A Combined Experimental and Theoretical Study of Lithiation Mechanism in ZnFe2O4 Anode Materials

MRS Advances ◽  
2018 ◽  
Vol 3 (14) ◽  
pp. 773-778 ◽  
Author(s):  
Lei Wang ◽  
Alison McCarthy ◽  
Kenneth J. Takeuchi ◽  
Esther S. Takeuchi ◽  
Amy C. Marschilok
Keyword(s):  
Early Stage ◽  
Deep Understanding ◽  
Lithium Ion ◽  
Oxidation Products ◽  
Ex Situ ◽  
Theoretical Modelling ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Absorption

ABSTRACTZnFe2O4 (ZFO) represents a promising anode material for lithium ion batteries, but there is still a lack of deep understanding of the fundamental reduction mechanism associated with this material. In this paper, the complete visualization of reduction/oxidation products irrespective of their crystallinity was achieved experimentally through a compilation of in situ X-ray diffraction, synchrotron based powder diffraction, and ex-situ X-ray absorption fine structure data. Complementary theoretical modelling study further shed light upon the fundamental understanding of the lithiation mechanism, especially at the early stage from ZnFe2O4 up to LixZnFe2O4 (x = 2).

Size dependent behavior of Fe3O4crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Size Dependent ◽  
Transmission Electron ◽  
Dependent Behavior ◽  
X Ray Absorption

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.

scholarly journals Expanding the Mechanochemical Toolbox: Combining X-Ray Absorption Spectroscopy and Scattering for in Situ Time-Resolved Monitoring of Gold Nanoparticle Mechanosynthesis

2020 ◽  
Author(s):  
Paulo F M de Oliveira ◽  
Adam Michalchuk ◽  
Ana de Oliveira Guilherme Buzanich ◽  
Ralf Bienert ◽  
Roberto M. Torresi ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Electronic Materials ◽  
Early Stage ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
Subsequent Formation ◽  
X Ray ◽  
Detection Capabilities ◽  
X Ray Absorption

<div>The development of time-resolved in situ approaches for monitoring mechanochemical</div><div>transformations has revolutionized the field of mechanochemistry. Currently, the established in</div><div>situ approaches greatly limit the scope of investigations that are possible. Here we develop a new</div><div>approach to simultaneously follow the evolution of bulk atomic and electronic structure during a</div><div>mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based</div><div>X-ray methods: X-ray absorption spectroscopy and X-ray diffraction. We apply this method to</div><div>investigate the bottom-up mechanosynthesis of technologically important Au nanoparticles in the</div><div>presence of three different reducing agents. Moreover, we demonstrate how X-ray absorption</div><div>spectroscopy offers unprecedented insight into the early stage generation of growth species (e.g.</div><div>monomers and clusters), which lead to the subsequent formation of nanoparticles. These</div><div>processes are beyond the detection capabilities of diffraction methods. The approach is general,</div><div>and not limited to monitoring NP mechanosynthesis. This combined X-ray approach paves the</div><div>way to new directions in mechanochemical research of advanced electronic materials.</div>

scholarly journals Expanding the Mechanochemical Toolbox: Combining X-Ray Absorption Spectroscopy and Scattering for in Situ Time-Resolved Monitoring of Gold Nanoparticle Mechanosynthesis

2020 ◽  
Author(s):  
Paulo F M de Oliveira ◽  
Adam Michalchuk ◽  
Ana de Oliveira Guilherme Buzanich ◽  
Ralf Bienert ◽  
Roberto M. Torresi ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Electronic Materials ◽  
Early Stage ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
Subsequent Formation ◽  
X Ray ◽  
Detection Capabilities ◽  
X Ray Absorption

<div>The development of time-resolved in situ approaches for monitoring mechanochemical</div><div>transformations has revolutionized the field of mechanochemistry. Currently, the established in</div><div>situ approaches greatly limit the scope of investigations that are possible. Here we develop a new</div><div>approach to simultaneously follow the evolution of bulk atomic and electronic structure during a</div><div>mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based</div><div>X-ray methods: X-ray absorption spectroscopy and X-ray diffraction. We apply this method to</div><div>investigate the bottom-up mechanosynthesis of technologically important Au nanoparticles in the</div><div>presence of three different reducing agents. Moreover, we demonstrate how X-ray absorption</div><div>spectroscopy offers unprecedented insight into the early stage generation of growth species (e.g.</div><div>monomers and clusters), which lead to the subsequent formation of nanoparticles. These</div><div>processes are beyond the detection capabilities of diffraction methods. The approach is general,</div><div>and not limited to monitoring NP mechanosynthesis. This combined X-ray approach paves the</div><div>way to new directions in mechanochemical research of advanced electronic materials.</div>

scholarly journals Using In-Situ Laboratory and Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries Characterization: A Review on Recent Developments

2020 ◽  
Vol 5 (4) ◽  
pp. 75
Author(s):  
Alice V. Llewellyn ◽  
Alessia Matruglio ◽  
Dan J. L. Brett ◽  
Rhodri Jervis ◽  
Paul R. Shearing
Keyword(s):  
Structural Evolution ◽  
Deep Understanding ◽  
Lithium Ion ◽  
Market Demand ◽  
X Ray Diffraction ◽  
Battery Materials ◽  
X Ray ◽  
Challenges And Opportunities ◽  
Materials Research

Renewable technologies, and in particular the electric vehicle revolution, have generated tremendous pressure for the improvement of lithium ion battery performance. To meet the increasingly high market demand, challenges include improving the energy density, extending cycle life and enhancing safety. In order to address these issues, a deep understanding of both the physical and chemical changes of battery materials under working conditions is crucial for linking degradation processes to their origins in material properties and their electrochemical signatures. In situ and operando synchrotron-based X-ray techniques provide powerful tools for battery materials research, allowing a deep understanding of structural evolution, redox processes and transport properties during cycling. In this review, in situ synchrotron-based X-ray diffraction methods are discussed in detail with an emphasis on recent advancements in improving the spatial and temporal resolution. The experimental approaches reviewed here include cell designs and materials, as well as beamline experimental setup details. Finally, future challenges and opportunities for battery technologies are discussed.

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 X-Ray Diffraction Investigations during Diffusion Anneals of Ni-Cu Thin Film Diffusion Couples

2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer
Keyword(s):  
Thermal Stresses ◽  
Stress Generation ◽  
Ex Situ ◽  
Diffusion Annealing ◽  
X Ray Diffraction ◽  
Individual Layer ◽  
X Ray ◽  
Bilayer System ◽  
Stress Changes

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

scholarly journals In Situ Investigation of the Early-Stage Growth of Nanoporous Alumina

2018 ◽  
Vol 2018 ◽  
pp. 1-9
Author(s):  
Thérèse Gorisse ◽  
Ludovic Dupré ◽  
Marc Zelsmann ◽  
Alina Vlad ◽  
Alessandro Coati ◽  
...  
Keyword(s):  
Early Stage ◽  
Grazing Incidence ◽  
Alumina Layer ◽  
Nanoporous Alumina ◽  
X Ray ◽  
X Ray Scattering ◽  
In Situ Investigation ◽  
Low X ◽  
X Ray Absorption

We report the successful use of in situ grazing incidence small-angle X-ray scattering to follow the anodization of aluminum. A dedicated electrochemical cell was designed and developed for this purpose with low X-ray absorption, with the possibility to access all azimuthal angles (360°) and to remotely control the temperature of the electrolyte. Three well-known fabrication techniques of nanoporous alumina, i.e., single, double, and pretextured, were investigated. The differences in the evolution of the scattering images are described and explained. From these measurements, we could determine at which moment the pores start growing even for very short anodization times. Furthermore, we could follow the thickness of the alumina layer as a function of the anodization time by monitoring the period of the Kiessig fringes. This work is aimed at helping to understand the different steps taking place during the anodization of aluminum at the very early stages of nanoporous alumina formation.

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