X-ray Diffraction (XRD) to study the crystal structure and bond lengths of battery materials.

January 31, 2024 3 min read

X-ray Diffraction (XRD) to study the crystal structure and bond lengths of battery materials.

Systems for Research is proud to announce the release of a new white paper title “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

The 3/3 part of this white paper series dives more into the use of X-ray Diffraction (XRD) with EclipseXRM and Apex XCT to study the crystal structure and bond lengths of battery materials.

 

A Technique Overview

X-ray microscopy (XRM) is a powerful tool for the analysis of the structure of materials at various length scales, ranging from microns to nanometers. The approach measures the absorption of x-rays to form images of the internal structures of intact samples after or during charging cycles.

 

Systems Overview

Sigray offers the two leading XRM models: EclipseXRM and Apex XCT. EclipseXRM is a breakthrough nanoCT system that scans a range of intact and cut battery samples at worldleading 300 nm spatial resolution. In contrast to the EclipseXRM, Sigray’s Apex XCT is specifically designed for planar samples (including pouch cell batteries) and can image such samples at 0.5 µm resolution within minutes.

 

 X-ray Microscopy and Battery Research

Lithium ion batteries (LIBs) are complex electrochemical systems with hierarchical multiscale structures and repeated imaging of a battery between charging cycles or in operando is essential for a quantitative understanding of structural changes.

EclipseXRM: X-ray microscopy is unique as it has the power to carry out hierarchical 3D imaging at multiple length scales. EclipseXRM enables imaging of intact batteries at zoomed-out overviews (coarser resolution) and zoomed-in (0.3 nm) detailed views of defects and microstructures.

 

Examples of the range of battery defects that can be imaged using the EclipseXRM are shown in the figure below. 

 

Apex XCT: Pouch cell batteries have high aspect ratios and often are difficult to image using conventional x-ray imaging approaches at high resolutions beyond 10s of microns. The Apex XCT’s patented scanning geometry is ideal for planar samples, enabling submicron resolution on intact pouch cell batteries and at high throughputs of down to single digit minutes.

 

Conclusion

Advances in battery research depend on a multi-technique approach to develop comprehensive understanding of chemical and structural battery degradation mechanisms. Synchrotron x-ray techniques have been critical in significant discoveries, but the lack of accessibility slows the pace of research. Sigray has developed a suite of spectroscopy and imaging laboratory tools for 24 hours a day, 7 days a week access to synchrotron-like capabilities to accelerate battery research.

 

Systems for Research and Sigray: A Meaningful Partnership 

Systems for Research (SFR) is a proud partner of Sigray, the leading name in X-Ray Microscopy and we are diving into the potential of this suite of spectroscopy and laboratory tools in a four-part series. Stay tuned as we dive into part ¾ of this series as we discover more about X-ray Microscopy with EclipseXRM and Apex XCT.