Study of the first step of hydrogen release in ammonia borane using high-resolution Raman spectroscopy and different heating ramps.

Ammonia borane, as a source of hydrogen, has attracted much attention due to its high hydrogen content, low molecular weight, and high stability in solution. However, the process and enhancement of hydrogen release must be done practically under ambient conditions. For this work, Raman spectroscopy, principal component analysis (PCA), and molecular simulation were applied to study the hydrogen release process of ammonia borane. Three stages of release were observed from room temperature to 1300 °C. The shift, the appearance, and the disappearance of the Raman bands were evident in the whole process. In-situ monitoring of Raman and PCA, with four different heating rates between 70 and 130 °C, was done; ammonia borane showed visible variations in its first release step, in which a fast rate helped reduce distortion in the release process. Finally, molecular simulation of ammonia borane using the Density Functional Theory (DFT) in calculations showed that dihedral rotation and stretching of the hydrogen bonds can occur before the first release step.

Ammonia borane structural study by temperature through high-resolution Raman spectroscopy and principal component analysis.

The structural change by temperature of the ammonia borane has been studied through Raman spectroscopy and principal components analysis (PCA). Its phase transition, from tetragonal to orthorhombic, was observed at 212 K. In addition, between 99 and 83 K, a zone of structural stability was observed. These behaviors could be observed thanks to the application of the PCA technique to the Raman data. Here, we can find a characteristic Raman signal which can also be associated with the orthorhombic structure. Also using the PCA technique, we have observed two Raman bands in the low frequency region, below 100 cm-1, which could be associated with the lattice vibrational contribution.

Moles quantification in liquid samples by Raman spectroscopy.

The mole is a unit of measurement that expresses amounts of a chemical substance. Its importance lies in that the mass and the number of molecules of a substance can be determined with this value. In this work, we suggest a mathematical expression that relates the number of moles of the sample studied with the Raman signal and the experimental parameters used. In other words, with this mathematical expression it is possible to obtain quantitative information in a simple manner from Raman spectra. We have applied this method to different samples and we have observed an excellent correlation between the experimental and expected data.

The effect of Nd and Mg doping on the micro-Raman spectra of LiNbO(3) single-crystals.

The LiNbO(3) congruent crystals doped with small Nd concentrations, <1 mol% Nd, and co-doped with Mg ions, 0-9 mol% Mg, were systematically investigated by means of micro-Raman spectroscopy in the Y and Z crystal directions. Results obtained from an undoped congruent crystal, an Nd-doped crystal, a Mg-doped crystal and Nd, Mg-co-doped crystals are compared. From the analyses of the results obtained in the Y direction, the Nd and Mg content dependence of the two lowest-Raman A(1)(TO(1)) and A(1)(TO(2)) modes, the half-width composition and the area ratio of the A(1)(TO(4)) and E(TO(8)) bands, we reached several conclusions about the incorporation mechanism of the Nd and Mg ions into the LiNbO(3) lattice. Likewise the Raman shift and half-width of the E(TO(1)) and E(TO(7)) modes were investigated in the Z direction. Results indicate that Mg and Nd ions are located in the Li site for low doping concentrations and for larger concentrations there is a replacement in both Li and Nb ion sites.

Phototransformation of C60 thin films by UV pulsed laser irradiation: comparative photoacoustic, AFM, and Raman studies.

Fullerene C60 films deposited by sublimation were irradiated with Kr-F laser in a wide fluence interval from 15 to 40 mJ/cm2. In situ photoacoustic analysis was applied to study the phase transformation during the irradiation. The results obtained were discussed in conjunction with atomic force microscopy (AFM) and Raman spectroscopy data. It was found that for a irradiation fluence interval from 22 to 30 mJ/cm2, 80% of C60 undergoes photopolymerization (presumably through 2 + 2 cycloaddition). For a laser energy higher than 30 mJ/cm2, a new amorphous carbon phase forms, having a large content of diamond-like, tetra-amorphous carbon (ta-C).

Application of principal component analysis and Raman spectroscopy in the analysis of polycrystalline BaTiO3 at high pressure.

The principal component analysis (PCA) was applied to Raman spectra of polycrystalline BaTiO(3) under pressure from atmospheric pressure to approximately 6.72 GPa. For the system utilized, PCA was able to distinguish spectral features and to determine the phase transition pressure: tetragonal to cubic at approximately 2.0 GPa. The present study demonstrates the potentialities of the application of PCA to the investigation on phase transitions at high pressure by Raman spectroscopy.