ABSTRACT Manganese oxides were synthesized during 40 min at 140 ºC via Microwave-Assisted Hydrothermal (MAH) method and treated at different temperatures in order to evaluate the phase evolution using structure refinement (Rietveld method). The samples obtained were heat treated at temperatures defined by means of thermal analysis (160 ºC, 480 ºC, 715 ºC, 870 ºC, 920 ºC and 1150 ºC) and analyzed by X-Ray Diffractometry (XRD), X-Ray Fluorescence (XRF), Fourier Transform Infrared (FTIR) spectroscopy, Raman scattering, UV-Vis absorption and Scanning Electron Microscopy (SEM). Structural characterizations allowed to identify five distinct phases: α-MnO2, Mn3O4, Mn5O8, Na2Mn5O10 and Na4Mn9O18 with weight percentages dependent on the heat treatment. The hausmannite structure (average crystallite size ranging from 28.9 nm to 99.1 nm) is present in all samples and go through various oxidation and reduction processes from 160 ºC to 1150 ºC without any major variation in the lattice parameters. Chemical characterizations identifies the presence of Na+ ions in all samples, either as substitution defects or as components of specific crystalline structures (Na2Mn5O10 and Na4Mn9O18), showing that the synthesized manganese oxides works as Na+ intercalation compounds, important materials for energy storage devices optimization. The results presented enables a better interpretation of the thermal and structural characteristics of manganese oxides synthesized via MAH.

The analysis of supramolecular arrangement is essential to understand the role of this key factor on the optical and electrical properties of organic thin films. In this work, thin solid films of bis(phenethylimido) perylene (PhPTCD) fabricated using physical vapor deposition (PVD) technique (thermal evaporation), deposited simultaneously onto different substrates (Ag mirror, Ge, and quartz plates) contingent on the characterization technique. The main objective is to study the PhPTCD supramolecular arrangement and the thermal stability of this arrangement in PVD films. The ultraviolet-visible absorption reveals a controlled growth of the PVD films, and the micro-Raman scattering data show that the PhPTCD molecule is not thermally degraded in the conditions of these experiments. The microscopy also shows a homogeneous morphological surface of the PVD film at macro and micro scales, with molecular aggregates at nanoscale. Besides, the PVD film roughness does not follow substrate roughness. The X-ray diffraction indicates a crystalline structure for PhPTCD powder and an amorphous form for PhPTCD PVD film. The infrared absorption spectroscopy points to a preferential flat-on organization of the molecules in the PVD films. In addition, the annealing process (200 ºC for 20 minutes) does not affect the supramolecular arrangement of the PhPTCD PVD films.

The supramolecular structure of organic thin films is a key factor in their optical and electrical properties and, consequently, in the technological applications involving organic electronic. Here, thin films of a perylene derivative, the bis butylimido perylene (BuPTCD), were produced by vacuum thermal evaporation (PVD, physical vapor deposition). The main objective is to investigate the supramolecular structure of the BuPTCD in these PVD films, which implies to control their thickness at nanometer scale and to determine their molecular organization, morphology at micro and nanometer scales and crystallinity. The ultraviolet-visible absorption reveals a uniform growth of the PVD films. The optical and atomic force microscopy images show a homogeneous surface of the film at micro and nanometer scales, respectively. The X-ray diffraction indicates that both powder and PVD film are in the crystalline form. Complementary, a preferential head-on orientation of the molecules in the PVD films is determined via infrared absorption spectroscopy. Besides, the annealing process (200oC) did not affect the molecular organization of the PVD films, revealing a thermal stability of the BuPTCD molecules within the PVD films. Through DC electrical measurements, an electrical conductivity of 7.45x10-10 S/m was determined for BuPTCD PVD films onto Au interdigitated electrodes (IDE-structured devices), which can be enhanced, under illumination, by two orders of magnitude (photoconductivity effect). As proof-of-concept, the IDE-structured devices are tested as gas sensor for trifluoroacetic acid.