ABSTRACT Fourier transform infrared spectroscopy techniques, associated or not to others, are a well-studied subject used for characterizing polymers/energetic materials that have been employed mainly in aerospace industries. However, the infrared analyses are usually qualitative and performed using the mid-infrared. This paper discusses the Fourier transform infrared spectroscopy qualitative and quantitative methodologies, coupled or not with thin layer chromatography and thermogravimetric analysis, for characterization of aerospace polymer systems, in some cases, using mid-infrared, near-infrared and far-infrared regions, by traditional accessories and the latest generation spectra mode, universal attenuated total reflection. This short review was made based on methodologies developed during the last two decades and published by many scientific and industrial research groups, emphasizing studies usually carried out in the last five years. A critical assessment and future trends were included.

ABSTRACT Carbon fibers have been widely used as structural reinforcement in aeronautical composites, because of their exceptional mechanical properties. However, carbon fibers present few polar groups on their surfaces inducing a weak interaction with some thermosetting and thermoplastic matrices. Surface treatments, such as thermal and electrochemical oxidation, are generally followed by sizing in order to improve interfacial adhesion between carbon fibers and some matrices. The precise surface characterization, by means of its chemical groups and radical identification, has been pointed out as an effective tool of carbon fibers finishing assessment process. Goniometry and Fourier transforminfrared spectroscopy are widely used to characterize some materials applied in industry, but not for carbon fibers, mainly because of their filamentary shape and the high concentration of carbon even in their near surface. In this paper, unsized and sized Torayca T300 carbon fibers were characterized by goniometry tests to evaluate hydrophilic or hydrophobic character. Qualitatively, it was noticed the effect of sizing on carbon fibers by their hydrophilic behavior, which has not been observed in unsized samples. Chemical analysis was performed by Fourier transform-infrared spectroscopy using different setups: photoacoustic, attenuated total reflectance and universal attenuated total reflectance. The Fourier transform-infrared spectroscopy/attenuated total reflectance/Germanium was shown to be the most promising technique to analyze carbon fibers surface, despite the low level of relative intensities of some bands. By this technique, it was possible to observe differences between unsized and sized carbon fibers spectra.

Técnicas FT-IR (UATR, PAS e MIC, com objetiva ATR) foram escolhidas para a caracterização da superfície da borracha de EPDM vulcanizada, após tratamento em plasma de Ar/O2 e N2/H2/Ar gerado em micro-ondas. Após tratamento, grupos oxigenados foram detectados por UATR e MIC/FT-IR, com objetiva ATR para as duas misturas gasosas, e possíveis grupos nitrogenados foram inseridos na superfície das amostras tratadas com plasma de N2/H2/Ar. A análise MIC/FT-IR sugeriu a formação de grupos em uma camada mais externa, para as amostras tratadas com plasma de N2/H2/Ar, sendo possível observar a redução na intensidade das bandas da absorção do CH2 e CH3, o que pode estar relacionado ao fato de o nitrogênio ser um gás menos permeável que o oxigênio. Diferentes velocidades, 0,05 cm.s-1 e 0,2 cm.s-1, foram utilizadas na análise PAS para avaliar a superfície após tratamento, e apenas para a velocidade 0,05 cm.s-1 com plasma de Ar/O2 alterações espectroscópicas foram detectadas. A redução na medida de ângulo de contato e o aumento na resistência ao descascamento da colagem indicaram melhoras nas propriedades adesivas da superfície. Falhas de adesão foram observadas entre a interface do filme de adesivo de PU e da borracha de EPDM, e confirmados por UATR/FT-IR.

The FT-IR techniques UATR, PAS and MIC with ATR objective were chosen to characterize the surface of EPDM rubber vulcanized after treatment in Ar/O2 or N2/H2/Ar plasma generated in a microwave oven. After treatment, oxygenated groups were detected by UATR and MIC-FT-IR, with ATR objective for the two gas mixtures, and possible nitrogenous groups were inserted on the surface after the plasma treatment with N2/H2/Ar. The MIC/FT-IR analysis suggested that groups were formed on an outermost layer, inferred from a reduced intensity of the CH2 and CH3 absorption bands for the treatment in N2/H2/Ar plasma, probably because nitrogen is less permeable than oxygen. Different speeds with PAS analyses (0.05 cm.s-1 and 0.2 cm.s-1) were used to evaluate the surface after treatment. Only for the speed 0.05 cm.s-1 in Ar/O2 plasma were spectroscopic changes detected. The decrease in the contact angle and the increased resistance to peel indicated improvements in the bonding adhesive properties of the surface. Bonding failure was observed between the adhesive PU film and the EPDM rubber, which was confirmed by UATR/FT-IR.

ABSTRACT: The surface of vulcanized ethylene propylene diene terpolymers (EPDM) was modified by Ar and N2, microwave generated plasma in order to improve adhesion properties. Surface modification was characterized by universal attenuated total reflectance Fourier Transform Infrared (UATR/FT-IR), because it presented lower interference of ingredients of EPDM formulation when compared with other techniques used for the attenuated total reflectance (ATR) to different crystals (ATR/KRS-5 and ATR/Ge). Oxygenated groups were introduced on the surface after treatments which were formed when the activated surface was exposed to the plasma gas. In treatments with nitrogen, oxygen groups and probable nitrogen groups were formed on the surface and could be identified by FT-IR. Reduction in the measurement of the contact angle and an increase in the work of adhesion and in the peel strength (EPDM X Polyurethane (PU)) were observed after the treatment resulted in the improvement of the adhesion properties of the modified surface.