Compromising Science by Ignorant Instrument Calibration—Need to Revisit Half a Century of Published XPS Data

Greczyński, Grzegorz; Hultman, Lars

doi:10.1002/ange.201916000

Cited by 179 publications

(27 citation statements)

References 22 publications

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“…3d) shows signals coming from all oxygenated species at the surface. The prominent oxygen peak at 532 eV corresponds to a mix of oxygen from NiAl LDH structure and other oxygenated species from surface contamination environments (CO and COO groups) [40]. The XPS analysis demonstrates that the Ni 2+ and Al 3+ elements coexist in the product, which is in good accordance with the prediction.…”

Section: Resultssupporting

confidence: 79%

Electrochemical study on nickel aluminum layered double hydroxides as high-performance electrode material for lithium-ion batteries based on sodium alginate binder

Fortunato

Cardinale

et al. 2021

J Solid State Electrochem

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Nickel aluminum layered double hydroxide (NiAl LDH) with nitrate in its interlayer is investigated as a negative electrode material for lithium-ion batteries (LIBs). The effect of the potential range (i.e., 0.01–3.0 V and 0.4–3.0 V vs. Li+/Li) and of the binder on the performance of the material is investigated in 1 M LiPF6 in EC/DMC vs. Li. The NiAl LDH electrode based on sodium alginate (SA) binder shows a high initial discharge specific capacity of 2586 mAh g−1 at 0.05 A g−1 and good stability in the potential range of 0.01–3.0 V vs. Li+/Li, which is better than what obtained with a polyvinylidene difluoride (PVDF)-based electrode. The NiAl LDH electrode with SA binder shows, after 400 cycles at 0.5 A g−1, a cycling retention of 42.2% with a capacity of 697 mAh g−1 and at a high current density of 1.0 A g−1 shows a retention of 27.6% with a capacity of 388 mAh g−1 over 1400 cycles. In the same conditions, the PVDF-based electrode retains only 15.6% with a capacity of 182 mAh g−1 and 8.5% with a capacity of 121 mAh g−1, respectively. Ex situ X-ray photoelectron spectroscopy (XPS) and ex situ X-ray absorption spectroscopy (XAS) reveal a conversion reaction mechanism during Li+ insertion into the NiAl LDH material. X-ray diffraction (XRD) and XPS have been combined with the electrochemical study to understand the effect of different cutoff potentials on the Li-ion storage mechanism. Graphical abstract The as-prepared NiAl-NO3−-LDH with the rhombohedral R-3 m space group is investigated as a negative electrode material for lithium-ion batteries (LIBs). The effect of the potential range (i.e., 0.01–3.0 V and 0.4–3.0 V vs. Li+/Li) and of the binder on the material’s performance is investigated in 1 M LiPF6 in EC/DMC vs. Li. Ex situ X-ray photoelectron spectroscopy (XPS) and ex situ X-ray absorption spectroscopy (XAS) reveal a conversion reaction mechanism during Li+ insertion into the NiAl LDH material. X-ray diffraction (XRD) and XPS have been combined with the electrochemical study to understand the effect of different cutoff potentials on the Li-ion storage mechanism. This work highlights the possibility of the direct application of NiAl LDH materials as negative electrodes for LIBs.

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Section: Resultssupporting

confidence: 79%

Electrochemical study on nickel aluminum layered double hydroxides as high-performance electrode material for lithium-ion batteries based on sodium alginate binder

Fortunato

Cardinale

et al. 2021

J Solid State Electrochem

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“…[ 18 ] The XPS binding energy calibration is based on the Mg 2p peak in this study ( Figure 1 a), as several studies have indicated that using C 1s for calibration is sometimes not robust. [ 19 ] The Ti oxidation state is relatively stable upon calcination (Figure 1c). As indicated by the O 1s spectra (Figure 1d), the precursor is composed of chemisorbed/physisorbed water and metal hydroxide (Ni hydroxide predominantly).…”

Section: Resultsmentioning

confidence: 99%

Probing Dopant Redistribution, Phase Propagation, and Local Chemical Changes in the Synthesis of Layered Oxide Battery Cathodes

Yang

Hou

et al. 2020

Advanced Energy Materials

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Achieving the targeted control of layered oxide properties calls for more fundamental studies to mechanistically probe their evolution during their synthesis. Herein, dopant distribution, phase propagation, and local chemical changes as well as their interplay in multielement‐doped LiNiO2 materials are investigated using spectroscopic, imaging, and scattering techniques. It is shown that dopants undergo dynamic redistribution in the Ni(OH)2 host lattice at the early stage of calcination (below 300 °C). Such redistribution behavior exhibits strong dopant‐dependent characteristics, allowing for targeted surface and bulk doping control. The Ni oxidation process exhibits depth‐dependent characteristics and the most rapid Ni oxidation takes place between 300 and 700 °C. Using Ni oxidation state as the proxy for the phase transformation, the buildup of heterogenous phase propagation in the early stage of calcination is shown, especially along the radial direction of secondary particles. The radial heterogenous phase distribution gradually decreases upon completing the calcination. However, a high degree of mosaic‐like heterogeneity may still be present in the final product, departing from the perfect layered oxide. The present study offers fundamental insights into manipulating multiscale materials properties during calcination for obtaining stable, high‐energy layered oxide cathodes.

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“…It is worth to point out that the binding energy (BE) scale of the spectrometer was calibrated using the ISO-certified procedure to avoid problems related to the use of the C 1s peak of adventitious carbon [81,82] .…”

Section: X-ray Photoelectron Spectroscopymentioning

confidence: 99%

Nonstoichiometric Multicomponent Nitride Thin Films

Shu

2020

Linköping Studies in Science and Technology. Licentiate Thesis

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High entropy ceramics have rapidly developed as a class of materials based on high entropy alloys; the latter being materials that contain five or more elements in near-equal proportions. Their unconventional compositions and chemical structures hold promise for achieving unprecedented combinations of mechanical, electrical and chemical properties. In this thesis, high entropy ceramic films, (TiNbZrTa)Nx were deposited using reactive magnetron sputtering with segmented targets. The stoichiometry x was tuned with two deposition parameters, i.e., substrate temperature and nitrogen flow ratio fN, their effect on microstructure and mechanical, electric, and electrochemical properties were investigated.

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Compromising Science by Ignorant Instrument Calibration—Need to Revisit Half a Century of Published XPS Data

Cited by 179 publications

References 22 publications

Electrochemical study on nickel aluminum layered double hydroxides as high-performance electrode material for lithium-ion batteries based on sodium alginate binder

Electrochemical study on nickel aluminum layered double hydroxides as high-performance electrode material for lithium-ion batteries based on sodium alginate binder

Probing Dopant Redistribution, Phase Propagation, and Local Chemical Changes in the Synthesis of Layered Oxide Battery Cathodes

Nonstoichiometric Multicomponent Nitride Thin Films

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