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Isotope analysis plays a critical role in various disciplines, including environmental science, archaeology, and forensic investigations. Traditional methods such as mass spectrometry provide precise isotopic data but often require complex, costly setups and extensive sample preparation. As an alternative, optical spectrometry has emerged as a versatile and less invasive technique. This presentation explores the advancements and applications of optical spectrometry methods in isotope analysis, emphasizing their benefits and challenges.
Lithium (Li), Boron (B), Nitrogen (N), Magnesium (Mg), and Calcium (Ca) are pivotal elements across various spheres such as the hydrosphere, biosphere, and lithosphere, significantly impacting (bio-) geochemical and physiological processes. These elements exhibit stable isotopes with substantial roles in geological, environmental, and biological studies. The traditional method for measuring isotope amount ratios has been through mass spectrometry, which, despite its accuracy, comes with high operational costs, the need for skilled operators, and time-consuming sample preparation processes.
Combining optical spectroscopy with chemometrics introduces an innovative, cost-effective approach by the hand of high-resolution continuum source atomic and molecular absorption spectrometry (HR-CS-AAS and HR-CS-MAS) for the analysis of isotope ratios in Li, B, N, Mg, and Ca. By analyzing the atomic or molecular absorption spectrum of the in-situ generated cloud of atoms of diatomic molecules (e.g., Li, BH, NO, MgF, CaF) during the electronic transition from the fundamental state, this method allows for the rapid determination of isotope ratios directly from sample solutions without the need for complex sample preparation.
For each element, the respective atomic or molecule's absorption spectrum was deconvoluted into its isotopic components using partial least squares regression or machine learning algorithms. Robust calibration models were developed, calibrated with enriched isotope, and validated against certified reference materials. Spectral data underwent preprocessing to optimize the modeling to determine the optimal number of latent variables.
The findings showcase that this optical spectrometric method yields results that agree with those obtained via inductively coupled plasma mass spectrometry (ICP-MS), offering a promising, cost-effective, and rapid alternative for isotope analysis with precisions as low as ± 0.2‰. This approach is a significant advancement in analytical chemistry, providing a new way to study isotope variations in biological, environmental, and geological samples.
What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries?
(2024)
Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries.
Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies.
Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance.
In this study, we demonstrate the applicability of nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) for Ca, Fe, and Se quantification in human serum using isotope dilution (ID) analysis. The matrix tolerance of MICAP-MS in Na matrix was investigated, uncovering that high Na levels can suppress the signal intensity. This suppression is likely due to the plasma loading and the space charge effect. Moreover, 40Ca and 44Ca isotopic fractionation was noted at elevated Na concentration. Nine certified serum samples were analyzed using both external calibration and ID analysis. Overestimation of Cr, Zn, As, and Se was found in the results of external calibration, which might be resulted from C-induced polyatomic interference and signal enhancement, respectively. Further investigations performed with methanol showed a similar enhancement effect for Zn, As, and Se, potentially supporting this assumption. The mass concentrations determined with ID analysis show metrological compatibility with the reference values, indicating that MICAP-MS combined with ID analysis can be a promising method for precise Ca, Fe, and Se determination. Moreover, this combination reduces the influences of matrix effects, broadening the applicability of MICAP-MS for samples with complex matrix.
Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben.
Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben.
Research into new sources for EUV lithography is driving advancements in experimental methods tailored for this short wavelength range. This progress enables the exploration of spectroscopic techniques aimed at monitoring electronic transitions within this energy spectrum. Laser-induced breakdown spectroscopy (LIBS) serves as a rapid tool for elemental analysis, primarily established in the UV-vis range. However, LIBS encounters challenges such as limited repeatability precision and elevated background noise resulting from continuum radiation.
In parallel, laser-induced extreme UV spectroscopy (LIXS) delves into the initial stages of plasma evolution, characterized by the emergence of soft X-ray and extreme UV radiation. The method benefits from a fast timeframe and constrained plasma confinement, leading to better precision. Nevertheless, LIXS encounters convoluted spectra arising from unresolved transition arrays (UTA), particularly pronounced for heavier elements. This complexity renders conventional univariate data analysis impractical, demanding the adoption of a multivariate data analysis approach.
Multiple cathode samples, each coated with varying stoichiometries of lithium nickel manganese cobalt oxide (NMC), were prepared and used for calibration purposes. Through the application of Partial Least Squares (PLS) regression, a robust correlation with an R2 value exceeding 0.97 was achieved. The LIXS technique underwent a comparative evaluation against UV-vis LIBS. Furthermore, a comparison between univariate and multivariate analysis approaches was conducted, incorporating validation through y-randomization to mitigate overfitting risks.
The viability of this approach was confirmed through the testing of an NMC reference material. The results showed metrological compatibility with reference values, underscoring the potential capability of the proposed methodology.
The application of multivariate data analysis is essential in extracting the full potential of laser-induced XUV spectroscopy (LIXS) for high-precision elemental mapping. LIXS offers significant advantages over traditional laser-induced breakdown spectroscopy in UV-vis (LIBS), including higher precision and a wider dynamic range,[1,2] while making it possible to determine light elements like lithium and fluorine. However, it is challenged by the presence of unresolved transition arrays (UTAs) for heavier elements. These UTAs add considerable complexity to the spectral data, often concealing crucial information. In this study, we employ well-established multivariate data analysis techniques and intensive data preprocessing to unravel this contained information.
The refined analysis reveals a high level of detail, enabling the precise identification of inhomogeneities within material samples. Our approach has particular relevance for studying aging processes in lithium-ion batteries (LIBs), specifically in relation to varying cathode materials and fluorine-containing polymer binder content. By combining elemental distribution with structural information, this improved method can offer a more comprehensive understanding of sample inhomogeneities and aging processes in LIBs, contributing to the development of more reliable and sustainable battery technologies.
Laser-induced XUV spectroscopy (LIXS) is an emerging technique for elemental mapping. In comparison to conventional laser-induced breakdown spectroscopy in UV-vis (LIBS), it has a higher precision and wider dynamic range, and it is well suited for the quantification light elements like lithium and fluorine. Further it can spot oxidation states. The XUV spectra are produced at a very early stage of the plasma formation. Therefore, effects from plasma evolution on the reproducibility can be neglected. It has been shown, that high-precision elemental quantification in precursor materials for lithium-ion batteries (LIBs) can be performed using LIXS. Based on these results, LIXS mapping was used to investigate aging processes in LIBs. Different cathode materials with varying compositions of fluorine containing polymer binders were compared at different stages of aging. Due to effects comparable to X-ray photoelectron spectroscopy but in reverse, monitoring of changes in the oxidation state is envisioned, which makes information about the chemical environment of the observed elements accessible. The combination of elemental distribution and structural information leads to a better understanding of aging processes in LIBs, and the development of more sustainable and safe batteries.
Introduction
Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs.
Methods
In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution.
Results
The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries.
Innovative aspects
- Quantitative depth profiling of cathode material
-Monitoring of corrosion processes in high energy-density lithium-ion batteries
- Systematic investigation of the influence of different cathode materials