Estrutura e algumas propriedades ópticas de difenilfosfinatos de terras-raras

Coordination compounds of trivalent lanthanides cations with diphenylphosphinate are originated from direct reaction between a lanthanide salt and diphenylphosphinic acid. These complexes have peculiar and intriguing features, as (i) quickly obtainment through wet process precipitation, (ii) appreciable thermal stability, similar to inorganic phosphates, (iii) polymeric structure, and consequently, (iv) low solubility in both polar and non-polar solvents. Nowadays, coordination polymers are classified as coordination networks or, in case of porous materials, as metal-organic frameworks (MOFs). By this study, we aim to determine some optical properties of rare-earth diphenylphosphinate (RE = La3+, Eu3+, Gd3+, Lu3+) and conduct an updated classification of these compounds, bringing more details of its structure and the possible proposal of new materials with applications in lighting, detection of ionizing radiation and magnetism. The complexes of trivalent rare-earth cation with diphenylphosphinate were prepared by direct mixture of diphenylphosphinic acid with rare-earth metal chloride, both in ethanolic solution. The solution of diphenylphosphinic acid was kept in a beaker under constant stirring with pH measurements of the solution and gadolinium chloride solution was then dripped slowly with the aid of a burette until its complete addition; the following metal:ligand molar ratios were tested: 1:1, 1:2, 1:3, 2:1 e 3:1. The compounds were characterized by spectroscopic and structural techniques. By Fourier Transform Infrared Spectroscopy (FT-IR), it was possible to check the total ionization of diphenylphosphinic acid in synthesized complexes, confirmed by the absence of the band type A, B, C related to ѵ(O-H) of the acid (2663 cm-1, 2168 cm-1, 1684 cm-1), as well as the disappearance of ѵ(P-OH)=961 cm-1. Furthermore, the occurrence of bands shifts of ѵ(POO-) [symmetrical and asymmetrical] of...

Aplicação de carbono vítreo monolítico para produção de eletrodos a partir da resina furfurílica com diferentes variações de pH

Nowadays, we live in a time of rapid research for technological advances, in a way that this pursuit of new technologies is deeply connected to the diversity of new materials that have been developed by mankind. It deals with issues such as materials with enhanced properties which offer better quality, less cost and high performance, while they are accessible both in their production and moment of operation. In this context, it was required to develop electrodes that were easy to prepare as well as which present high electric conductivity and good mechanic proprieties by using carbonaceous material as basis. For this reason, the best parameters of the furfuryl resin cures were established with different pH variations through viscosimetric measurements and differential scanning calorimetry. By scanning electron microscopy (SEM) was possible to identify an increased porosity in the samples with pH 7 and pH 8, as compared to samples with lower pH content. After carbonization of the material, the characterization of monolithic glassy carbon was held by means of FT-IR techniques, Raman spectroscopy, X-ray diffraction and cyclic voltammetry. The spectra showed that the change in pH does not have significant influence on the crystallographic ordering of the material and its structural characteristics. As for the electrochemical character, the CVM electrodes showed excellent response, with good reversibility and wide potential window. Some voltammetric curve deviations were only observed for the sample with pH 4, which may be related to processing parameters adopted