White Paper Series 1: In Situ X-ray Approaches in Battery Research

Systems for Research is proud to announce the release of a new white paper titled “In Situ X-ray Approaches in Battery Research” by its leading partner, Sigray. 

The paper effectively highlights the development of a suite of groundbreaking lab-based x-ray tools for energy research with performance capabilities approaching that of synchrotron-based approaches. 

When it comes to x-ray techniques for battery development, we often look at four commonly used techniques: 

• X-ray absorption spectroscopy (XAS) to provide electrochemical information such as chemical or valence states, bond length, coordination number 
• Micro X-Ray Fluorescence (microXRF) for elemental composition, migration, and contamination 
• X-ray Diffraction (XRD) to study the crystal structure and bond lengths of battery materials 
• X-ray Microscopy (XRM) for failure analysis and to study structural degradation and particle agglomeration in intact batteries and in operando pouch cells

This 1/4 part of this white paper series dives more into the use of X-ray absorption spectroscopy with Quantum Leap. 

A technique Overview 

X-ray Absorption Spectroscopy (XAS) is a powerful technique to understand the local electronic structure of atoms during an electrochemical process. Unlike X-ray diffraction (XRD), XAS is not limited to crystalline materials and is often used for studying transition metals of importance in battery research. X-ray Absorption Spectroscopy (XAS) is a powerful technique to understand the local electronic structure of atoms during an electrochemical process. Unlike X-ray diffraction (XRD), XAS is not limited to crystalline materials and is often used for studying transition metals of importance in battery research.

Systems Overview 

Sigray QuantumLeap XAS is the first laboratory system that provides synchrotron-like XAS capabilities with sub-eV resolution with acquisition times within minutes, and the only commercial XAS with access to both transmission-mode XAS (for concentrated samples) and fluorescence-mode XAS (low concentrations of 5% wt or lower).

QuantumLeap’s breakthrough design enables it to be the only laboratory system to enable high energy resolution acquisition at low Bragg angles.

Applications in Battery Research 

QuantumLeap products span the energy range of 2.1 to 25 keV, covering a vast majority of the elements of interest in battery research, including sulfur and all transition metals (nickel, manganese, cobalt, zinc). 

Li-Ion Batteries (LIBs):As the only system with fluorescence-mode XAS, QuantumLeap has become instrumental in the development of NMC-type Li-Ion battery materials, in which the goal is to minimize the weight percentage of Mn and Co to improve their cost.

Because it is the only system with fluorescence-mode XAS, QuantumLeap has become instrumental in the development of NMC-type Li-Ion battery materials, in which the goal is to minimize the weight percentage of Mn and Co to improve their cost. Such samples cannot be analyzed using conventional transmission-mode laboratory XAS because the high weight percentage of Ni and concentrations of Mn and Co do not provide adequate signal-to-noise (SNR).

Intact Pouch Cells: Keeping the electrode material within an intact pouch cell prevents environmental-induced chemistry changes and, importantly, enables in situ and repeated studies. However, intact pouch cells are highly absorbing to intact pouch cell batteries, even challenging ones with low x-ray transmission of <1% (Fig 5 shows ~0.2-0.3% transmission data).

 Systems for Research is diving into the potential of this suite of spectroscopy and laboratory tools in a four-part series. Stay tuned as we dive into the potential of each of these techniques.