Enhancing Lithium-Ion Battery Recycling: The Role of XRF and ICP-OES in Black Mass Analysis

Enhancing Lithium-Ion Battery Recycling: The Role of XRF and ICP-OES in Black Mass Analysis

Introduction

The growing popularity of electric vehicles and the widespread use of lithium-ion batteries have increased the demand for effective recycling methods. Efficient recycling of these batteries is crucial for sustainability and minimizing environmental impact. This newsletter explores how advanced spectroscopic techniques, such as X-Ray Fluorescence (XRF) and Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), enable the efficient analysis and process control for the recycling of lithium-ion battery black mass.


Understanding Black Mass

Lithium-Ion Battery Black Mass

Black mass is the residual material left after the initial mechanical and thermal treatment of spent lithium-ion batteries. It contains valuable metals like lithium, cobalt, nickel, and manganese, as well as other elements such as copper, aluminum, fluorine, phosphorus and graphite. Accurate analysis of black mass is essential for determining the content of recoverable metals and optimizing the recycling process.


The Importance of Recycling

Recycling lithium-ion batteries efficiently is crucial for sustainability. It not only helps recover valuable metals but also reduces environmental pollution and decreases dependency on raw material extraction. Accurate analysis ensures that the recycling process is optimized to extract the maximum amount of valuable materials, supporting a circular economy.

In the EU, this is regulated by the regulation (EU) 2023/1542 of the European Parliament and of the council of 12 July 2023 concerning batteries and waste batteries. Annex XII of this regulation outlines targets for the recovery of materials by the end of 2027 and the end of 2031.

Targets for Recovery of Materials (EU Regulation 2023/1542)



XRF in Black Mass Analysis

XRF Technology

X-Ray Fluorescence (XRF) is a powerful analytical technique used for the qualitative and quantitative determination of elemental composition in materials. Its non-destructive nature, speed, and ability to handle a wide range of concentrations make it ideal for analyzing the complex matrices found in lithium-ion battery black mass.


The XRF Principle


The XRF analysis process involves:

1. Sample Preparation: Grinding the black mass sample into a fine powder and pressing it into a stable pellet.

2. Instrument Calibration: Using standardless analysis methods, which are optimized using certified reference materials.

3. Sample Analysis: Using the SPECTRO XEPOS, the sample is irradiated with high-energy X-rays, and the emitted fluorescence X-rays are measured to quantify elemental concentrations.


Results and Benefits of XRF

The SPECTRO XEPOS demonstrated excellent precision and accuracy in determining the content of elements such as nickel, manganese, cobalt, fluorine, copper, phosphorus, and aluminum in black mass. XRF offers several key benefits:

  • Non-Destructive Testing: Allows repeated analyses without altering the sample.
  • Speed and Efficiency: Fast and easy sample preparation, quick analysis times enable rapid processing of samples.
  • Wide Range of Detection: Capable of detecting and quantifying a broad spectrum of elements.



SPECTRO XEPOS results show good agreement with the mean of the ILS results for the elements F, Co, Mn.


SPECTRO XEPOS result shows good agreement with the mean of the ILS results for the element Ni.



ICP-OES in Black Mass Analysis


ICP-OES Technology

Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) is another highly effective technique for analyzing lithium-ion battery black mass. It excels in handling complex compositions and accurately determining the concentration of multiple elements simultaneously.

The ICP-OES analysis process involves:

1. Sample Preparation: Homogenizing and digesting/extracting the black mass sample using acids.

2. Sample Introduction: Introducing the sample as an aerosol into the plasma via a nebulizer and a spray chamber.

3. Plasma Generation and Optical Emission Detection: Evaporation and dissociation of the sample into atoms; partial ionization and excitation to the emission of radiation characteristic for the specific elements contained in the sample. Transfer of the emitted light into an optical, diffraction of the light and detection of the light intensities of the specific wavelengths.

4. Calibration and Quantification: Comparing the emitted light intensity to the intensities obtained for calibration standards to determine elemental concentrations.


Results and Advantages of ICP-OES

The SPECTRO ARCOS MultiView system demonstrated high sensitivity and precision in detecting elements such as lithium, manganese, cobalt, and nickel, as well as trace elements in black mass. ICP-OES offers several advantages:

  • High Sensitivity: Capable of detecting trace elements.
  • High Accuracy: Capable of detecting the main components with high precision and accuracy
  • Simultaneous Multi-Element Analysis: Efficiently analyzes multiple elements, - major, minor and traces in a single run.
  • Versatility: Suitable for a wide range of sample types and matrices.



A Comparison Between ICP-OES and XRF Technology

Conclusion

Advanced spectroscopic techniques such as XRF and ICP-OES are crucial for the efficient recycling of lithium-ion batteries. These methods offer high sensitivity, precision, and the ability to handle complex materials, making them indispensable for ensuring the sustainable management of valuable resources. By adopting these technologies, industries can significantly contribute to environmental conservation and resource sustainability.


The Lithium-Ion Batteries Recycling Circle


Live Webinar on August 22, 2024

Join the live webinar "Lithium-Ion Battery Recycling: Elemental Analysis of Black Mass Using ED-XRF and ICP-OES" and discover innovative technologies and methods for analyzing black mass, crucial for a sustainable circular economy. Learn from experts and get your questions answered live. Register now: https://go.spectro.com/webinar-black-mass-august-2024

Learn More

Interested in learning more about how advanced spectroscopy can enhance your recycling operations? We have two detailed application reports available:

Contact us today to discover how our innovative solutions can support your sustainability goals and drive efficiency in resource management.

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