Abstract Composites are relevant to high-performance materials in the aerospace sector and have attracted the attention of the scientific and technological communities. Bentonites present very fine granulometry which enables their use in composites. This study showed the development of water absorbent composite based on sodium polyacrylate, bentonite coated by epoxy resin. Since there are gaps in the quantification of composite materials by near-infrared spectroscopy, especially by reflectance analysis (NIRA), this paper shows a quantification methodology (A7200/A5202) of sodium polyacrylate and bentonite. The methodology error found was 1.45% (95% of coefficient of determination). The effectiveness of the developed infrared methodology was verified showing that values are close to the nominal, especially for lower bentonite content. Besides, scanning electron microscopy (SEM) and universal attenuated total reflection (UATR) analysis evidenced the coating with the epoxy resin. Such development ensures rapid and precise methodologies that can be applied to the quality control of composite materials.

Abstract A variety of fiber-reinforced polymer (FRP) has been described in literature, with a considerable subset of studies focused on fiber surface treatment (sizing), performance enhancement of matrix and fibers both synthetic and natural, and development of more ecologically sustainable composites. The present review discusses the different types of fibers and matrices and their applications, depending on the chemical and mechanical properties of their composites. In order to evaluate the performance of FRP composites and explore the characteristics of the involved materials, some analytical techniques are considered paramount, such as thermal analysis, microscopy, Fourier transform-infrared spectroscopy (FT-IR), and others. On this basis, this review addresses the state-of-the-art of material characterization methodologies, provides a comprehensive overview of different types of FRP found in literature, as well as links the analytical techniques with the main applications contributing to future studies and research in this area.

ABSTRACT Ethylene propylene diene monomer rubber is used as flexible thermal protection for rocket engines, as well as in blends with polychloroprene, which can be applied in the aeronautical sector, and with great potential in the defense sector. However, there is not a considerable number of studies considering both polymers as a blend. In general, elastomer content quantification in blends is done by more complex instrumental methods. When performed by Fourier transform-infrared spectroscopy, the conventional transmission mode is used, usually without including the developed methodology error. Therefore, the Fourier transform infrared spectroscopy (FT-IR) methodology is proposed using the universal attenuated total reflection mode, with sample treatment (pyrolysis) to determine polychloroprene content in the mixture with ethylene propylene diene monomer. In accordance with the infrared spectrometer precision limits and rubber blends studies data found in the literature, the methodology error analysis shows a value close to 2%. In addition, it has the advantage of being a less complex methodology. This actual study uses a simple FT-IR analytical tool, scarce, especially for the rubber research community, to determine the content of rubber minor phase within the major phase. It is valuable in weapons reverse engineering, aiming at the knowledge of new thermal protections.

ABSTRACT Ethylene-propylene-diene elastomer (EPDM) is employed as thermal insulation for rocket motors, as well as EPDM blends with ethylene vinyl acetate (EVA) have been used in the aerospace industry. The quantification of these blends is more common using Fourier Transform Infrared Spectrometry (FT-IR) by transmission mode, but without discussing sample preparation and methodology error. Considering this fact, a methodology was developed for determining EVA content in binary blend with EPDM samples, by Universal Attenuated Total Reflection (UATR) technique, associated to thermogravimetric analysis (TGA). This last one, it was applied to determine Vinyl Acetate (VA) content in EVA and to identify differences between EPDM/EVA blends. Samples of the analyzed blends showed two VA contents and five proportions of EPDM/EVA: 90/10, 70/30, 50/50, 30/70, and 10/90. The carbonyl stretching vibration band C=O at 1740 cm-1 was used as analytical band in FT-IR quantification. Finally, the results presented excellent accuracy with a good linear correlation coefficient (R > 0.940) and with relative error values lower than 2%, respecting the precision limits of the FT-IR spectrometer.

ABSTRACT When some materials need to be characterized, the hydroxyl number (IOH) determination is especially useful, mainly for those applied in the aerospace field. Usually, this characterization is performed by wet chemistry, using methodologies involving several steps, such as derivatization. This is a time-consuming and costly step. On the other hand, when the analysis is performed by Fourier transform infrared (FT-IR) spectroscopy, the most used region is the medium infrared (MIR) and transmission techniques are usually employed. However, FT-IR methodology developed error is usually not discussed. FT-IR methodology was developed in near infrared (NIR) and MIR regions, including non-conventional techniques, such as universal attenuated total reflection (UATR) and transflectance (near infrared reflection accessory [NIRA]), and transmission, to determine IOH in surfactants, used in aerospace catalysts/cosmetic products, and polyesters, applied in paints. According to the samples’ characteristics, surfactants were analyzed by transmission/solution and, as received, by NIRA. Polyesters were analyzed by UATR and NIRA, as received. The IOH values for all samples were also measured by wet chemistry and/or potentiometry (supplier’s data) and used as reference. Good linear correlations were observed between 0.939 and 0.976, being considered with good precision, and between 88% (NIRA) and 98% (MIR) of the results were explained by developed methodologies.

Abstract Rubber blends are important materials in automotive industry, as well as in other sectors. However, there are implications when suitable use of a polymer in an artifact is not made. In the automotive area, for example, the use of an elastomer without the fuel resistance requirement would result in component degradation, potential fuel leakage, and danger of fire. The use of polymer blends may be the solution to this problem. Fourier transform infrared spectroscopy (FT-IR) can be used for the knowledge of the polymer content of these blends. Then, FT-IR quantitative methodologies for determining acrylonitrile-butadiene copolymer (NBR) copolymer and butadiene-styrene copolymer (SBR) contents were developed by the transflectance accessory, NIRA, and the transmission mode, being the sample analyzed by transmission and universal attenuated total reflection (UATR) in the medium infrared (MIR). UATR and NIRA methodologies showed better accuracy. However, the MIR analysis showed a detection limit between 10-20% of NBR.

Abstract The bicomponent fibers are a special class of fibers that consolidate two polymers in only one fiber in order to explore individual properties of each polymer and can be designed in a spatial configuration that allows the enhancement in application of this material. Thereby, an appropriate characterization of bicomponent fibers is very valuable to process monitoring, quality control and forensic investigation. The sheath-core bicomponent fiber composed by polyethylene (PE), polypropylene (PP) and titanium dioxide (TiO2) was analyzed by Fourier transform infrared (FT-IR) spectroscopy and other analytical methodologies. Results obtained by FT-IR using modern accessories showed efficiency to characterize the polymers of sheath (PE) and core (PP), moreover these polymers were confirmed by DSC (Differential Scanning Calorimetry). The morphology and elemental composition were also studied by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDS). The thermogravimetric analysis (TGA) and colorimetric analysis allowed characterize and quantify the concentration of TiO2.

Abstract The paint industry requires rapid and accurate methodologies of raw materials qualitiy controls. For example, the evaluation of the suitable ratio of binary mixtures of polymer/plasticizer such as nitrocellulose (NC)/acetyl tributyl citrate (ATBC) must be done, since this ratio is directly related to the performance of the final product. However, there is a small number of quantitative methodologies of such control in the literature. In this context, in this paper, the applicability of Infrared Fourier Transform Spectroscopy (FT-IR) techniques by using universal total attenuated reflection (UATR), in the middle infrared (MIR), and the reflectance analysis in the near infrared region (NIRA) is evaluated for the quantification of plasticizer ATBC in mixtures with NC. MIR and NIR methodologies presented good results such as: practicality of not requiring refined sample preparation, analysis time about 30 min and good accuracy, suitable data for using in the quality control laboratories of paint industry.

Abstract It is a well-established fact that rubber accelerator is essential to provide solution in different sectors. However, there is a reversal process which can reduce the material performance. Sulfur accelerators donors and organic peroxides have been presented as a solution to the problem. The methodology development that can separate or characterize those components is a challenge and still allows gaps, explained by the application of conventional technique to reach this goal. This study aimed at contributing to the use of off-line coupling of thin layer chromatography (TLC)/infrared spectroscopy (IR) by Universal Attenuated Total Reflection (UATR) for analysis of N-cyclohexyl-2-benzotiazolsulfenamide (CBS), tetraethylthiuram disulfide (TMTD) and dicumyl peroxide (DCP), in natural poly-cis-isoprene (NR) formulations, containing naphthenic oil. The best results were obtained for the plasticizer and DCP, in formulations that had a greater proportion of these compounds. The separation of CBS and TMTD was made with less effectiveness, due to bands overlapping.

Thermal protection systems (TPS) are components designed to protect the internal and external areas of a rocket motor from high temperatures. There has been studies in Brazil of resin-based polybutadiene hydroxylated (HTPB) loaded with asbestos since the 1970s. Nevertheless, asbestos has been banned in several countries because it is severely harmful to the human health. In this context, the development of asbestos free in flexible thermal protection (FTP) is extremely important. This study evaluates the use of Expanded Perlite (PExp) as an asbestos substitute. Lower densities were observed, which become a very interesting achievement for the aerospace field. Samples with 5 phr of Expanded Perlite showed similar results when comparing with 47 phr of fillers in PTF reference on oxy-acetylene torch test, and a reduction about 20 % of mass loss rate in test with solid propellant, thus showing that Expanded Perlite can replace asbestos in FTP.

Abstract Epoxy resins (EP) usually cure in autoclave to minimize resin voids and to achieve the desired resin/fiber ratio. Cure parameters such as temperature, vacuum and pressure levels are controlled and monitored. Aiming time and cost optimization, new out-of-autoclave (OOA) cure processes have been developed lately. This study evaluated the cure cycle and the effect of non-programmed interruptions in an OOA process. Fourier Transform Infrared spectroscopy (FT-IR) results show similarities between the resin used and diglycidyl ether of bisphenol A (DGEBA) and also that the curing system is composed of cyan and sulfur hardeners, codified in industry, as Components of #2511 Resin System. The cure cycle and its interruptions were simulated by dynamic-mechanical analysis (DMA). The samples obtained were evaluated by FT-IR and differential scanning calorimetry (DSC), whose results show that the degree of cure varying between 0.8 to 0.85 was achieved at 120 °C.

ABSTRACT: The development of polyaniline and graphene oxide composites aims to join the unique properties of each material for aerospace applications. The present paper demonstrates an easy and quick method, compared to the ones found in the literature, to obtain a composite made with polyaniline doped with dodecylbenzenesulfonic acid, a combination commonly called polyaniline, and graphene oxide. Nowadays, the most common studied methods are electrochemistry and in situ chemical polymerization. Differently from these methods, the films were obtained by a physical mixture of equimolar suspension of graphene oxide (4 mg/mL) with 3 concentrations of polyaniline powder: 25; 50 and 75%, being compared to pure graphene oxide and polyaniline. The morphology and structure behavior of all the films were studied, besides the bonding nature between both materials. The films were analyzed by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and differential scanning calorimetry. The apparent interaction between graphene oxide corrugated sheets and polyaniline grains was verified by scanning electron microscopy images. It can be noticed, as the concentration of polyaniline increases, that more polymer was entrapped. To prove the formation of polyaniline/graphene oxide composite, X-ray diffraction and Fourier transform infrared spectroscopy techniques demonstrated the changes on graphene oxide crystallographic plans and on the chemical bonding between polyaniline and graphene oxide, suggesting an interaction between polyaniline and graphene oxide, especially in the composite with 50% polyaniline/50% graphene oxide. Differential scanning calorimetry was used to highlight this effect through the increase in thermal stability. The method of physical mixture was efficient to obtain the polyaniline/ graphene oxide composites.

Abstract The knowledge of the components that constitutes a rubber composition is important to justify the properties of the final device, particularly when it comes to elastomeric compositions used in the aerospace industry. The development of methodologies that can detect components, specially the smallest proportion of the rubbers composition is a constant challenge and an important gap in the studies of this nature. Therefore, methodologies by using standard techniques and/or of last generation are important in rubber industry and research laboratories, aiming application in related research. In this context, this study shows the coupling/association techniques (off-line) of thin layer chromatography and infrared spectroscopy (TLC/IR), being the IR spectra obtained by universal attenuated total reflection (UATR), applied to the analysis of additives in rubber compositions of ethylene-propylene-diene rubber (EPDM). Two EPDM compositions, a kind of eluent system and Gibbs' reagent, as developer, were used. Basically, all organic components were detected by this methodology, being possible to suggest that it can be applied for detecting additives of similar chemical structures, even though it's presents in small amounts in the composition.

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.