RESUMO Três processos diferentes para a sintetização de composto de grafite intercalado esfoliado foram testados em dois tipos de grafites diferentes, um em forma de pó e o outro na forma de flocos. Cada grafite foi oxidado nas mesmas condições experimentais (de sonificação, neutralização, filtragem e secagem), porém utilizando três agentes oxidantes diferentes (H2O2, HNO3 e KClO3), previamente misturados com H2SO4. As amostras sintetizadas resultantes foram caracterizadas por difração de raios X, espectroscopia Raman e microscopia eletrônica de varredura. A análise dos espectros Raman das amostras oxidadas mostrou correspondência com a do grafeno de poucas camadas. Delaminação e exfoliação em maior proporção foram observadas nas amostras do grafite original em pó, tratado com H2SO4/HNO3.

ABSTRACT Three different processes for the synthetization of exfoliated graphite intercalation compound have been tested in two different type of graphite, one in powder form and the other one as flakes. Each graphite was oxidized applying the same experimental conditions (sonification, neutralization, filtering and drying) but using three different auxiliary oxidizers (H2O2, HNO3 and KClO3) previously mixed with H2SO4. The resulting synthesized samples were characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscopy. The Raman spectra analysis of the oxidized samples correspond to that of a graphene of few layers. Stronger delamination and exfoliation were observed in the samples of graphite, originally in powder form, treated with H2SO4/HNO3.

A mechanical spectroscopy study of Cu-Zr-Al bulk metallic glasses, was performed with two types of equipment: a Kê-type inverted torsion pendulum and an acoustic elastometer, working in the frequency ranges of Hz and kHz, respectively, with a heating rate of 1 K/min. The analysis of the anelastic relaxation shows similar spectra for both types of equipment resulting in internal friction patterns that vary with temperature and are not reproducible at each thermal cycle. The normalized of the square of the frequency changes from the first to later measurement cycles. These results indicate that the specimens of Cu-Zr-Al alloys were changing by mechanical relaxation, owing to the motion of atoms or clusters in the glassy state and possible "defects" produced during the processing of alloys.

Dynamical Elastic Moduli of the Ti-13Nb-13Zr biomaterial alloy were obtained using the mechanical spectroscopy technique. The sample with heat treatment at 1170K for 30 minutes and water quenched with subsequent aging treatment at 670 K for 3 hours (TNZ + WQ + 670 K/3 h), was characterized through decay of free oscillations of the sample in the flexural vibration mode. The spectra of anelastic relaxation (internal friction and frequency) in the temperature range from 300 K to 625 K not revealed the presence of relaxation process. As shown in the literature, the hcp structure usually does not exhibit any relaxation due to the symmetry of the sites in the crystalline lattice, but if there is some relaxation, this only occurs in special cases such as low concentration of zirconium or saturation of the stoichiometric ratio of oxygen for zirconium. Dynamical elastic modulus obtained for TNZ + WQ + 670 K/3 h alloy was 87 GPa at room temperature, which is higher than the value for Ti-13Nb-13Zr alloy (64 GPa) of the literature. This increment may be related to the change of the proportion of α and β phases. Besides that, the presence of precipitates in the alloy after aging treatment hardens the material and reduces its ductility.

Mechanical spectroscopy measurements have been extensively used in the last decades to obtain information about many aspects of the behavior of solutes in metallic materials. Metals of body-centered cubic lattice that contain heavy interstitial elements (oxygen, nitrogen and carbon) in solid solution, present anelastic relaxation peaks when submitted to cyclic tensions, due to process know stress-induced ordering. Internal friction and frequency as a function of temperature were performed between 300 K and 650 K in a polycrystalline sample of Nb, for three distinct conditions, using a torsion pendulum inverted Kê-type operating in a frequency oscillation between 1Hz and 10 Hz range, with a heating rate of 1 K/min and pressure lower than 2 x 10-5 mbar. The experimental spectra obtained for each condition of the sample, were decomposed by the successive subtraction method in elementary Debye peaks. The following metal-interstitial interactions were identified: Nb-O and Nb-N for all conditions of the sample. From the anelastic relaxation parameters obtained (relaxation strength, peak temperature, activation energy and relaxation time) and lattice parameter (obtained from x ray diffraction), the determination of the oxygen and nitrogen interstitial diffusion coefficient in Nb was possible, for each condition of the sample.

Impurity interstitial atoms present in metals with BCC structure can diffuse in the metallic matrix by jumps to energetically equivalent crystallographic sites. Anelastic spectroscopy (internal friction) is based on the measurement of mechanical loss or internal friction as a function of temperature. Due to its selective and nondestructive nature, anelastic spectroscopy is well suited for the study of diffusion of interstitial elements in metals. Internal friction measurements were made using the torsion pendulum technique with oscillation frequency of a few Hz, temperature interval from 300 to 700 K, heating rate of about 1 K/min, and vacuum better than 10-5 mbar. The polycrystalline Nb and Ta samples used were supplied by Aldrich Inc. The results obtained showed thermally activated relaxation structures due to stress-induced ordering of oxygen atoms around the Nb (or Ta) atoms of the metallic matrix. The results were interpreted by three methods and led to activation enthalpy values for the diffusion of oxygen in Nb and Ta of 1.15 eV and 1.10 eV, respectively.

Átomos de oxigênio, presentes em metais com estrutura cristalina cúbica de corpo centrado, são localizados preferencialmente em sítios octaedrais. Na ausência de uma tensão mecânica externa, estes átomos são distribuídos aleatoriamente. Na presença de oscilações mecânicas, a redistribuição dos átomos nos diferentes sítios deve ocorrer pela interação com esta tensão, levando a perdas na energia elástica. Este trabalho mostra o estudo da interação de átomos de oxigênio presentes em amostras da liga Nb-16% p. Ti, utilizando um pêndulo de torção. Os resultados mostram espectros bastante complexos, que foram decompostos em seus picos constituintes, representando os processos de relaxação devido à reorientação induzida por tensão de átomos e pares de átomos de oxigênio em torno de átomos de nióbio da matriz metálica e átomos de oxigênio em torno de átomos de titânio (interação substitucional-intersticial).

Measurements of internal friction as a function of temperature were performed in samples of Nb containing different amounts of substitutional (Zr) and interstitial (O, N) solutes. These data were resolved using the method of successive subtraction, into a series of constituent Debye peaks corresponding to different interactions. For each relaxation process we obtained the height (Q-1max) and temperature (Tp) of the peak, the activation energy (E) and the relaxation time (t0). The height, shape and temperature of the peaks depend on the concentration of interstitial and substitutional elements. With the addition of substitutional solute one can observed interactions between the two types of solutes (substitutional and interstitial), showing that the random distribution of the interstitial atoms was affected by presence of substitutional atoms. The peaks observed were associated with matrix-interstitial (Nb-O, Nb-N) and substitutional-interstitial (Zr-O) interaction processes.

The Gorsky Effect was investigated by internal friction measurements in the Nb-46 wt.% Ti-H system. The internal friction measurements were performed in a torsion pendulum with frequency of 3.8 Hz in a temperature range from 80 to 700 K. An interpretation of the experimental data showed that the hydrogen diffusion coefficient D obeys the Arrhenius' law in the temperature interval of 300 to 700 K, with D0 = 7.4 × 10-4 cm²/s and activation energy E = (0.102 ± 0.005) eV. At low temperatures, Do and E were found to be respectively 2.0 × 10-4 cm²/s and (0.063 ± 0.005) eV, with a deviation of the Arrhenius law of higher temperatures.