We report on the delithiation of LiCoO2 thin films using oxalic acid (C2H2O4) with the goal of understanding the structural degradation of an insertion oxide associated with Li chemical extraction. Using a multi-technique approach that includes synchrotron radiation X-ray diffraction, scanning electron microscopy, micro Raman spectroscopy, photoelectron spectroscopy and conductive atomic force microscopy we reveal the balance between selective Li extraction and structural damage. We identify three different delithiation regimes, related to surface processes, bulk delithiation and damage generation. We find that only a fraction of the grains is affected by the delithiation process, which may create local inhomogeneities. However, the bulk delithiation regime is effective to delithiate the LCO film. All experimental evidence collected indicates that the delithiation process in this regime mimics the behavior of LCO upon electrochemical delithiation. We discard the formation of Co oxalate during the chemical extraction process. In conclusion, the chemical route to Li extraction provides additional opportunities to investigate delithiation while avoiding the complications associated with electrolyte breakdown and simplifying in-situ measurements.

/pdf/a-multi-technique-approach-to-understanding-delithiation-59m3riolgv.pdf

A multi-technique approach to understanding delithiation damage in LiCoO2 thin films

Infrared (IR) spectroscopy is a powerful technique to characterize the chemical structure and dynamics of various types of samples. However, the signal-to-noise-ratio drops rapidly when the sample thickness gets much smaller than penetration depth, which is proportional to wavelength. This poses serious problems in analysis of thin films. In this work, an approach is demonstrated to overcome these problems. It is shown that a standard IR spectroscopy can be successfully employed to study the structure and composition of films as thin as 20 nm, when the layers were grown on porous substrates with a well-developed surface area. In contrast to IR spectra of the films deposited on flat Si substrates, the IR spectra of the same films but deposited on porous ceramic support show distinct bands that enabled reliable chemical analysis. The analysis of Zn-S ultrathin films synthesized by atomic layer deposition (ALD) from diethylzinc (DEZ) and 1,5-pentanedithiol (PDT) as precursors of Zn and S, respectively, served as proof of concept. However, the approach presented in this study can be applied to analysis of any ultrathin film deposited on target substrate and simultaneously on porous support, where the latter sample would be a reference sample dedicated for IR analysis of this film.

Infrared Absorption Study of Zn–S Hybrid and ZnS Ultrathin Films Deposited on Porous AAO Ceramic Support

We report on the delithiation of LiCoO2 thin films using oxalic acid (C2H2O4) with the goal of understanding the structural degradation of an insertion oxide associated with Li chemical extraction. Using a multi-technique approach that includes synchrotron radiation x-ray diffraction, scanning electron microscopy, micro Raman spectroscopy, photoelectron spectroscopy and conductive atomic force microscopy we reveal the balance between selective Li extraction and structural damage. We identify three different delithiation regimes, related to surface processes, bulk delithiation and damage generation. We find that only a fraction of the grains is affected by the delithiation process, which may create local inhomogeneities. The chemical route to Li extraction provides additional opportunities to investigate delithiation while avoiding the complications associated with electrolyte breakdown and could simplify in situ measurements.


 This work focuses on the investigation of Co/Cu removal rate (RR) selectivity and reduction of galvanic corrosion associated with Co and Cu by using oxalic acid (weak acid) as the complexing agent and imidazole as an inhibitor in hydrogen peroxide (H2O2) and fumed silica-based slurry. The results obtained from a dissolution study, polishing experiments, and potentiodynamic polarization measurements revealed that the proposed chemistry can achieve a desirable Co/Cu RR selectivity and a significant decrease in corrosion potential of Co and Cu (pH 9) to be used in the semiconductor industry. The corrosion potential difference (CuEcorr - CoEcorr) was reduced to 12 mV by using 0.1 wt.% H2O2 + 0.02 M oxalic acid + 5 ppm imidazole solution at pH 9. Meanwhile, a removal rate of ~147 nm/min for Co and ~140 nm/min for Cu was achieved using the same composition in a fumed silica slurry which resulted in Co/Cu selectivity ratio of 1.05:1, which is acceptable for cobalt barrier and copper interconnect CMP. Based on Fourier transform infrared and ultraviolet spectra, the dissolution mechanism in the proposed chemistry is also discussed.

Controlling Galvanic Corrosion with Oxalic Acid and Imidazole for Chemical Mechanical Planarization of Cobalt-Copper Interface

Evaluation of photocatalytic properties of zinc and cobalt mixed oxide recycled from spent Li-ion and Zn–MnO2 batteries in photo-Fenton-like process

Synthesis and Characterization of Cobalt Oxalate Nanomaterial for Li-Ion Battery

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Synthesis and Characterization of Cobalt Oxalate Nanomaterial for Li-Ion Battery