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Recyclability-by-design of Printed Electronics by Low-Temperature Sintering of Silver Microparticles
(2025)
A low-temperature sintering mechanism of silver microparticles is established and used to enable the design-for-recycling of printed electronics. The formation of necks during the initial phase sintering of precipitated and atomized silver microparticles is studied. Temperature- and time-dependent in-situ analyses indicate the existence of a mobile silver species that provides efficient mass transport. The activation energy of neck formation identifies silver ion formation as the rate-limiting step of low-temperature silver sintering. It is demonstrated that resistivities of 271 times that of bulk silver can be attained after 40 minutes at 150°C. Low-temperature sintering not only reduces the energy required during thermal treatment but it yields layers that are suitable for recycling, too. The resulting layers have conductive necks that are mechanically weak enough to be broken during recycling. Printed layers are redispersed and the recycled silver powder is reused without loss of the electrical performance in new prints. Their conductivities are industrially relevant, which makes this recyclability-by-design approach promising for manufacturing more sustainable printed electronics.
Introduction: produced by renewable resources, biodegradable polymers with their competitive mechanical properties, thermal stability and biocompatibility are important alternatives to other synthetic materials for use in medical devices, i.e. endotracheal suction catheters. However, infected catheters may lead to nosocomial infections, such as lower respiratory tract infections, with mechanical ventilation being a major risk for these. Antimicrobially coated endotracheal suction catheters may be one measure to reduce this risk. Methods: two procedures using ethanol and sodium hydroxide were tested to immobilize poly(hexamethylene biguanide) (PHMB) to polylactide-ε-caprolactone (PLA-ε-CL). The cytocompatibility of the coating was verified via the MTT assay and cytokine analysis in a cell monolayer and in a 3D mucosa model. The antimicrobial efficacy was tested using S. epidermidis; after this bacterial contamination and the adherence and viability of cells were tested. Chemical surface analysis has been performed with pristine and PHMB-coated specimens by means of infrared spectroscopy (ATR-FTIR). Results: with both applied coating procedures, PHMB could be immobilized onto the PLA-ε-CL surface. The biocompatibility of PLA-ε-CL was not impaired by the PHMB coating. IL-1α was slightly but significantly increased. Reduction of S. epidermidis was about 4 lg-levels after 6 h of incubation. Contamination of the surface prior to cell culture did not impair the adherence of the cells. Conclusion: we demonstrated that PLA-ε-CL coated with PHMB has good biocompatible properties with antimicrobial activity thus revealing the polymer to be a suitable material for the development of medical devices that are able to prevent bacterial contaminations and infections.
Friction between fingertip and surface is a key contribution to tactile perception during active exploration of materials. We explore the role of skin factors such as stratum corneum thickness and hydration, deformability, elasticity, or density of sweat glands and of Meissner corpuscles in friction and tactile perception. The skin parameters were determined non-invasively for the glabrous skin at the index finger pad of 60 participants. Sets of randomly rough plastic surfaces and of micro-structured fibrillar rubber surfaces were explored as model materials with well-defined parameterized textures. Friction varies greatly between participants, and this variation can be explained to 70% by skin factors for the randomly rough plastic surfaces. The predictability of friction by skin factors is much lower for micro-structured rubber surfaces with bendable fibrils, where 50% of variance is explained for the stiffest fibrils but only 20% for the most bendable fibrils. The participants’ age is the key predictor for their tactile sensitivity to perceive the fibrils, where age is negatively correlated to the density of Meissner corpuscles. The results suggest that stratum corneum hydration, skin deformability, and age are important factors for friction and perception in active tactile exploration of materials.
Lithium-ion batteries play a crucial role in powering electric vehicles and portable electronics, making them indispensable in modern technology and driving a significant increase in global lithium demand. With more and more batteries reaching their end of life and the challenges of lithium extraction, including rising prices, geopolitical constraints, and environmental concerns, the efficient recovery of lithium from spent battery cells is crucial for sustainable battery recycling. While state-of-the-art battery recycling focuses mainly on pyro- and hydrometallurgical methods, electrochemical recycling methods can be an environmentally friendly, energy-efficient, and cost-effective alternative. This study optimizes an energy-efficient electrochemical method for selective LiCl extraction from leaching solutions derived from cathode materials of a typical battery cell format (lithium cobalt oxide (LCO)). This places our electrochemical separation within the hydrometallurgical processing of spent battery materials (black mass) and prior to subsequent lithium refining steps. Applying carbon-coated lithium iron phosphate (LFP) electrodes for selective lithium recovery yielded an average uptake capacity of 11.4 mgLi gLFP/C-1 over 300 cycles, maintaining a significant discharge capacity (30 mAh g-1) after 500 cycles.
This report is about the chemical formation of gels from ultrathin gold nanowires (AuNWs) and the gels’ properties. An excess of triphenylphosphine (PPh3) initiated the gelation of AuNWs with core diameters below 2 nm and an oleylamine (OAm) ligand shell dispersed in cyclohexane. The ligand exchange of OAm by PPh3 changes the AuNW-solvent interactions and leads to phase separation of the solvent to form a macroscopic gel. Small angle X-ray scattering and transmission electron microscopy indicate that hexagonal bundles in the original dispersion are dispersed, and the released nanowires entangle. Rheological analyses indicate that the resulting gel is stabilized both by physical entanglement and crosslinking of AuNWs by Van der Waals and π–π interactions. Chemically formed AuNW gels have solid-like properties and crosslinks that distinguish them from highly concentrated non-crosslinked AuNW dispersions. The AuNW gel properties can be tuned via the Au:PPh3 ratio, where smaller ratios led to stiffer gels with higher storage moduli.
The importance of shape: flakes and spheres in recyclable conductive pastes for printed electronics
(2025)
Silver microflakes and -spheres are common fillers for electrically conductive screen-printing pastes. Here, we report on the effects of filler shapes and sizes on conductivity, sintering, and recyclability. We printed pastes based on flakes and spheres, treated them at 110 °C to 300 °C, and evaluated the electrical conductivity of the resulting layers. The electrical conductivity of the layers treated at 110 °C was dominated by particle–particle contact resistances; flakes yielded layers that were five times more conductive than sphere-based layers due to differences in the particle–particle contact area. Increasing temperature led to a reduction of the resistivity of all layers through sintering. At 300 °C, prints based on spheres were 4 times more conductive than those from flakes. Tomography of the sintered structures showed that the difference was caused by a lower tortuosity factor for spheres. In a final study, we showed that silver flakes and spheres could be recycled after sintering and reused for a new generation of prints without losing electrical performance. The more porous structure of sintered flakes allowed for higher recycling yields compared to spheres. At 140 °C, 91.6% of the flakes and 69.7% of the spheres were recovered as reusable dispersions.
Metabolite-Responsive Control of Transcription by Phase Separation-Based Synthetic Organelles
(2025)
Living natural materials have remarkable sensing abilities that translate external cues into functional changes of the material. The reconstruction of such sensing materials in bottom-up synthetic biology provides the opportunity to develop synthetic materials with life-like sensing and adaptation ability. Key to such functions are material modules that translate specific input signals into a biomolecular response. Here, we engineer a synthetic organelle based on liquid–liquid phase separation that translates a metabolic signal into the regulation of gene transcription. To this aim, we engineer the pyruvate-dependent repressor PdhR to undergo liquid–liquid phase separation in vitro by fusion to intrinsically disordered regions. We demonstrate that the resulting coacervates bind DNA harboring PdhR-responsive operator sites in a pyruvate dose-dependent and reversible manner. We observed that the activity of transcription units on the DNA was strongly attenuated following recruitment to the coacervates. However, the addition of pyruvate resulted in a reversible and dose-dependent reconstitution of transcriptional activity. The coacervate-based synthetic organelles linking metabolic cues to transcriptional signals represent a materials approach to confer stimulus responsiveness to minimal bottom-up synthetic biological systems and open opportunities in materials for sensor applications.
The water dynamics in a nanocomposite film that consists of the electrically conductive poly(3,4-ethylene dioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) and cellulose nanofibrils (CNFs) have been investigated during three cycles of exposure to low and high relative humidity (RH = 5% and 85%, respectively) using quasi-elastic neutron scattering (QENS). The obtained dynamical structure factors are transformed into the imaginary part of the dynamic susceptibility to better differentiate between the individual relaxation processes. In a humid environment, two different water species are present inside the films: fast-moving bulk water and slow-moving hydration water. During the first cycle, a large amount of hydration water enhances the polymer chain mobility, eventually leading to irreversible structural rearrangements within the film. In the subsequent cycles, we observed a release of all bulk water and portions of hydration water upon drying, along with an uptake of both water species in a humid environment. The relaxation times of hydration water diffusion as a function of momentum transfer can be described by a jump-diffusion model. The obtained jump lengths, residence times, and diffusion coefficients of hydration water suggest a change in the hydration layer upon drying: water molecules around hydrophobic groups are released from the film, while the hydrogen bonds between water and hydrophilic groups are sufficiently strong to keep these molecules inside the films, even in a dry state. The QENS results can be correlated to the structural and conductive properties. In the dry state, the low hydration water content and the absence of bulk water allow for improved wetting of the CNFs by PEDOT:PSS, which eventually increases the electrical conductivity of the films.
Materials that can be switched between a polycationic/antimicrobial and a polyzwitterionic/protein-repellent state have important applications, e.g., as biofilm-reducing coatings in medical devices. However, the lack of stability under storage and application conditions so far restricts the lifetime and efficiency of such materials. In this work, a polynorbornene-based polycarboxybetaine with an optimized molecular structure for improved hydrolytic stability is presented. The polymer is fully characterized on the molecular level. Surface-attached polymer networks are obtained by spin-coating and UV cross-linking. These coatings are highly uniform and demonstrate charge-switching in zeta-potential studies. Storage stability in the dry state, as well as in aqueous systems at pH 4.5 and 7.4 for 28 days, is demonstrated. At pH 8, hydrolytic degradation is observed. Overall, the materials are substantially more stable than the corresponding ester-based systems.
Photocrosslinkable formulations based on the radical thiol-ene reaction are considered better alternatives than methacrylated counterparts for light-based fabrication processes. This study quantifies differences between thiol-ene and methacrylated crosslinked hydrogels in terms of precursors stability, the control of the crosslinking process, and the resolution of printed features particularized for hyaluronic acid (HA) inks at concentrations relevant for bioprinting. First, the synthesis of HA functionalized with norbornene, allyl ether, or methacrylate groups with the same molecular weight and comparable degrees of functionalization is presented. The thiol-ene hydrogel precursors show storage stability over 15 months, 3.8 times higher than the methacrylated derivative. Photorheology experiments demonstrate up to 4.7-times faster photocrosslinking. Network formation in photoinitiated thiol-ene HA crosslinking allows higher temporal control than in methacrylated HA, which shows long post-illumination hardening. Using digital light processing, 4% w/v HA hydrogels crosslinked with a dithiol allowed printing of 13.5 × 4 × 1 mm3 layers with holes of 100 µm resolution within 2 s. This is the smallest feature size demonstrated in DLP printing with HA-based thiol-ene hydrogels. The results are important to estimate the extent to which the synthetic effort of introducing –ene functions can pay off in the printing step.