Antireflective Coatings with Adjustable Refractive Index and Porosity Synthesized by Micelle-Templated Deposition of MgF₂ Sol Particles

Minimizing efficiency losses caused by unwanted light reflection at the interface between lenses, optical instruments and solar cells with the surrounding medium requires antireflective coatings with adequate refractive index and coating thickness. We describe a new type of antireflective coating material with easily and independently tailorable refractive index and coating thickness based on the deposition of colloidal MgF₂ nanoparticles. The material synthesis employs micelles of amphiphilic block copolymers as structure directing agent to introduce controlled mesoporosity into MgF₂ film. The coatings thickness can be easily adjusted by the applied coating conditions. The coatings refractive index is determined by the materials porosity, which is controlled by the amount of employed pore template. The refractive index can be precisely tuned between 1.23 and 1.11, i.e., in a range that is not accessible to nonporous inorganic materials. Hence, zero reflectance conditions can be established for a wide range of substrate materials

A New Model for Nano-TiO₂ Crystal Birth and Growth in Hydrothermal Treatment Using an Oriented Attachment Approach

The synthesis of TiO₂ was studied in an original hydrothermal process that uses triethanolamine titanium complex Ti­(TeoaH)₂ as a Ti precursor and triethanolamine (TeoaH₃) as a shape controller to obtain bipyramidal anatase nanoparticles. Backed-up by experimental evidence, i.e., time profiles for Ti­(IV) species concentrations together with crystal shape and particle size distributions measured by dynamic light scattering and electron microscopy, a mathematical model was built. The model includes chemical reactions responsible for TiO₂ generation in solution and the subsequent anatase nucleation and crystal growth. The oriented attachment mechanism was adopted to explain the build-up of crystals with equilibrium anatase structure (Wulff structure) and time-varying shape factor. This complex mathematical model was solved writing and validating an in-house software using the Matlab (Natick, MA, USA) environment. The process was simulated for a batch time of 50 h, and the results, in terms of main species concentration and crystal size distributions, are in rather good agreement with the experimental measurements

New Approach on Quantification of Porosity of Thin Films via Electron-Excited X‑ray Spectra

One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thin templated mesoporous TiO₂ films, dip-coated on silicon wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films