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1.
Nanoscale ; 14(30): 10950-10957, 2022 Aug 04.
Artigo em Inglês | MEDLINE | ID: mdl-35860928

RESUMO

We have investigated the early stages of the formation of iron oxide nanoparticles from iron stearate precursors in the presence of sodium stearate in an organic solvent by in situ liquid phase transmission electron microscopy (IL-TEM). Before nucleation, we have evidenced the spontaneous formation of vesicular assemblies made of iron polycation-based precursors sandwiched between stearate layers. Nucleation of iron oxide nanoparticles occurs within the walls of the vesicles, which subsequently collapse upon the consumption of the iron precursors and the growth of the nanoparticles. We then evidenced that fine control of the electron dose, and therefore of the local concentration of reactive iron species in the vicinity of the nuclei, enables controlling crystal growth and selecting the morphology of the resulting iron oxide nanoparticles. Such a direct observation of the nucleation process templated by vesicular assemblies in a hydrophobic organic solvent sheds new light on the formation process of metal oxide nanoparticles and therefore opens ways for the synthesis of inorganic colloidal systems with tunable shape and size.

2.
Small Methods ; 6(2): e2100891, 2022 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-34954905

RESUMO

Micro-batteries are attractive miniaturized energy devices for new Internet of Things applications, but the lack of understanding of their degradation process during cycling hinders improving their performance. Here focused ion beam (FIB)-lamella from LiMn1.5 Ni0.5 O4 (LMNO) thin-film cathode is in situ cycled in a liquid electrolyte inside an electrochemical transmission electron microscope (TEM) holder to analyze structural and morphology changes upon (de)lithiation processes. A high-quality electrical connection between the platinum (Pt) current collector of FIB-lamella and the microchip's Pt working electrode is established, as confirmed by local two-probe conductivity measurements. In situ cyclic voltammetry (CV) experiments show two redox activities at 4.41 and 4.58/4.54 V corresponding to the Ni2+/3+ and Ni3+/4+ couples, respectively. (S)TEM investigations of the cycled thin-film reveal formation of voids and cracks, loss of contact with current collector, and presence of organic decomposition products. The 4D STEM ASTAR technique highlights the emergence of an amorphization process and a decrease in average grain size from 20 to 10 nm in the in situ cycled electrode. The present findings, obtained for the first time through the liquid electrochemical TEM study, provide several insights explaining the capacity fade of the LMNO thin-film cathode typically observed upon cycling in a conventional liquid electrolyte.

3.
J Am Chem Soc ; 142(43): 18422-18436, 2020 Oct 28.
Artigo em Inglês | MEDLINE | ID: mdl-33054192

RESUMO

Fast-ion conductors are critical to the development of solid-state batteries. The effects of mechanochemical synthesis that lead to increased ionic conductivity in an archetypical sodium-ion conductor Na3PS4 are not fully understood. We present here a comprehensive analysis based on diffraction (Bragg and pair distribution function), spectroscopy (impedance, Raman, NMR and INS), and ab initio simulations aimed at elucidating the synthesis-property relationships in Na3PS4. We consolidate previously reported interpretations regarding the local structure of ball-milled samples, underlining the sodium disorder and showing that a local tetragonal framework more accurately describes the structure than the originally proposed cubic one. Through variable-pressure impedance spectroscopy measurements, we report for the first time the activation volume for Na+ migration in Na3PS4, which is ∼30% higher for the ball-milled samples. Moreover, we show that the effect of ball-milling on increasing the ionic conductivity of Na3PS4 to ∼10-4 S/cm can be reproduced by applying external pressure on a sample from conventional high-temperature ceramic synthesis. We conclude that the key effects of mechanochemical synthesis on the properties of solid electrolytes can be analyzed and understood in terms of pressure, strain, and activation volume.

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