Structure solution and refinement of metal-ion battery cathode materials using electron diffraction tomography

2019 ◽  
Vol 75 (4) ◽  
pp. 485-494 ◽  
Author(s):  
Joke Hadermann ◽  
Artem M. Abakumov
Keyword(s):  
Electron Diffraction ◽  
Cathode Materials ◽  
Metal Ion ◽  
Structural Changes ◽  
Liquid Electrolyte ◽  
Ex Situ ◽  
Diffraction Tomography ◽  
Transmission Electron ◽  
Structure Solution ◽  
Electrochemical Cycling

The applicability of electron diffraction tomography to the structure solution and refinement of charged, discharged or cycled metal-ion battery positive electrode (cathode) materials is discussed in detail. As these materials are often only available in very small amounts as powders, the possibility of obtaining single-crystal data using electron diffraction tomography (EDT) provides unique access to crucial information complementary to X-ray diffraction, neutron diffraction and high-resolution transmission electron microscopy techniques. Using several examples, the ability of EDT to be used to detect lithium and refine its atomic position and occupancy, to solve the structure of materials ex situ at different states of charge and to obtain in situ data on structural changes occurring upon electrochemical cycling in liquid electrolyte is discussed.

scholarly journals Quantitative electron diffraction tomography for the structure solution of cathode materials for Li-ion batteries

2016 ◽  
pp. 790-791
Author(s):  
Olesia Karakulina ◽  
Stanislav Fedotov ◽  
Vasiliy Sumanov ◽  
Oleg Drozhzhin ◽  
Nellie Khasanova ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Cathode Materials ◽  
Diffraction Tomography ◽  
Li Ion Batteries ◽  
Structure Solution ◽  
Li Ion

Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

1989 ◽  
Vol 47 ◽  
pp. 462-463
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Transmission Electron

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.

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 Probing planar defects in nanoparticle superlattices by 3D small-angle electron diffraction tomography and real space imaging

Nanoscale ◽  
2014 ◽  
Vol 6 (22) ◽  
pp. 13803-13808 ◽  
Author(s):  
Arnaud Mayence ◽  
Dong Wang ◽  
German Salazar-Alvarez ◽  
Peter Oleynikov ◽  
Lennart Bergström
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
Real Space ◽  
Diffraction Tomography ◽  
Planar Defects ◽  
Pd Nanoparticle ◽  
Transmission Electron ◽  
Nanoparticle Superlattices ◽  
Microscopy Techniques

Planar defects in Pd nanoparticle superlattices were revealed by a combination of real and reciprocal space transmission electron microscopy techniques. 3D electron diffraction tomography was extended to characterize mesoscale imperfections.

scholarly journals Self-Substitution and the Temperature Effects on the Electrochemical Performance in the High Voltage Cathode System LiMn1.5+xNi0.5−xO4 (x = 0.1)

2017 ◽  
Vol 14 (2) ◽  
Author(s):  
Yun Xu ◽  
Mingyang Zhao ◽  
Syed Khalid ◽  
Hongmei Luo ◽  
Kyle S. Brinkman
Keyword(s):  
Electrochemical Performance ◽  
High Voltage ◽  
Cathode Materials ◽  
Metal Ion ◽  
Structural Changes ◽  
Rate Capability ◽  
Performance Testing ◽  
Capacity Loss ◽  
Stable Performance ◽  
Li Ion

The high voltage cathode material, LiMn1.6Ni0.4O4, was prepared by a polymer-assisted method. The novelty of this work is the substitution of Ni with Mn, which already exists in the crystal structure instead of other isovalent metal ion dopants which would result in capacity loss. The electrochemical performance testing including stability and rate capability was evaluated. The temperature was found to impose a change on the valence and structure of the cathode materials. Specifically, manganese tends to be reduced at a high temperature of 800 °C and leads to structural changes. The manganese substituted LiMn1.5Ni0.5O4 (LMN) has proved to be a good candidate material for Li-ion battery cathodes displaying good rate capability and capacity retention. The cathode materials processed at 550 °C showed a stable performance with negligible capacity loss for 400 cycles.

3D electron diffraction techniques

2019 ◽  
Vol 75 (4) ◽  
pp. 495-504 ◽  
Author(s):  
Mauro Gemmi ◽  
Arianna E. Lanza
Keyword(s):  
Structural Analysis ◽  
Electron Diffraction ◽  
High Sensitivity ◽  
Reliable Data ◽  
Zone Axis ◽  
Diffraction Tomography ◽  
Proof Of Concept ◽  
Structure Solution ◽  
Continuous Rotation ◽  
3D Electron

3D electron diffraction is an emerging technique for the structural analysis of nanocrystals. The challenges that 3D electron diffraction has to face for providing reliable data for structure solution and the different ways of overcoming these challenges are described. The route from zone axis patterns towards 3D electron diffraction techniques such as precession-assisted electron diffraction tomography, rotation electron diffraction and continuous rotation is also discussed. Finally, the advantages of the new hybrid detectors with high sensitivity and fast readout are demonstrated with a proof of concept experiment of continuous rotation electron diffraction on a natrolite nanocrystal.

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