TiO2 nanoparticles (NPs), 3 nm in size, were injected inside a very-low-pressure O2 plasma reactor using a liquid injector and following an iterative injection sequence.Simultaneously, hexamethyldisiloxane (HMDSO) vapor precursor was added to create a SiO2 matrix and a TiO2-SiO2 nanocomposite (NC) thin film. Both the liquid injection and vapor precursor parameters were established to address the main challenges observed when creating NCs. In contrast to most aerosol-assisted plasma deposition processes, Scanning/Transmission Electron Microscopy (S/TEM) indicated isolated (i.e. non-agglomerated) NPs distributed in a rather uniform way in the matrix. The fraction of the TiO2 NPs inside the SiO2 matrix was estimated by SEM, Spectroscopic Ellipsometry (SE), and X-ray Photoelectron Spectroscopy.All techniques provided coherent values, with percentages between 12 and 19%. Despite the presence of TiO2 NPs, SE measurements confirmed that the plasma-deposited SiO2 matrix was dense with an optical quality similar to the one of thermal silica. Finally, the percentage of TiO2 NPs inside the SiO2 matrix and the effective refractive index of the NCs can be tuned through judicious control of the injection sequence.

TiO2 nanoparticles (NPs) thin films with a thickness of 50 nm and a coreshell nanostructure were prepared using the spin coating technique and were treated using an inductively coupled O2 plasma at low pressure. While no significant features were observed during pumping, two kinetics can be identified during plasma processing using in situ spectroscopic ellipsometry. For very short plasma treatment times, the removal of solvent-based organic moieties surrounding TiO2 nanoparticles produces a densification of the inorganic TiO2 films. Such mineralization effect by the O2 plasma treatment was confirmed by X-ray photoelectron microscopy. For larger time scales, the average size of TiO2 NPs rises and significant changes of the optical properties occur. While no significant changes in the film nanostructure were observed by Scanning Electron Microscopy, a rise in the crystallite size and an increase in the agglomeration of TiO2 nanoparticles were confirmed by Transmission Electron Microscopy and Atomic Force Microscopy, respectively. The mechanisms involved in such plasma-induced modification of nanostructured TiO2 thin films are discussed in line with the energy fluxes of plasma-generated species.

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