The interaction of (3-Aminopropyl)triethoxysilane (APTES) with pulsed late Ar-O 2 afterglow is characterized by the synthesis of OH, CO and CO 2 in the gas phase as main by-products. Other minor species like CH, CN and C 2 H are also produced. We suggest that OH radicals are produced in a first step by dehydrogenation of APTES after interaction with oxygen atoms. In a second step, the molecule is oxidized by any O 2 state, to form peroxides that transform into by-products, break thus the precursor CC bonds. If oxidation is limited, i.e. a low duty cycle, fragmentation of the precursor is limited and produced nanoparticles keep the backbone structure of the precursor, but contain amide groups produced from the amine groups initially available in APTES. At high duty cycle, silicon-containing fragments contain some carbon and react together and produce nanoparticles with a non-silica-like structure.
From results of in situ FTIR absorption and optical emission spectroscopy, the interaction of (3‐aminopropyl)triethoxysilane (APTES) with late ArN2 afterglow is shown to occur mainly with N atoms. They react preferentially with carbon from CHx groups in the precursor, leading to the synthesis of CN bonds. No production of NH radical is observed, demonstrating the lack of direct reaction between active nitrogen and APTES. The NH2 group is not affected by the afterglow. One of the CC bonds of the propylamine group in the APTES is likely broken. These nanoparticles present secondary amides due to reactions with active nitrogen. They are amorphous and react in air to produce a salt.
Discharges in heptane in pin-to-plate configuration are produced between a platinum wire and a (100)-oriented silicon wafer coated by a carbon nanotube (CNT) carpet. This carpet is used to simulate the behavior of a nanostructured surface in electro-discharge machining (EDM) where small protrusions on the surface could play a similar role. CNTs behave like simple electrical conductors between the discharge and the silicon wafer. They act as if they would focus the current on smaller areas. The average diameter of impacts is about five times smaller if the silicon wafer is coated by a CNTcarpet. The underlying silicon surface is heated by the plasma and melts, forming a central spot surrounded by a serrated trailing edge. The current density being about one order of magnitude larger when a CNT carpet is present, the induced magnetic field stirs the molten silicon, creating serrations all around the impact. Hot nanoparticles of carbon coming from the plasma fall and roll randomly on the silicon surface where they create wavy micro-channels. Nanowires that are detached from the surface are covered by nanoparticles of platinum in the plasma and embedded within an amorphous carbon layer deposited on the nanotube. However, these effects can only be observed if the current density is high enough (>%10 A mm À2 depending on the material) like in micro-EDM but not in nano-EDM.
RuO2 nanowires are synthesized by oxidation of ruthenium thanks to a micro-post-discharge at atmospheric pressure. However, RuO2 nanowires form islands. The growth mechanism depending on surface defects, the surface density of the nanowires is limited. We report on the influence of two alkali salts, NaCl and KCl, deposited as grains on ruthenium to act as defects and increase the nanowire density. These grains induce the growth of RuO2 nanowires all around them, creating a circular area where nanowires are found. Nanowires start growing at the triple point at the grain base where the alkali-salt grain, ruthenium from the substrate and oxidizing gaseous species coexist. When nanowires grow, the stress induced in the surrounding layer creates new cracks, making possible the radial propagation of the nanowires. The presence of nanowires on grains is due to the etching mechanism that converts the alkali salt into an oxide, enabling onward oxidation of ruthenium.
Oxidation by a micro-post-discharge at atmospheric pressure of thin films of ruthenium deposited on fused silica by pressure-modulated magnetron sputtering is studied. Single-crystalline RuO 2 nanowires are obtained for the first time with a diffusion process over large areas. Nanowires grow typically at temperatures below 550-600 K, provided the level of stress is high enough to fragment grains in sub-grains with sizes between 30 and 50 nm. Because of the alternation of dense and porous layers forming the coating, inward diffusion of vacancies leads to no patent Kirkendall's effect, pores being distributed over the whole coating thickness and not mainly at the interface with the substrate. The centre of the treatment being heated at temperatures higher than 900 K, gaseous RuO 4 is formed, leading to an evaporated area. At its edge, a ring of microcrystals is formed, likely by a CVD mechanism.
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