes are available in this system to satisfy the time scale from subsecond (in the X-ray absorption near-edge structure region) to 1 min. Here, the trapezoidal-scan method is presented as being complementary to the continuous-scan method, in order to maintain high energy resolution and good signal-to-noise ratio. The system is demonstrated to be very reliable and has been combined with in situ cells to carry out time-resolved XAFS studies.

scholarly journals Next generation X-ray detectors for in-house XRD

2008 ◽  
Vol 23 (2) ◽  
pp. 101-105 ◽  
Author(s):  
Takeyoshi Taguchi ◽  
Christian Brönnimann ◽  
Eric F. Eikenberry
Keyword(s):  
Generation X ◽  
Dynamic Range ◽  
Single Photon ◽  
Signal To Noise Ratio ◽  
Photon Counting ◽  
Next Generation ◽  
Large Area ◽  
X Ray ◽  
Array Detectors ◽  
Good Signal

A novel type X-ray detector, called PILATUS, has been developed at the Paul Scherrer Institut in Switzerland during the last decade. PILATUS detectors are two-dimensional hybrid pixel array detectors, which operate in single-photon counting mode. PILATUS detectors feature a very wide dynamic range (1:1 000 000), very short readout time (<3.0 ms), no readout noise, and very high counting rate (>2×106counts/s/pixel). In addition, a lower energy threshold can be set in order to suppress fluorescence background from the sample, thus a very good signal-to-noise ratio is achieved. The combination of these features for area detectors is unique and thus the PILATUS detectors are considered to be the next generation X-ray detectors. The basic building block of all the detectors is the PILATUS module having an active area of 83.8×33.5 mm2. The PILATUS 100K is a complete detector system with one module. PILATUS detector systems can have other configurations, including large area systems consisting of 20 to 60 modules that can cover up to an area of 431×448 mm2. Such large systems are mainly used for macromolecular structure determination, such as protein crystallography and small angle X-ray scattering. The PILATUS 100K detector can be easily adapted to many systems; the single-module detector is integrated to an in-house X-ray diffraction (XRD) system. Examples of XRD measurements with the PILATUS 100K detector are given.

scholarly journals Extended Interfacial Stability Through Simple Acid Rinsing in a Li-Rich Oxide Cathode Material

2019 ◽  
Author(s):  
Srinivasan Ramakrishnan ◽  
Byungchun Park ◽  
Jue Wu ◽  
Wanli Yang ◽  
Bryan D. McCloskey
Keyword(s):  
Cathode Material ◽  
Surface Treatment ◽  
High Voltage ◽  
Surface Passivation ◽  
Photoelectron Spectra ◽  
Ex Situ ◽  
Rate Performance ◽  
Interfacial Instabilities ◽  
X Ray ◽  
Oxide Cathode

<p>Layered Li-rich Ni, Mn, Co (NMC) oxide cathodes in Li-ion batteries provide high specific capacities (>250 mAh/g) via O-redox at high voltages. However, associated high-voltage interfacial degradation processes require strategies for effective electrode surface passivation. Here, we show that an acidic surface treatment of a Li-rich NMC layered oxide cathode material leads to a substantial suppression of CO<sub>2</sub> and O<sub>2</sub> evolution, ~90% and ~100% respectively, during the first charge up to 4.8 V vs. Li<sup>+/0</sup>. CO<sub>2</sub> suppression is related to Li<sub>2</sub>CO<sub>3</sub> removal as well as effective surface passivation against electrolyte degradation. This treatment does not result in any loss of discharge capacity and provides superior long-term cycling and rate performance compared to as-received, untreated materials. We also quantify the extent of lattice oxygen participation in charge compensation (“O-redox”) during Li<sup>+</sup> removal by a novel ex-situ acid titration. Our results indicate that the peroxo-like species resulting from O-redox originate on the surface at least 300 mV earlier than the activation plateau region around 4.5 V. X-ray photoelectron spectra and Mn<i>-L</i> X-ray absorption spectra of the cathode powders reveal a Li<sup>+</sup> deficiency and a partial reduction of Mn ions on the surface of the acid-treated material. More interestingly, although the irreversible oxygen evolution is greatly suppressed through the surface treatment, our O K-edge resonant inelastic X-ray scattering shows the lattice O-redox behavior largely sustained. The acidic treatment, therefore, only optimizes the surface of the Li-rich material and almost eliminates the irreversible gas evolution, leading to improved cycling and rate performance. This work therefore presents a simple yet effective approach to passivate cathode surfaces against interfacial instabilities during high-voltage battery operation.</p>

Na7V3(P2O7)4 as a high voltage electrode material for Na-ion batteries: crystal structure and mechanism of Na+ extraction/insertion by operando X-ray diffraction

2020 ◽  
Vol 8 (40) ◽  
pp. 21110-21121
Author(s):  
Vadim M. Kovrugin ◽  
Jean-Noël Chotard ◽  
François Fauth ◽  
Christian Masquelier
Keyword(s):  
Crystal Structure ◽  
Cathode Material ◽  
Electrochemical Properties ◽  
Crystal Chemistry ◽  
High Voltage ◽  
Electrode Material ◽  
High Voltage Electrode ◽  
X Ray Diffraction ◽  
X Ray

The crystal chemistry and the electrochemical properties of Na7V3(P2O7)4 as a high voltage cathode material upon Na+ extraction/insertion were investigated by operando X-ray diffraction.

scholarly journals Size and structure of hexanuclear plutonium oxo-hydroxo clusters in aqueous solution from synchrotron analysis

2022 ◽  
Vol 29 (1) ◽  
Author(s):  
Thomas Dumas ◽  
Matthieu Virot ◽  
Denis Menut ◽  
Christelle Tamain ◽  
Cyril Micheau ◽  
...  
Keyword(s):  
Signal To Noise Ratio ◽  
Water Soluble ◽  
Saxs Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Good Signal ◽  
Constrained Conditions ◽  
Future Work ◽  
X Ray Absorption ◽  
Sample Dispersion

The size and shape of a water-soluble hexanuclear plutonium cluster were probed by combining synchrotron small-angle X-ray scattering (SAXS) and extended X-ray absorption fine structure (EXAFS). A specific setup coupling both techniques and dedicated to radioactive samples on the MARS beamline endstation at Synchrotron SOLEIL is described. The plutonium hexanuclear cores are well stabilized by the 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid ligands and this allows a good evaluation of the setup to probe the very small plutonium core. The results show that, in spite of the constrained conditions required to avoid any risk of sample dispersion, the flux and the sample environment are optimized to obtain a very good signal-to-noise ratio, allowing the detection of small plutonium aggregates in an aqueous phase. The structure of the well defined hexanuclear cluster has been confirmed by EXAFS measurements in solution and correlated with SAXS data processing and modelling. An iterative comparison of classical fit models (Guinier or sphere form factor) with the experimental results allowed a better interpretation of the SAXS signal that will be relevant for future work under environmentally relevant conditions.

In Situ Observation of Polytype Switches during SiC PVT Bulk Growth by High Energy X-Ray Diffraction

2009 ◽  
Vol 615-617 ◽  
pp. 23-26 ◽  
Author(s):  
Peter J. Wellmann ◽  
Katja Konias ◽  
Philip Hens ◽  
Rainer Hock ◽  
Andreas Magerl
Keyword(s):  
Signal To Noise Ratio ◽  
High Energy ◽  
In Situ Observation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bulk Growth ◽  
Diffraction Patterns ◽  
Set Up ◽  
Good Signal

This work reports on the in-situ observation of a polytype switch during physical vapor transport (PVT) growth of bulk SiC crystals by x-ray diffraction. A standard PVT reactor for 2” and 3” bulk growth was set up in a high-energy x-ray diffraction lab. Due to the high penetration depth of the high-energy x-ray beam no modification of the PVT reactor was necessary in order to measure Laue diffraction patterns of the growing crystal with good signal to noise ratio. We report for the first time upon the in-situ observation of polytype switching during SiC bulk PVT growth.

scholarly journals Extended Interfacial Stability Through Simple Acid Rinsing in a Li-Rich Oxide Cathode Material

2019 ◽  
Author(s):  
Srinivasan Ramakrishnan ◽  
Byungchun Park ◽  
Jue Wu ◽  
Wanli Yang ◽  
Bryan D. McCloskey
Keyword(s):  
Cathode Material ◽  
Surface Treatment ◽  
High Voltage ◽  
Surface Passivation ◽  
Photoelectron Spectra ◽  
Ex Situ ◽  
Rate Performance ◽  
Interfacial Instabilities ◽  
X Ray ◽  
Oxide Cathode

<p>Layered Li-rich Ni, Mn, Co (NMC) oxide cathodes in Li-ion batteries provide high specific capacities (>250 mAh/g) via O-redox at high voltages. However, associated high-voltage interfacial degradation processes require strategies for effective electrode surface passivation. Here, we show that an acidic surface treatment of a Li-rich NMC layered oxide cathode material leads to a substantial suppression of CO<sub>2</sub> and O<sub>2</sub> evolution, ~90% and ~100% respectively, during the first charge up to 4.8 V vs. Li<sup>+/0</sup>. CO<sub>2</sub> suppression is related to Li<sub>2</sub>CO<sub>3</sub> removal as well as effective surface passivation against electrolyte degradation. This treatment does not result in any loss of discharge capacity and provides superior long-term cycling and rate performance compared to as-received, untreated materials. We also quantify the extent of lattice oxygen participation in charge compensation (“O-redox”) during Li<sup>+</sup> removal by a novel ex-situ acid titration. Our results indicate that the peroxo-like species resulting from O-redox originate on the surface at least 300 mV earlier than the activation plateau region around 4.5 V. X-ray photoelectron spectra and Mn<i>-L</i> X-ray absorption spectra of the cathode powders reveal a Li<sup>+</sup> deficiency and a partial reduction of Mn ions on the surface of the acid-treated material. More interestingly, although the irreversible oxygen evolution is greatly suppressed through the surface treatment, our O K-edge resonant inelastic X-ray scattering shows the lattice O-redox behavior largely sustained. The acidic treatment, therefore, only optimizes the surface of the Li-rich material and almost eliminates the irreversible gas evolution, leading to improved cycling and rate performance. This work therefore presents a simple yet effective approach to passivate cathode surfaces against interfacial instabilities during high-voltage battery operation.</p>

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