In situ analyses for ion storage materials

Abstract

Development of high performance electrode materials for energy storage is one of the most important issues for our future society. However, a lack of clear analytical views limits critical understanding of electrode materials. This review covers useful analytical work using X-ray diffraction, X-ray absorption spectroscopy, microscopy and neutron diffraction for ion storage systems. The in situ observation facilitates comprehending real-time ion storage behaviour while the ion storage system is operating, which help us to understand detailed physical and chemical properties. We will discuss how the tools have been used to reveal detailed reaction mechanisms and underlying properties of electrode materials.

Advances in the Cathode Materials for Lithium Rechargeable Batteries

“…During charge and discharge,the Li ions go out and come in following the 8c-4a and 8c-12d pathway . [74,75] Both ordered and disordered spinel materials crystallize in acubic structure.During the de-intercalation process,the size of the crystal structure becomes smaller in proportion to the amount of de-intercalated Li ions.The overall behavior of the phase transition is similar in the ordered and disordered spinel material, but there are differences in the lattice parameter disparity among each phase.F igure 10 as hows in situ XRD patterns of both disordered and ordered spinel phases in the first cycle and the corresponding lattice parameter of each phase in the first two cycles.F or the ordered spinel, the phase transition shows appreciable distinction between cubic 1, cubic 2, and cubic 3p hases.I n contrast, disordered type spinel exhibits solid-solution-like phase transition between cubic 1and cubic 2phases. [38] In the case of the ordered LiNi 0.5 Mn 1.5 O 4 spinel, there is only one plateau around 4.7 Vwhich comes from the Ni 2+/3+ and Ni 3+/4+ redox.…”

Kathodenmaterialien für wiederaufladbare Lithiumbatterien

“…Beim Laden und Entladen wandern die Li‐Ionen über den 8c→4a‐ und 8c→12d‐Weg aus der Wirtstruktur heraus bzw. hinein . Sowohl geordnete als auch fehlgeordnete Spinellmaterialien kristallisieren in einer kubischen Struktur.…”

In situ/operando synchrotron-based X-ray techniques for lithium-ion battery research

“…The significant advantages of in situ/operando approaches over ex situ characterization are as follows: (1) In situ measurements instantly probe the reaction taking place at the specific interested location of a sample, providing better reliability and higher precision for the data analysis; (2) in operando measurements continuously monitor electrochemical, physical, or chemical processes on a single sample or a device under operating conditions, eliminating the preparation of multiple samples for ex situ measurements and providing closer to real-time operation information; (3) this method allows the investigation of the non-equilibrium or fast-transient process during electrochemical or chemical reactions. The nonequilibrium or short-lived intermediate states or species, which cannot be captured by ex situ characterizations, can be detected [2][3][4][5] . (4) In situ approaches remove the possibility for contamination, relaxation, or irreversible changes of highly reactive charged/discharged samples when preparing, handling, and transferring them for ex situ measurements (e.g., the reaction with organic solvent during sample washing, the reaction with moisture and oxygen during sample transfer, etc.)…”

“…The nonequilibrium or short-lived intermediate states or species, which cannot be captured by ex situ characterizations, can be detected [2][3][4][5] . (4) In situ approaches remove the possibility for contamination, relaxation, or irreversible changes of highly reactive charged/discharged samples when preparing, handling, and transferring them for ex situ measurements (e.g., the reaction with organic solvent during sample washing, the reaction with moisture and oxygen during sample transfer, etc.) 3 , and the true reaction products can be more reliably identified.…”