scholarly journals Application of Operando X-ray Diffractometry in Various Aspects of the Investigations of Lithium/Sodium-Ion Batteries

Energies ◽  
2018 ◽  
Vol 11 (11) ◽  
pp. 2963 ◽  
Author(s):  
Wen Zhu ◽  
Yuesheng Wang ◽  
Dongqiang Liu ◽  
Vincent Gariépy ◽  
Catherine Gagnon ◽  
...  
Keyword(s):  
High Performance ◽  
Electrode Materials ◽  
Rechargeable Batteries ◽  
Operating Conditions ◽  
Cycle Life ◽  
Side Reactions ◽  
X Ray ◽  
The Impact ◽  
Working Mechanisms

The main challenges facing rechargeable batteries today are: (1) increasing the electrode capacity; (2) prolonging the cycle life; (3) enhancing the rate performance and (4) insuring their safety. Significant efforts have been devoted to improve the present electrode materials as well as to develop and design new high performance electrodes. All of the efforts are based on the understanding of the materials, their working mechanisms, the impact of the structure and reaction mechanism on electrochemical performance. Various operando/in-situ methods are applied in studying rechargeable batteries to gain a better understanding of the crystal structure of the electrode materials and their behaviors during charge-discharge under various conditions. In the present review, we focus on applying operando X-ray techniques to investigate electrode materials, including the working mechanisms of different structured materials, the effect of size, cycling rate and temperature on the reaction mechanisms, the thermal stability of the electrodes, the degradation mechanism and the optimization of material synthesis. We demonstrate the importance of using operando/in-situ XRD and its combination with other techniques in examining the microstructural changes of the electrodes under various operating conditions, in both macro and atomic-scales. These results reveal the working and the degradation mechanisms of the electrodes and the possible side reactions involved, which are essential for improving the present materials and developing new materials for high performance and long cycle life batteries.

Mechanistic Study of Electrode Materials for Rechargeable Batteries beyond Lithium Ion by In-situ Transmission Electron Microscopy

2021 ◽  
Author(s):  
Shaojun Guo ◽  
yousaf Muhammad ◽  
Ufra Naseer ◽  
Yiju Li ◽  
Zeeshan Ali ◽  
...  
Keyword(s):  
High Performance ◽  
Electrode Materials ◽  
Lithium Ion ◽  
Rechargeable Batteries ◽  
Electrochemical Process ◽  
Atomic Scale ◽  
Mechanistic Study ◽  
Electrochemical Reactions ◽  
Transmission Electron

Understanding the fundamental mechanisms of advanced electrode materials at the atomic scale during the electrochemical process is condemnatory to develop the high-performance rechargeable batteries. The complex electrochemical reactions involved inside...

scholarly journals Battery research using synchrotron powder X-ray diffraction

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.

scholarly journals Laboratory X-ray Microscopy Study of Microcrack Evolution in a Novel Sodium Iron Titanate-Based Cathode Material for Li-Ion Batteries

Crystals ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 3
Author(s):  
Viktor Shapovalov ◽  
Kristina Kutukova ◽  
Sebastian Maletti ◽  
Christian Heubner ◽  
Vera Butova ◽  
...  
Keyword(s):  
Cathode Material ◽  
Electrode Materials ◽  
Morphological Changes ◽  
Li Ion Batteries ◽  
X Ray ◽  
3D Morphology ◽  
Iron Titanate ◽  
Li Ion ◽  
The Impact

The long-term performance of batteries depends strongly on the 3D morphology of electrode materials. Morphological changes, i.e., particle fracture and surface deterioration, are among the most prominent sources of electrode degradation. A profound understanding of the fracture mechanics of electrode materials in micro- and nanoscale dimensions requires the use of advanced in situ and operando techniques. In this paper, we demonstrate the capabilities of laboratory X-ray microscopy and nano X-ray computed tomography (nano-XCT) for the non-destructive study of the electrode material’s 3D morphology and defects, such as microcracks, at sub-micron resolution. We investigate the morphology of Na0.9Fe0.45Ti1.55O4 sodium iron titanate (NFTO) cathode material in Li-ion batteries using laboratory-based in situ and operando X-ray microscopy. The impact of the morphology on the degradation of battery materials, particularly the size- and density-dependence of the fracture behavior of the particles, is revealed based on a semi-quantitative analysis of the formation and propagation of microcracks in particles. Finally, we discuss design concepts of the operando cells for the study of electrochemical processes.

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

2002 ◽  
Vol 47 (19) ◽  
pp. 3137-3149 ◽  
Author(s):  
M. Morcrette ◽  
Y. Chabre ◽  
G. Vaughan ◽  
G. Amatucci ◽  
J.-B. Leriche ◽  
...  
Keyword(s):  
Electrode Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Battery Electrode

Vacancies-engineered MoO3 and Na+-preinserted MnO2 in-situ grown N-doped graphene nanotubes as electrode materials for high-performance asymmetric supercapacitor

2021 ◽  
Author(s):  
Jian Zhao ◽  
He Cheng ◽  
Huanyu Li ◽  
Yan-Jie Wang ◽  
Qingyan Jiang ◽  
...  
Keyword(s):  
High Performance ◽  
Electrode Materials ◽  
High Energy ◽  
Cooperative Effect ◽  
Electrochemical Energy Storage ◽  
Asymmetric Supercapacitor ◽  
Asymmetric Supercapacitors ◽  
Doped Graphene ◽  
Power Densities

Developing advanced negative and positive electrode materials for asymmetric supercapacitors (ASCs) as the electrochemical energy storage can enable the device to reach high energy/power densities resulting from the cooperative effect...

scholarly journals Tracking Metamorphic Dehydration Reactions in Real Time with Transmission Small- and Wide-Angle Synchrotron X-ray Scattering: the Case of Gypsum Dehydration

2020 ◽  
Vol 61 (6) ◽  
Author(s):  
C E Schrank ◽  
K Gioseffi ◽  
T Blach ◽  
O Gaede ◽  
A Hawley ◽  
...  
Keyword(s):  
Real Time ◽  
Wide Angle ◽  
Length Scales ◽  
X Ray ◽  
Rock Samples ◽  
X Ray Scattering ◽  
Dehydration Reactions ◽  
The Impact ◽  
Ray Scattering

Abstract We present a review of a unique non-destructive method for the real-time monitoring of phase transformations and nano-pore evolution in dehydrating rocks: transmission small- and wide-angle synchrotron X-ray scattering (SAXS/WAXS). It is shown how SAXS/WAXS can be applied to investigating rock samples dehydrated in a purpose-built loading cell that allows the coeval application of high temperature, axial confinement, and fluid pressure or flow to the specimen. Because synchrotron sources deliver extremely bright monochromatic X-rays across a wide energy spectrum, they enable the in situ examination of confined rock samples with thicknesses of ≤ 1 mm at a time resolution of order seconds. Hence, fast kinetics with reaction completion times of about hundreds of seconds can be tracked. With beam sizes of order tens to hundreds of micrometres, it is possible to monitor multiple interrogation points in a sample with a lateral extent of a few centimetres, thus resolving potential lateral spatial effects during dehydration and enlarging sample statistics significantly. Therefore, the SAXS/WAXS method offers the opportunity to acquire data on a striking range of length scales: for rock samples with thicknesses of ≤ 10-3 m and widths of 10-2 m, a lateral interrogation-point spacing of ≥ 10-5 m can be achieved. Within each irradiated interrogation-point volume, information concerning pores with sizes between 10-9 and 10-7 m and the crystal lattice on the scale of 10-10 m is acquired in real time. This article presents a summary of the physical principles underpinning transmission X-ray scattering with the aim of providing a guide for the design and interpretation of time-resolved SAXS/WAXS experiments. It is elucidated (1) when and how SAXS data can be used to analyse total porosity, internal surface area, and pore-size distributions in rocks on length scales from ∼1 to 300 nm; (2) how WAXS can be employed to track lattice transformations in situ; and (3) which limitations and complicating factors should be considered during experimental design, data analysis, and interpretation. To illustrate the key capabilities of the SAXS/WAXS method, we present a series of dehydration experiments on a well-studied natural gypsum rock: Volterra alabaster. Our results demonstrate that SAXS/WAXS is excellently suited for the in situ tracking of dehydration kinetics and the associated evolution of nano-pores. The phase transformation from gypsum to bassanite is correlated directly with nano-void growth on length scales between 1 and 11 nm for the first time. A comparison of the SAXS/WAXS kinetic results with literature data emphasises the need for future dehydration experiments on rock specimens because of the impact of rock fabric and the generally heterogeneous and transient nature of dehydration reactions in nature. It is anticipated that the SAXS/WAXS method combined with in situ loading cells will constitute an invaluable tool in the ongoing quest for understanding dehydration and other mineral replacement reactions in rocks quantitatively.

scholarly journals Lanthanoid Complexes Supported by Retro-Claisen Condensation Products of β-Triketonates

2018 ◽  
Author(s):  
Laura Abad Galán ◽  
Alexandre N. Sobolev ◽  
Eli Zysman-Colman ◽  
Mark Ogden ◽  
Massimiliano Massi
Keyword(s):  
Chelating Ligands ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Claisen Condensation ◽  
X Ray ◽  
Condensation Products ◽  
Complexation Reactions ◽  
The Impact ◽  
Low Solubility

<i>β</i>-Triketonates have been recently used as chelating ligands for lanthanoid ions, presenting unique structures varying from polynuclear assemblies to polymers. In an effort to overcome low solubility of the complexes of tribenzoylmethane, four <i>β</i>-triketones with higher lipophilicity were synthesised. Complexation reactions were performed for each of these molecules using different alkaline bases in alcoholic media. X-ray diffraction studies suggested that the ligands were undergoing decomposition under the reaction conditions. This is proposed to be caused by <i>in situ</i>retro-Claisen condensation reactions, consistent with two examples that have been reported previously. The lability of the lanthanoid cations in the presence of a varying set of potential ligands gave rise to structures where one, two, or three of the molecules involved in the retro-Claisen condensationreaction were linked to the lanthanoid centres. These results, along with measurements of ligand decomposition in the presence of base alone, suggest that using solvents of lower polarity will mimimise the impact of the retro-Claisen condensation in these complexes. <br>

scholarly journals Fabrication of Strontium Bismuth Oxides as Novel Battery-Type Electrode Materials for High-Performance Supercapacitors

2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Yinghui Han ◽  
Le Li ◽  
Yunpeng Liu ◽  
Xue Li ◽  
Xiaohan Qi ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
High Performance ◽  
Electrode Materials ◽  
Specific Capacity ◽  
Structural Features ◽  
High Electron ◽  
Strontium Content ◽  
X Ray ◽  
Bismuth Oxides ◽  
Improved Performance

A simple and efficient process method for the preparation of strontium bismuth oxides (SBOs) via an impregnation-calcination method is presented. The synthesized active materials are characterized using X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy. The electrochemical performance of the as-synthesized SBO samples is observed to decrease gradually as the strontium content is increased from 25% to 50%. The SBO sample with a Sr/Bi ratio of 1 : 3 shows the highest specific capacitance of 1228.7 F g−1 (specific capacity of 204.8 mAh g−1) at a current density of 1 A g−1 and a good cycling stability (75.1%) over 3000 charge-discharge cycles. The improved performance of the supercapacitors can be attributed to the unique structural features resulting from the addition of appropriate portions of Sr, which supports high electron conductivity and rapid ion/electron transport within the electrode and at the electrode/electrolyte interface. All the results show that the SBOs have considerable potential for use as high-performance battery-type electrodes in supercapacitors.

Testing of solid oxide cells at high current densities

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
André Weber
Keyword(s):  
Single Cell ◽  
High Performance ◽  
High Efficiency ◽  
Electrochemical Impedance ◽  
Single Cells ◽  
Operating Conditions ◽  
Solid Oxide ◽  
Current Densities ◽  
Cell Testing ◽  
The Impact

Abstract Solid Oxide Cells (SOCs) have gained an increasing interest as electrochemical energy converters due to their high efficiency, fuel flexibility and ability of reversible fuel cell/electrolysis operation. During the development process as well as in quality assurance tests, the performance of single cells and cell stacks is commonly evaluated by means of current/voltage- (CV-) characteristics. Despite of the fact that the measurement of a CV-characteristic seems to be simple compared to more complex, dynamic methods as electrochemical impedance spectroscopy or current interrupt techniques, the resulting performance strongly depends on the test setup and the chosen operating conditions. In this paper, the impact of different single cell testing environments and operating conditions on the CV-characteristic of high performance cells is discussed. The influence of cell size, contacting and current collection, contact pressure, fuel flow rate and composition on the achievable cell performance is presented and limitations arising from the test bed and testing conditions will be pointed out. As today’s high performance cells are capable of delivering current densities of several ampere per cm2 a special emphasis will be laid on single cell testing in this current range.

scholarly journals A Novel Low-Temperature Non-Corrosive Sulfate/Sulfide Scale Dissolver

2020 ◽  
Vol 12 (6) ◽  
pp. 2455
Author(s):  
Hany Gamal ◽  
Salaheldin Elkatatny ◽  
Dhafer Al Shehri ◽  
Mohamed Bahgat
Keyword(s):  
Low Temperature ◽  
Corrosion Rate ◽  
High Performance ◽  
Oil And Gas ◽  
Ethylenediaminetetraacetic Acid ◽  
Gas Production ◽  
Operating Conditions ◽  
Superior Performance ◽  
X Ray ◽  
Dissolution Efficiency

The oil and gas production operations suffer from scale depositions. The scale precipitations have a damaging impact on the reservoir pores, perforations, downhole and completion equipment, pipeline network, wellhead chokes, and surface facilities. Hydrocarbon production possibly decreased because of the scale accumulation in the well tubular, leading to a well plugging, this requires wells to be shut-in in severe cases to perform a clean-out job. Therefore, scale deposition is badly affecting petroleum economics. This research aims to design a scale dissolver with low cost, non-damaging for the well equipment and has a high performance at the field operating conditions. This paper presents a novel non-corrosive dissolver for sulfate and sulfide composite scale in alkaline pH and works at low-temperature conditions. The scale samples were collected from a production platform from different locations. A complete description of the scale samples was performed as X-ray diffraction (XRD) and X-ray fluorescence (XRF). The new scale dissolver was prepared in different concentrations to examine its dissolution efficiency for the scale with time at low temperatures. The experimental design studied the solid to fluid ratio, temperature, solubility time, and dissolution efficiency in order to achieve the optimum and most economic performance of solubility in terms of high dissolution efficiency with the smallest possible amount of scale dissolver. A solubility comparison was performed with other commercial-scale-dissolvers and the corrosion rate was tested. The experimental work results demonstrated the superior performance of the new scale dissolver. The new scale dissolver showed a solubility efficiency of 91.8% at a low temperature of 45 °C and 79% at 35 °C. The new scale dissolver showed a higher solubility ratio for the scale sample than the ethylenediaminetetraacetic acid (EDTA) (20 wt. %), diethylenetriamine pentaacetic acid (DTPA) (20 wt. %), and HCl (10 wt. %). The corrosion rate for the new non-corrosive dissolver was 0.01357 kg/m2 (0.00278 lb./ft²) which was considered a very low rate and non-damaging for the equipment. The low corrosive effect of the new dissolver will save the extra cost of adding the corrosion inhibitors and save the equipment from the damaging effect of the corrosive acids.

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