TY - JOUR A1 - Flegler, Andreas A1 - Schneider, Michael A1 - Prieschl, Johannes A1 - Stevens, Ralph A1 - Vinnay, Thomas A1 - Mandel, Karl T1 - Continuous flow synthesis and cleaning of nano layered double hydroxides and the potential of the route to adjust round or platelet nanoparticle morphology JF - RSC Advances N2 - Here, we report a continuous flow synthesis of nano LDH, comprising a continuous precipitation process using static mixers and followed by an immediate cleaning process via a semi-continuous centrifuge to obtain the final product in one-go. Via this synthesis setup, it is possible to independently vary the concentrations of the reactants during precipitation and at the same time ensure constant reaction conditions and an immediate "quenching" of the precipitate due to "on the flow"-washing. We found that this paves the way to adjust the synthesis parameters in a way that the final morphology of the nano-LDH particles can be controlled to be either round or platelet-like. KW - MgAl LDH KW - nano LDH KW - static mixer KW - synthesis process Y1 - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-191305 VL - 6 IS - 62 ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Zukrowski, Jan A1 - Przybylski, Marek A1 - Sikora, Marcin A1 - Safonova, Olga A1 - Shmeliov, Aleksey A1 - Nicolosi, Valeria A1 - Schneider, Michael A1 - Granath, Tim A1 - Oppmann, Maximilian A1 - Straßer, Marion A1 - Mandel, Karl T1 - Pushing up the magnetisation values for iron oxide nanoparticles via zinc doping: X-ray studies on the particle's sub-nano structure of different synthesis routes JF - Physical Chemistry Chemical Physics N2 - The maximum magnetisation (saturation magnetisation) obtainable for iron oxide nanoparticles can be increased by doping the nanocrystals with non-magnetic elements such as zinc. Herein, we closely study how only slightly different synthesis approaches towards such doped nanoparticles strongly influence the resulting sub-nano/atomic structure. We compare two co-precipitation approaches, where we only vary the base (NaOH versus NH\(_3\)), and a thermal decomposition route. These methods are the most commonly applied ones for synthesising doped iron oxide nanoparticles. The measurable magnetisation change upon zinc doping is about the same for all systems. However, the sub-nano structure, which we studied with Mossbauer and X-ray absorption near edge spectroscopy, differs tremendously. We found evidence that a much more complex picture has to be drawn regarding what happens upon Zn doping compared to what textbooks tell us about the mechanism. Our work demonstrates that it is crucial to study the obtained structures very precisely when "playing'' with the atomic order in iron oxide nanocrystals. KW - Ferrite KW - FE Y1 - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-187390 VL - 18 IS - 36 ER - TY - THES A1 - Mandel, Karl T1 - Synthesis and Characterisation of Superparamagnetic Nanocomposite Particles for Water Purification and Resources Recovery T1 - Synthese und Charakterisierung von superparamagnetischen Nanokompositpartikeln zur Wasserreinigung und Wertstoffrückgewinnung N2 - Superparamagnetic nanocomposite microparticles, compromised of magnetite nanoparticles in a silica matrix, have been synthesised and surface-modified to act as adsorbers for substances (e.g. toxic heavy metals or valuable resources) dissolved in fluids like water. The particles can be used for a magnetic-extraction-assisted separation process of these target substances which thereby can be recovered from the fluid. N2 - In der vorliegenden Arbeit wurden superparamagnetische Nanokomposit-Mikropartikel, bestehend aus Magnetitnanopartikeln in einer Silica-Matrix, hergestellt. Die Oberfläche der Partikel wurde modifiziert, so dass die Partikel als Adsorber für gelöste Substanzen (z.B. giftige Schwermetalle oder Wertstoffe) in Fluiden wie z.B. Wasser eingesetzt werden können. Mit Hilfe der Partikel kann eine Abtrennung und damit Rückgewinnung der Zielstoffe auf Basis eines Magnetseparationsprozesses durchgeführt werden. KW - Magnetisches Trennverfahren KW - Superparamagnetismus KW - Recycling KW - Wasserreinigung KW - Eisenoxide KW - Siliciumdioxid KW - Superparamagnetismus KW - Nano KW - Wertstoffrückgewinnung KW - Magnetseparation KW - superparamagnetism KW - nano KW - water purification KW - resources recovery KW - magnetic separation KW - Nanotechnologie KW - Synthese KW - Magnetismus Y1 - 2013 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-81208 ER - TY - JOUR A1 - Sanchez-Naya, Roberto A1 - Stepanenko, Vladimir A1 - Mandel, Karl A1 - Beuerle, Florian T1 - Modulation of Crystallinity and Optical Properties in Composite Materials Combining Iron Oxide Nanoparticles and Dye-Containing Covalent Organic Frameworks JF - Organic Materials N2 - Two series of organic–inorganic composite materials were synthesized through solvothermal imine condensation between diketopyrrolopyrrole dialdehyde DPP-1 and 5,10,15,20-tetrakis(4-aminophenyl)porphyrin (TAPP) in the presence of varying amounts of either amino- or carboxy-functionalized superparamagnetic iron oxide nanoparticles (FeO). Whereas high FeO loading induced cross-linking of the inorganic nanoparticles by amorphous imine polymers, a lower FeO content resulted in the formation of crystalline covalent organic framework domains. All hybrid materials were analyzed by magnetization measurements, powder X-ray diffraction, electron microscopy, IR, and UV/Vis absorption spectroscopy. Crystallinity, chromophore stacking, and visible absorption features are directly correlated to the mass fraction of the components, thus allowing for a fine-tuning of materials properties. KW - covalent organic frameworks KW - diketopyrrolopyrroles KW - porphyrins KW - iron oxide nanoparticles KW - hybrid materials KW - superparamagnetism Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-231480 VL - 3 ER - TY - JOUR A1 - Wintzheimer, Susanne A1 - Oppmann, Maximilian A1 - Dold, Martin A1 - Pannek, Carolin A1 - Bauersfeld, Marie‐Luise A1 - Henfling, Michael A1 - Trupp, Sabine A1 - Schug, Benedikt A1 - Mandel, Karl T1 - Indicator Supraparticles for Smart Gasochromic Sensor Surfaces Reacting Ultrafast and Highly Sensitive JF - Particle & Particle Systems Characterization N2 - The detection of toxic gases, such as NH\(_{3}\) and CO, in the environment is of high interest in chemical, electronic, and automotive industry as even small amounts can display a health risk for workers. Sensors for the real‐time monitoring of these gases should be simple, robust, reversible, highly sensitive, inexpensive and show a fast response. The indicator supraparticles presented herein can fulfill all of these requirements. They consist of silica nanoparticles, which are assembled to supraparticles upon spray‐drying. Sensing molecules such as Reichardt's dye and a binuclear rhodium complex are loaded onto the microparticles to target NH\(_{3}\) and CO detection, respectively. The spray‐drying technique affords high flexibility in primary nanoparticle size selection and thus, easy adjustment of the porosity and specific surface area of the obtained micrometer‐sized supraparticles. This ultimately enables the fine‐tuning of the sensor sensitivity and response. For the application of the indicator supraparticles in a gas detection device, they can be immobilized on a coating. Due to their microscale size, they are large enough to poke out of thin coating layers, thus guaranteeing their gas accessibility, while being small enough to be applicable to flexible substrates. KW - CO sensing KW - NH\(_{3}\) KW - sensor supports KW - silica supraparticles KW - smart surfaces Y1 - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-213671 VL - 36 IS - 10 ER - TY - JOUR A1 - Granath, Tim A1 - Löbmann, Peer A1 - Mandel, Karl T1 - Oxidative Precipitation as a Versatile Method to Obtain Ferromagnetic Fe\(_{3}\)O\(_{4}\) Nano‐ and Mesocrystals Adjustable in Morphology and Magnetic Properties JF - Particle & Particle Systems Characterization N2 - Oxidative precipitation is a facile synthesis method to obtain ferromagnetic iron oxide nanoparticles from ferrous salts—with unexplored potential. The concentration of base and oxidant alone strongly affects the particle's structure and thus their magnetic properties despite the same material, magnetite (Fe\(_{3}\)O\(_{4}\)), is obtained when precipitated with potassium hydroxide (KOH) from ferrous sulfate (FeSO\(_{4}\)) and treated with potassium nitrate (KNO\(_{3}\)) at appropriate temperature. Depending on the potassium hydroxide and potassium nitrate concentrations, it is possible to obtain a series of different types of either single crystals or mesocrystals. The time‐dependent mesocrystal evolution can be revealed via electron microscopy and provides insights into the process of oriented attachment, yielding faceted particles, showing a facet‐dependent reactivity. It is found that it is the nitrate and hydroxide concentration that influences the ligand exchange process and thus the crystallization pathways. The presence of sulfate ions contributes to the mesocrystal evolution as well, as sulfate apparently hinders further crystal fusion, as revealed via infrared spectroscopy. Finally, it is found that nitrite, as one possible and ecologically highly relevant reduction product occurring in nature in context with iron, only evolves if the reaction is quantitative. KW - colloidal nanostructures KW - nanoparticle aggregation KW - non‐classical crystallization KW - oriented attachment Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-224419 VL - 38 IS - 3 ER - TY - JOUR A1 - Schneider, Michael A1 - Tschöpe, André A1 - Hanselmann, Doris A1 - Ballweg, Thomas A1 - Gellermann, Carsten A1 - Franzreb, Matthias A1 - Mandel, Karl T1 - Adsorber Particles with Magnetically‐Supported Improved Electrochemical Conversion Behavior for Waste Water Treatment Processes JF - Particle & Particle Systems Characterization N2 - Micron‐sized supraparticles, consisting of a plurality of discrete nano‐ and microscale functional units, are assembled and fused by means of a droplet extrusion process. By combining nano magnetite, activated carbon, and conductive carbon with a polymeric binder matrix, particles are obtained which unite good magnetic properties, electrical conductivity, and adsorber activity through the high accessible surface area of the incorporated activated carbon of about 570 m\(^{2}\) g\(^{-1}\), thereby enabling a new approach toward sustainable water treatment processes. Due to the interplay of the components, it is possible to adsorb target substances, dissolved in the water which is demonstrated by the adsorption of the model dye methylene blue. A very fast adsorption kinetic and an adsorption capacity of about 400 mg g\(^{-1}\) is determined. By using the developed composite particles, it is also possible to electrochemically alter substances flowing through a magnetically‐stabilized fluidized‐bed reactor by electrochemically charging/discharging, significantly supported by the magnetic field enabling alternatingly optimum mobility/adsorption phases with contact/charging intervals. The electrochemical conversion can be increased up to 151% depending on the applied flow‐rate and electrical voltage. By applying an external magnetic field, a further increase of electrochemical conversion of up to 70% can be observed. KW - composite supraparticles KW - dye adsorption KW - electrochemical conversion KW - magnetic particles KW - water purification Y1 - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-214738 VL - 37 IS - 2 ER - TY - JOUR A1 - Miller, Franziska A1 - Wintzheimer, Susanne A1 - Prieschl, Johannes A1 - Strauss, Volker A1 - Mandel, Karl T1 - A Supraparticle‐Based Five‐Level‐Identification Tag That Switches Information Upon Readout JF - Advanced Optical Materials N2 - Product identification tags are of great importance in a globalized world with increasingly complex trading routes and networks. Beyond currently used coding strategies, such as QR codes, higher data density, flexible application as well as miniaturization and readout indication are longed for in the next generation of security tags. In this work, micron‐sized supraparticles (SPs) with encoded information (ID) are produced that not only exhibit multiple initially covert identification levels but are also irreversibly marked as “read” upon readout. To achieve this, lanthanide doped CaF\(_{2}\) nanoparticles are assembled in various quantity‐weighted ratios via spray‐drying in presence of a broad‐spectrum stealth fluorophore (StFl), yielding covert spectrally encoded ID‐SPs. Using these as pigments, QR codes, initially dominated by the green fluorescence of the StFl, could be generated. Upon thermal energy input, these particle‐based tags irreversibly switch to an activated state revealing not only multiple luminescent colors but also spectral IDs. This strategy provides the next generation of material‐based security tags with a high data density and security level that switch information upon readout and can be, therefore, used as seal of quality. KW - multilevel luminescence identification KW - rare earth doped nanoparticles KW - security tags KW - stealth fluorophores KW - supraparticles Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-224469 VL - 9 IS - 4 ER - TY - JOUR A1 - Müssig, Stephan A1 - Koch, Vanessa M. A1 - Collados Cuadrado, Carlos A1 - Bachmann, Julien A1 - Thommes, Matthias A1 - Barr, Maïssa K. S. A1 - Mandel, Karl T1 - Spray‐Drying and Atomic Layer Deposition: Complementary Tools toward Fully Orthogonal Control of Bulk Composition and Surface Identity of Multifunctional Supraparticles JF - Small Methods N2 - Spray‐drying is a scalable process enabling one to assemble freely chosen nanoparticles into supraparticles. Atomic layer deposition (ALD) allows for controlled thin film deposition of a vast variety of materials including exotic ones that can hardly be synthesized by wet chemical methods. The properties of coated supraparticles are defined not only by the nanoparticle material chosen and the nanostructure adjusted during spray‐drying but also by surface functionalities modified by ALD, if ALD is capable of modifying not only the outer surfaces but also surfaces buried inside the porous supraparticle. Simultaneously, surface accessibility in the porous supraparticles must be ensured to make use of all functionalized surfaces. In this work, iron oxide supraparticles are utilized as a model substrate as their magnetic properties enable the use of advanced magnetic characterization methods. Detailed information about the structural evolution upon individual ALD cycles of aluminium oxide, zinc oxide and titanium dioxide are thereby revealed and confirmed by gas sorption analyses. This demonstrates a powerful and versatile approach to freely designing the functionality of future materials by combination of spray‐drying and ALD. KW - atomic layer deposition KW - spray‐drying KW - supraparticles Y1 - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:bvb:20-opus-262521 VL - 6 IS - 1 ER -