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Ultrasounds assisted electrosynthesis of zero valence iron nanoparticles : study of the deposit growth and dispersion by acoustic waves

Abstract : This study concerns the coupling of the ultrasounds with the electrodeposition process for the synthesis of zero-valent iron nanoparticles; it is structured in two sections. The first focuses on the electrode substrate used for the iron electrodeposition and aims to determine its influence on both the deposit growth and its dispersion by ultrasonication. The interfacial and the adhesion energies of the deposit on the substrate (Y_(Fe/substrate) and W_(Fe/substrate) respectively) being related to the surface energy and the roughness of the substrate, a particular focus is put on the influence of these two properties. Thus, two materials of different surface energies, gold (Au) and vitreous carbon (VC), as well as various roughnesses, are tested. Considering only the Van der Waals interactions, a theoretical development has enabled to determine that Y_(Fe/VC)>Y_(Fe/Au) which suggests a better affinity of the iron deposit with the gold than with the VC substrate. This difference impacts the deposit morphology (2D growth on the gold and 3D growth on the VC substrate) but also the deposit adhesion. Indeed, experiments performed to study the effect of ultrasounds on the iron electrodeposit reveal its progressive and complete dispersion for the vitreous carbon case while no dispersion (no removal of the deposit from the electrode) is obtained with the gold substrate. The second section of the present study deals with the synthesis of iron nanoparticles; to this end, the electrodeposition of branched deposits has been investigated in a Hele-Shaw cell integrating a vibrating element (piezoelectric diaphragm), expected to allow both the deposit formation and its fragmentation. Experiments reveal that the hydrogen bubbles, formed by the co-reduction of free protons during the iron electrodeposition, strongly influence the fragmentation process. Using high vibration frequencies and high amplitudes, the bubbles oscillate with surface deformations, inducing interface velocity sufficiently high (˜ 4 m/s) to allow the fragmentation of the deposit into particles of sizes ranging between 1 µm and 100 nm and showing a high specific surface due to their dendritic morphology. Thus this work opens the way for a new particles manufacturing technology.
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Audrey Iranzo. Ultrasounds assisted electrosynthesis of zero valence iron nanoparticles : study of the deposit growth and dispersion by acoustic waves. Chemical and Process Engineering. Université Paul Sabatier - Toulouse III, 2016. English. ⟨NNT : 2016TOU30317⟩. ⟨tel-01633833⟩

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