RESUMEN
This study is focused on the characterization and investigation of polyvinylidene fluoride (PVDF) nanofibers from the point of view of macro- and nanometer level. The fibers were produced using electrostatic spinning process in air. Two types of fibers were produced since the collector speed (300 rpm and 2000 rpm) differed as the only one processing parameter. Differences in fiber's properties were studied by scanning electron microscopy (SEM) with cross-sections observation utilizing focused ion beam (FIB). The phase composition was determined by Fourier-transform infrared spectroscopy (FTIR) and Raman spectroscopy. The crystallinity was determined by differential scanning calorimetry (DSC), and chemical analysis of fiber's surfaces and bonding states were studied using X-ray photoelectron spectroscopy (XPS). Other methods, such as atomic force microscopy (AFM) and piezoelectric force microscopy (PFM), were employed to describe morphology and piezoelectric response of single fiber, respectively. Moreover, the wetting behavior (hydrophobicity or hydrophilicity) was also studied. It was found that collector speed significantly affects fibers alignment and wettability (directionally ordered fibers produced at 2000 rpm almost super-hydrophobic in comparison with disordered fibers spun at 300 rpm with hydrophilic behavior) as properties at macrolevel. However, it was confirmed that these differences at the macrolevel are closely connected and originate from nanolevel attributes. The study of single individual fibers revealed some protrusions on the fiber's surface, and fibers spun at 300 rpm had a core-shell design, while fibers spun at 2000 rpm were hollow.
RESUMEN
The paper specifies the electrostatic spinning process of specific polymeric materials, such as polyvinylidene fluoride (PVDF), polyamide-6 (PA6, Nylon-6) and their combination PVDF/PA6. By combining nanofibers from two different materials during the spinning process, new structures with different mechanical, chemical, and physical properties can be created. The materials and their combinations were subjected to several measurements: scanning electron microscopy (SEM) to capture topography; contact angle of the liquid wettability on the sample surface to observe hydrophobicity and hydrophilicity; crystallization events were determined by differential scanning calorimetry (DSC); X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and Fourier-transform infrared spectroscopy (FT-IR) to describe properties and their changes at the chemical level. Furthermore, for the electrical properties of the sample, the dielectric characteristics and the piezoelectric coefficient were measured. The advantage of the addition of co-polymers was to control the properties of PVDF samples and understand the reasons for the changed functionality. The innovation point of this work is the complex analysis of PVDF modification caused by mixing with nylon PA6. Here we emphasize that the application of nylon during the spin influences the properties and structure (polarization, crystallization) of PVDF.
RESUMEN
The experimental study deals with the investigation of the effect of diverse crystallinity of imidazolium ionic-liquid-based SPE on conductivity and current fluctuations. The experimental study was carried out on samples consisting of [EMIM][TFSI] as ionic liquid, PVDF as a polymer matrix and NMP as a solvent. After the deposition, the particular sample was kept at an appropriate temperature for a specific time in order to achieve different crystalline forms of the polymer in the solvent, since the solvent evaporation rate controls crystallization. The ac/dc conductivities of SPEs were investigated across a range of temperatures using broadband dielectric spectroscopy in terms of electrical conductivity. In SPE samples of the higher solvent evaporation rate, the real parts of conductivity spectra exhibit a sharper transition during sample cooling and an increase of overall conductivity, which is implied by a growing fraction of the amorphous phase in the polymer matrix in which the ionic liquid is immobilized. The conductivity master curves illustrate that the changing of SPEs morphology is reflected in the low frequency regions governed by the electrode polarization effect. The dc conductivity of SPEs exhibits Vogel-Fulcher-Tammann temperature dependence and increases with the intensity of thermal treatment. Spectral densities of current fluctuations showed that flicker noise, thermal noise and shot noise seems to be major noise sources in all samples. The increase of electrolyte conductivity causes a decrease in bulk resistance and partially a decrease in charge transfer resistance, while also resulting in an increase in shot noise. However, the change of electrode material results in a more significant change of spectral density of current fluctuations than the modification of the preparation condition of the solid polymer electrolyte. Thus, the contact noise is considered to contribute to overall current fluctuations across the samples.
