Characterization of lithium phosphorus oxide thin film libraries by laser-induced breakdown spectroscopy imaging: A step towards high-throughput quantitative analyses

Berthou, William; Legallais, Maxime; Bousquet, Bruno; Motto-Ros, Vincent; Le Cras, Frédéric

doi:10.1016/j.sab.2024.106906

Spectrochimica Acta Part B: Atomic Spectroscopy

2024

DOI: 10.1016/j.sab.2024.106906

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Characterization of lithium phosphorus oxide thin film libraries by laser-induced breakdown spectroscopy imaging: A step towards high-throughput quantitative analyses

William Berthou,

Maxime Legallais,

Bruno Bousquet

et al.

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2024

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Cited by 2 publications

References 49 publications

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High‐Throughput Experimentation Unveils Composition – Structure – Conductivity Relationships in the Extended LiPON System

Berthou,

Legallais,

Sorieul

et al. 2024

Advanced Energy Materials

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A high‐throughput experimental approach is developed to assess the correlations between chemical composition, structure and conduction properties of inorganic solid ionic conductors. This approach covers the preparation of a large number of samples by combinatorial synthesis, followed by fast characterization of the material library. The approach is primarily based on combinatorial synthesis by magnetron co‐sputtering and the characterization of thin film samples where lithium phosphorus oxynitride (LiPON) is chosen as a case study. A library of 76 LiPON materials is prepared in one experiment from the reactive co‐sputtering of LiPO3 and Li3PO4 in a N2 atmosphere. A specific sample design allows conducting thickness and impedance measurements, Raman spectroscopy, then fast and spatially‐resolved chemical analysis by Laser‐Induced Breakdown Spectroscopy (LIBS) on each material. Particular developments are devoted to this technique to achieve quantitative analysis of lithium in thin films. The materials cover a wide range of compositions with 0.95<Li/P<2.03 and a high N/P nitrogen content of ≈1.0‐1.2. Two distinct compositional ranges can be distinguished. For 0.95<Li/P<1.2, conductivity increases and the PO3− chains gradually disappear, whereas for 1.2<Li/P<2.03, conductivity stabilizes despite continuous structural evolution, in parallel with an increase in charge carrier concentration.

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High‐Throughput Experimentation Unveils Composition – Structure – Conductivity Relationships in the Extended LiPON System

Berthou,

Legallais,

Sorieul

et al. 2024

Advanced Energy Materials

View full text Add to dashboard Cite

show abstract

Characterization of element distribution and thickness change in a high-capacity lithium-ion battery unit cell before and after charging via laser-induced plasma spectroscopy

Wang,

Lee,

Yoh

2024

Opt. Express

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The characterizations of the multi-layered cathode, separator, and anode as a single unit of commercial-grade high-nickel-based lithium-ion batteries (LIBs) are carried out to identify three-dimensional elemental distribution and to measure the electrode thickness change before and after being fully charged by using the laser-induced plasma spectroscopy (LIPS). It is found that, in addition to alterations in Li-ion concentration, the emission intensities in structural elements such as nickel in the cathode. Carbon in the anode also changed when the LIBs are charged to 100%, due to increased electron density from higher concentrations of easily ionized elements. Moreover, after charging, the contraction of the cathode and expansion of the anode are observed by correlation analysis of the depth-resolved plasma emission spectra. It is also revealed that the cathode thickness reduction caused by Li-ion deintercalation is smaller than the anode thickness expansion. Overall, the Li-ion structural units expand after charging. Unlike other approaches for measuring electrode thickness in LIBs, this study utilized LIPS mapping to uncover the electrode thickness changes. Thus, a simple and high-throughput method is explained for identifying the elemental and structural variations of high-nickel-based LIBs before and after charging.

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Characterization of lithium phosphorus oxide thin film libraries by laser-induced breakdown spectroscopy imaging: A step towards high-throughput quantitative analyses

Cited by 2 publications

References 49 publications

High‐Throughput Experimentation Unveils Composition – Structure – Conductivity Relationships in the Extended LiPON System

High‐Throughput Experimentation Unveils Composition – Structure – Conductivity Relationships in the Extended LiPON System

Characterization of element distribution and thickness change in a high-capacity lithium-ion battery unit cell before and after charging via laser-induced plasma spectroscopy

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