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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.
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.
In light-processing systems, light energy is converted into a photocurrent due to the photoelectric effect. This project focuses on the development of a high-precision energy-to-voltage conversion technique to optimize signal processing in light-processing systems, specifically for applications in space analytics or solid state physikcs, such as Mössbauer spectroscopy. Analog circuit development plays a vital role as downstream voltage conversion is necessary for signal processing. The objective is to enhance the signal quality and improve the signal-to-noise ratio through the design, optimization, and comparison of various circuits for voltage conversion. The development process involves the design and optimization of amplifier circuits, supplemented with the incorporation of filters and/or regulators for further improvement. A transimpedance amplifier is approximated as a second-order low-pass filter, while a state controller is designed and analyzed to efficient transient oscillation of the system towards optimal amplitude values for subsequent signal processing. The project's results contribute to the advancement of light-processing systems, enabling more precise analysis of light energy in Mössbauer spectroscopy. The findings are presented in a series of scientific publications, showcasing the effectiveness of the developed circuits and their impact on signal quality. Future work could focus on further optimization and validation of the circuits in real-world applications to confirm their performance and reliability. Overall, this project emphasizes the significance of meticulous circuit development and optimization for enhancing signal processing in light-processing systems, thus supporting their application in space analytics.
The miniaturized Mössbauer-spectrometer (MIMOS II), originally devised by Göstar Klingelhöfer, is further developed by the Renz group at the Leibniz University Hanover in cooperation with the Hanover University of Applied Sciences and Arts. A new processing unit with a two-dimensional (2D) data acquisition was developed by M. Jahns. The advantage of this data acquisition is that no thresholds need to be set before the measurement. The energy of each photon is determined and stored with the velocity of the drive. After the measurement, the relevant area can be selected for the Mössbauer spectrum. Now we have expanded the evaluation unit with a power supply for a MIMOS drive and a MIMOS PIN detector. So we have a very compact MIMOS transmissions measurement setup. With this setup it is possible to process the signals of two detectors serially. Currently we are working on a parallel signal processing.
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.
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.
Das Institut für Sensorik und Automation (ISA) stellt in acht Beiträgen aktuelle Ergebnisse aus seinen vielfältigen Forschungsprojekten vor. Es werden Themen angesprochen wie Lichttechnik in der Nutzgeflügelhaltung, Datenaustausch in der Produktion, hochfrequente Front-Ends für Umweltsensoren in der Gebäudeautomatisierung, Mössbauer-Spektroskopie, Entwicklung fortschrittlicher Transimpedanzverstärker, Optimierung monostatischer Transceiver, Datenverarbeitungsszenarien für Smart-Home-Systeme und Designüberlegungen für kryogene Analog-Digital-Wandler.
The phenomenon which is called spin crossover is known to occur in some coordination compounds with an octahedral ligand field and electron configurations from 3d4 to 3d7. Thereby, a reversible transition between spin states (high spin and low spin state) is possible, through several external stimuli. Iron(II) triazole complexes exhibit this phenomenon at a wide range of temperatures depending on the ligands and anions used. For this reason, they are often considered for several possible practical applications. It is also possible to combine ligands or anions to modify the transition temperature. The latter of which was rarely discussed in the past. In this study we synthesized a series of iron(II)‐4‐Aminotriazole complexes, with different ratios of chloride‐ and tetrafluoroborate‐anions, of the formula [Fe(Atrz)3]Cl2−X(BF4)X. We show that the combination of these anions leads to transition temperatures between those of their corresponding pure anion complexes. We furthermore present that a simple modification of the synthesis leads to a possible easy way of fine‐tuning transitions temperatures.