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Electrospun polymer fiber mats feature versatile applications in tissue engineering, drug delivery, water treatment and chemical processes. The orientation of fibers within these mats is a crucial factor that significantly influences their properties and performance. However, the analysis of fiber samples using scanning electron microscopy (SEM) has limitations such as time consumption, fixed assembly, and restricted field of vision. Therefore, a fast and reliable method for qualitative measurements of fiber orientation is required. Mueller matrix polarimetry, a well-established method for measuring orientation of chemical and biological species, was employed in this case. We investigated the effect of four important parameters of the electrospinning process, namely collector speed, applied voltage, needle-to-collector distance, and solution concentration, on fiber orientation using Mueller matrix polarimetry thus extending the range of parameters analyzed. Measurements were performed using two extreme values and a central optimized value for each fabrication parameter. Changes in matrix values were observed for each fabrication parameter, and their correlation with fiber orientation was analyzed based on the Lu-Chipman decomposition. The results were compared with SEM images, which served as the ground truth, and showed overall good agreement. In the future, the analysis of electrospun polymer fibers can be done by using Mueller matrix polarimetry as alternative to current technology and fabrication parameters, including solution concentration for the first time in this context and the production can quickly be adjusted based on the outcome of the measurements
Pressing of Functionalized Polymer Composite Materials to Improve Mössbauer Measurement Signals
(2024)
Coordination compounds, like iron(II) triazole complexes, exhibit spin crossover (SCO) behavior at around room temperature. Therefore, they are interesting for a variety of possible applications, and it is convenient to integrate them into polymers. Due to a reduction of the iron content and thus also 57Fe content in the sample through integration in polymers, Mössbauer measurements are only possible with greater difficulty or very long measurement times without expensive enrichment of the samples with 57Fe. So, other ways of improving the Mössbauer signal for these composite materials are necessary. Therefore, we pressed these composite materials to improve the Mössbauer spectra. In this study, we synthesized an iron(II) triazole spin crossover complex and an electrospun polymer complex composite nanofiber material including the same complex. For both products, Mössbauer measurements were performed at room temperature before and after using a press to show that the complex composite is not harmed through pressing. We investigate the influence of the pressing impact on the Mössbauer measurements in the context of measurement statistics and the measured signals. We show that pressing is not connected to any changes in the sample regarding the spin and oxidation state. We present that pressing improves the statistics of the Mössbauer measurements significantly. Furthermore, we use SEM measurements and PXRD to investigate whether or not the obtained fiber mats are destroyed in the pressing process.
Incorporation and Deposition of Spin Crossover Materials into and onto Electrospun Nanofibers
(2023)
We synthesized iron(II)-triazole spin crossover compounds of the type [Fe(atrz)3]X2 and incorporated and deposited them on electrospun polymer nanofibers. For this, we used two separate electrospinning methods with the goal of obtaining polymer complex composites with intact switching properties. In view of possible applications, we chose iron(II)-triazole-complexes that are known to exhibit spin crossover close to ambient temperature. Therefore, we used the complexes [Fe(atrz)3]Cl2 and [Fe(atrz)3](2ns)2 (2ns = 2-Naphthalenesulfonate) and deposited those on fibers of polymethylmethacrylate (PMMA) and incorporated them into core–shell-like PMMA fiber structures. These core–shell structures showed to be inert to outer environmental influences, such as droplets of water, which we purposely cast on the fiber structure, and it did not rinse away the used complex. We analyzed both the complexes and the composites with IR-, UV/Vis, Mössbauer spectroscopy, SQUID magnetometry, as well as SEM and EDX imaging. The analysis via UV/Vis spectroscopy, Mössbauer spectroscopy, and temperature-dependent magnetic measurements with the SQUID magnetometer showed that the spin crossover properties were maintained and were not changed after the electrospinning processes.
Compounds that exhibit the spin crossover effect are known to show a change of spin states through external stimuli. This reversible switching of spin states is accompanied by a change of the properties of the compound. Complexes, like iron (II)-triazole complexes, that exhibit this behavior at ambient temperature are often discussed for potential applications. In previous studies we synthesized iron (II)-triazole complexes and implemented them into electrospun nanofibers. We used Mössbauer spectroscopy in first studies to prove a successful implementation with maintaining spin crossover properties. Further studies from us showed that it is possible to use different electrospinning methods to either do a implementation or a deposition of the synthesized solid SCO material into or onto the polymer nanofibers. We now used a solvent in which both, the used iron (II)-triazole complex [Fe(atrz)3](2 ns)2 and three different polymers (Polyacrylonitrile, Polymethylmethacrylate and Polyvinylpyrrolidone), are soluble. This shall lead to a higher homogeneous distribution of the complex along the nanofibers. Mössbauer spectroscopy and other measurements are therefore in use to show a successful implementation without any significant changes to the complex.
Complexes like iron (II)-triazoles exhibit spin crossover behavior at ambient temperature and are often considered for possible application. In previous studies, we implemented complexes of this type into polymer nanofibers and first polymer-based optical waveguide sensor systems. In our current study, we synthesized complexes of this type, implemented them into polymers and obtained composites through drop casting and doctor blading. We present that a certain combination of polymer and complex can lead to composites with high potential for optical devices. For this purpose, we used two different complexes [Fe(atrz)3](2 ns)2 and [Fe(atrz)3]Cl1.5(BF4)0.5 with different polymers for each composite. We show through transmission measurements and UV/VIS spectroscopy that the optical properties of these composite materials can reversibly change due to the spin crossover effect.
