The effect of clay dispersion on the crystallization behavior of isotactic polypropylene (iPP)-based nanocomposites is reported. The
Tm
0 of the materials was calculated by the method proposed by Marand, the kinetics of crystallization was evaluated by the Avrami
analysis and also the Hoffman-Lauritzen theory of crystallization regimes was applied. Montmorillonite was found to depressTm
0, to
enhance the rate of crystallization and to ease the chain folding of macromolecules. These effects were magnified if clay was exfoliated,
rather than intercalated
Biodegradable polycaprolactone/organoclay nanocomposites were prepared by solvent casting, using different amounts of filler and matrices differing by average molecular weight. Intercalated nanocomposites were obtained. The nanocomposites were characterized by wide-angle X-ray diffraction (WAXD) and small-angle Xray scattering (SAXS) methods. Negligible variations in the degree of crystallinity were detected by WAXD. The thickness of crystalline lamellae, measured by SAXS, increased in low molecular weight polymer nanocomposites with increasing clay amount; this effect was weakened in matrices with high molecular weight. Differential scanning calorimetry showed an inhibiting effect of clay on crystallization. The composites' ductility was largely increased, whereas stiffness was retained. After biodegradation in compost, in all samples, the degree of crystallinity was increased, meaning that the less ordered portion of the sample was preferentially degraded. Clay slowed down the biodegradation rate, coherently with the observed increase in the lamellar thickness due to the filler. This may offer a strategy for tuning the biodegradability by calibrating their semicrystalline framework. POLYM. ENG.
In this work, an easy, quick and reproducible wet-synthesis coprecipitation route starting from oxalate precursors was optimised to synthesise cobalt, nickel, zinc and magnesium spinel ferrites CoFe2O4, NiFe2O4, ZnFe2O4 and MgFe2O4, as well as the manganese perovskite ferrite MnFeO3. Crystalline purity and crystallite sizes ranging from 30 to 190 nm were investigated by means of powder X-ray diffraction, and uniform morphology of the particles was shown through transmission electron microscopy. The chosen synthetic route afforded an excellent stoichiometric control over the products, as confirmed by combined X-ray photoelectron spectroscopy and inductively coupled plasma atomic emission spectroscopy analyses. The site geometry, degree of inversion in the spinels and chemical environments in the ferrites were explored by Mössbauer spectroscopy. The thermal evolution of the compounds during calcination and the decomposition pattern of the oxalates were studied through differential scanning calorimetry coupled with thermogravimetric analysis as well as in situ temperature-programmed X-ray diffraction. Magnetic properties of these oxides, as well as the transition of the perovskite from paramagnetic to ferrimagnetic behaviour at low temperatures, were investigated by superconducting quantum interferometer magnetometr
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