Commercialization is a bottleneck for many academic and R&D laboratories. Moving research from small-scale to large-scale often has unforeseen challenges. Finding superior materials while working at the lab bench does not necessarily translate to marketplace success. In fact, some industry professionals refer to the journey between discovery and commercialization as the “valley of death.”
In today’s battery research laboratories, “the valley of death” is alive and well. Battery R&D focuses on many different aspects—the supply chain, next-generation technologies, modification of materials, design optimization at the cell and pack level, and efficient recycling pathways. With such a complex workflow, success is occasionally lost somewhere between basic research, technology development, technology demonstrations, and commercialization.
Traditional analysis
The longevity of batteries is determined by the quality of the components used. Increasingly, more sensitive quality controls are required to comply with new and ever-evolving regulations. Both QC and R&D require detailed characterization of individual components and their interactions.
There are four main parts of the lithium-ion battery value chain:
- Mining and raw mineral processing: finding and extracting high-quality raw material from rock ores
- Component manufacturing: the manufacture of high-specification cathodes, electrolyte, anodes, and separators
- Cell assembly and QA/QC testing: cell assembly, electrolyte filling, electrode degassing, testing of the anode/cathode/assembled battery, and battery housing leak testing
- Recycling: raw materials from spent batteries can be reintroduced into the production chain, encouraging a circular lifecycle
In this workflow, a myriad of laboratory instruments are utilized. An ICP-OES can be used to quantify the elemental composition of battery materials by measuring the light emitted by excited atoms. It's effective for quality control and detecting impurities in raw materials and finished components, such as lithium, cobalt and nickel. Meanwhile, ICP-MS can be used for quantifying trace and ultra-trace impurities in battery materials. It measures the mass-to-charge ratio of ions generated from the sample in a plasma.
The non-destructive XRF technique, which analyzes the elemental composition of solid samples, is beneficial because it doesn't require the sample to be dissolved in a solution, allowing for the analysis of components in their original form. X-ray diffraction provides information on the crystalline structure and phase composition of battery materials, which is essential for understanding their performance and stability.
An SEM-EDS combines imaging with elemental analysis. An SEM provides a magnified view of the sample's surface and internal structure, while EDS detects X-rays generated when the electron beam interacts with the sample, allowing for rapid, accurate elemental mapping.
A simplified workflow
While all of these techniques provide valuable insights into structural and morphological changes, they lack the sensitivity needed to directly measure lithium. Additionally, more instruments present more opportunities for contamination, equipment failure, maintenance delays and more. Massbox, from Exum Instruments, addresses this gap by quantitatively measuring lithium—spatially and in depth—all in one instrument measuring 24" x 30" x 27".
At the heart of the Massbox is an analytical technique that combines Laser Ablation Laser Ionization (LALI) with Time-of-Flight Mass Spectrometry (TOF-MS). The first laser ablates tens to hundreds of nanometers of material from the sample’s surface. This enables direct analysis of solid or powdered materials without extensive sample preparation. Then, the ionization laser targets neutral particles created by the ablation process, creating ions that are more representative of the sample’s constituents than plasma-generated ions in traditional mass spectrometry techniques. Finally, the TOF mass analyzer creates a full mass spectrum at each laser spot, detecting low-mass elements like lithium and carbon to high-mass metallic elements. This capability supports comprehensive multi-element quantification and detailed elemental mapping.
Massbox operates under vacuum and features an advanced air-free transfer system, ensuring that lithium and other reactive materials can be analyzed without exposure to the atmosphere. This capability is crucial for preventing atmospheric reactions, preserving the integrity of the sample for accurate elemental analysis. Decreasing the time required for battery researchers and developers to characterize lithium behavior in electrodes helps accelerate research and product development cycles.
“For labs scaling up new battery chemistries, this efficiency translates directly to competitive advantage,” said Ellen Williams, EVP Business Development at Exum.
Depth profiling
Scientists developing and testing lithium-ion batteries must verify lithium distribution at different charge states; however, lithium is a challenging element to reliably measure and quantify with conventional techniques. Addressing these limitations, LALI-TOF-MS is a solution for depth profiling, mapping, and quantifying almost all elements in battery materials—including lithium.
Investigating the spatial distributions of elements helps characterize complex battery materials, track lithium, and identify failure mechanisms. For example, researchers at SLAC National Accelerator Laboratory used LALI-TOF-MS to track the elemental changes within electrodes to better understand solid electrolyte interphase formation.
A battery cell manufacturer explored 3D depth profiles for a set of silicon anodes at different charge states.3 Each anode was 40 microns thick and deposited on a copper current collector. The analysis examined areas of 1 mm by 1 mm with a 50-micron lateral resolution, continuing until the system ablated through the anode and into the copper current collector.
The results of the study showed that lithium was uniformly distributed throughout the anode’s cross section, providing data that can inform electrode and cell geometry optimization based on available lithium ions.
In addition to lithium, the analysis detected fluorine and trace amounts of cobalt. Since fluorine is a major constituent of the battery’s electrolyte, its presence in the anode confirms solid electrolyte interphase (SEI) layer formation. Understanding SEI formation and trace impurities in electrodes is critical to optimizing the battery cell’s performance, enhancing cycle life and improving safety.
Contamination detection
For battery scientists and engineers, challenges start with the supply chain as about 70% of the world’s cobalt comes from the Democratic Republic of Congo. That concentration in a single area can cause availability problems, forcing the industry to explore other options. However, labs must maintain quality control best practices to prevent manufacturing issues, such as metals contamination.
Spatial mapping reveals contaminants and non-uniform distributions of active elements, assisting in failure analyses and process control verification. LALI-TOF-MSenables the elemental mapping of electrodes by gathering comprehensive distribution data across material types. The LALI capabilities offer an adjustable laser spot size of 5 to 150 microns, revealing contaminant particles or local variations in electrodes’ active materials.
Visual mapping also makes variations in elemental concentrations easily identifiable. When engineers need to diagnose potential contaminants, LALI-TOF-MS determines the particles’ chemical compositions. Because Massbox chemically diagnoses and pinpoints problematic areas in less than 30 minutes, it supports quality control efforts without extensive sample preparation or laboratory operations.
Massbox’s elemental mapping and depth profiling can accelerate product development cycles and post-mortem failure analyses. Since the analytical process occurs under vacuum, it is suitable for air- and moisture-sensitive battery materials. Furthermore, its quantitative analysis empowers engineers to rapidly verify that all raw materials meet specifications.
Looking forward
The evolution from multiple specialized instruments to integrated analytical workflows represents more than just laboratory efficiency—it signals a fundamental shift in how battery research and product development can be conducted. As the industry faces mounting pressure to accelerate development timelines while maintaining rigorous quality standards, the ability to obtain comprehensive elemental data quickly becomes a competitive necessity.
The future of battery research will likely depend not just on novel materials, but on our ability to understand them comprehensively and quickly. In bridging the "valley of death" between research and commercialization, streamlined analytical workflows may prove as crucial as the innovations they're designed to characterize.
Emily Newton also contribued to this article