Novel cross-linked chitosan-based films were prepared using the solution casting technique. A naturally occurring and nontoxic cross-linking agent, genipin, was used to form the chitosan and chitosan/poly(ethylene oxide) (PEO) blend networks, where two types of PEO were used, one with a molecular weight of 20 000 g/mol (HPEO) and the other of 600 g/mol (LPEO). Genipin is used in traditional Chinese medicine and extracted from gardenia fruit. Importantly, it overcomes the problem of physiological toxicity inherent in the use of some common synthetic chemicals as cross-linking agents. The mechanical properties and the stability in water of cross-linked and un-crosslinked chitosan and chitosan/PEO blend films were investigated. It was shown that, compared to the transparent yellow, un-cross-linked chitosan/PEO blend films, the genipin-cross-linked chitosan-based film, blue in color, was more elastic, was more stable, and had better mechanical properties. Genipin-cross-linking produced chitosan networks that were insoluble in acidic and alkaline solutions but were able to swell in these aqueous media. The swelling characteristics of the films exhibit sensitivity to the environmental pH and temperature. The surface properties of the films were also examined by contact angle measurements using water and mixtures of water/ethanol. The results showed that, with the one exception of cross-linked pure chitosan in 100% water, the cross-linked chitosan and chitosan/PEO blends were more hydrophobic than un-crosslinked ones.

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We describe a novel thermal characterization technique based on a differential arrangement, which achieves spatially localized calorimetric analysis. It involves the use of an active probe which acts both as a highly localized heat source and a thermometer. This ability opens the way for the implementation of scanning calorimetric microscopy where image contrast will be created from thermal analysis data. For a number of polymers we have recorded events such as glass transitions, meltings, recrystallizations and thermal decomposition within volumes of material estimated at a few μm3. The data obtained are compared with those obtained from conventional calorimetry and the events registered in both cases are found to match. For a full quantitative analysis of the results obtained, mathematical modelling of the operation of the technique, taking account of physical and other changes in materials, is required.

Scanning probe thermal microscopy has been used to achieve sub-surface imaging of metallic particles embedded in a polymer matrix, using a probe which can act as both ohmic heater and thermometer. A lateral resolution of the order of a micron and a depth detection of a few microns were achieved. Together with the description of the technique and the experimental results obtained, a basic theoretical framework is presented which describes heat flow and temperature distributions within a sample consisting of inclusions buried within a bulk material. Computer models have been developed to give theoretical heat flows and temperature profiles: these are compared here with the experimental data. The theoretical lateral resolution was found to be in good agreement with the experimental observation. We show that theoretical modelling can be used to calibrate the instrument for specific investigations. For example, the technique could be used quantitatively to determine and map thermal conductivity variations across heterogeneous samples, or to determine the depth at which inclusions are located in the case where the thermal conductivities of both the inclusions and the enclosing material are known as well as the geometry of the inclusions.

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ABSTRACT:Coir fiber native to the Brazilian northeast coast has been characterized by mechanical, thermal, and microscopy techniques. The tensile strength, initial modulus, and elongation at break were evaluated for untreated and alkaline-treated fibers. The results showed an enhancement of mechanical properties after 48-h soaking in 5 wt % NaOH. The thermal stability slightly decreased after this alkaline treatment. A thermal event was observed between 28 and 38°C. The heat capacity, C p , as a function of temperature curves between Ϫ70 and 150°C, were obtained for the untreated and alkaline-treated coir fibers. The morphologies of the coir-fiber surfaces and cross sections were observed by scanning electron microscopy. The properties and the morphologies were discussed, comparing the native Brazilian coir fiber with the more extensively studied native Indian coir fiber.