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Organisationseinheit der BAM
A new method for top‐down, one‐pot, gram‐scale production of high quality nanographene by incubating graphite in a dilute sodium hypochlorite solution at only 40 °C is reported here. The produced sheets have only 4 at% oxygen content, comparable with nanographene grown by chemical vapor deposition. The nanographene sheets are covalently functionalized using a nondestructive nitrene [2+1] cycloaddition reaction that preserves their π‐conjugated system. Statistical analyses of Raman spectroscopy and X‐ray photoelectron spectroscopy indicate a low number of sp3 carbon atoms on the order of 2% before and 4% after covalent functionalization. The nanographene sheets are significantly more conductive than conventionally prepared nanographene oxide, and conductivity further increases after covalent functionalization. The observed doping effects and theoretical studies suggest sp2 hybridization for the carbon atoms involved in the [2+1] cycloaddition reaction leading to preservation of the π‐conjugated system and enhancing conductivity via n‐type doping through the bridging N‐atom. These methods are easily scalable, which opens the door to a mild and efficient process to produce high quality nanographenes and covalently functionalize them while retaining or improving their physicochemical properties.
Reliability study of a tunable ka-band SIW-phase shifter based on liquid crystal in LTCC-technology
(2014)
A tunable substrate-integrated waveguide phase shifter using low-temperature co-fired ceramic (LTCC)-technology is presented in this paper. By changing the effective permittivity in the liquid crystal (LC)-filled waveguide, the differential phase can be tuned continuously. This is achieved by means of an analog signal applied to the electrodes, surrounding the LC. The design allows for precise tuning of the differential phase, which is proven with a Monte Carlo measurement resulting in phase errors of less than 3° at 28 GHz. Besides that, the ambient temperature dependency of the module is shown. The phase shifter has a high integration level and can be included into a complete and lightweight single-phased array antenna module. The phase shifter is realized with a high level of integration which is available through the multilayer process of the LTCC. It has a length of 50 and provides a differential phase shift of more than 360° at 28 GHz. The figure of merit for tunable phase shifters is >40°/dB.
The relationship between fracture toughness and Yttria content in modern zirconia ceramics was revised. For that purpose, we evaluated here 10 modern Y2O3-stabilized zirconia (YSZ) materials currently used in biomedical applications, namely prosthetic and implant dentistry. The most relevant range between 2-5 mol% Y2O3 was addressed by selecting from conventional opaque 3 mol% YSZ up to more translucent compositions (4-5 mol% YSZs). A technical 2YSZ was used to extend the range of our evaluation. The bulk mol% Y2O3 concentration was measured by X-Ray Fluorescence Spectroscopy. Phase quantification by Rietveld refinement considered two tetragonal phases or an additional cubic phase. A first-account of the fracture toughness (KIc) of the pre-sintered blocks is given, which amounted to 0.4 – 0.7 MPa√m. In the fully-densified state, an inverse power-law behavior was obtained between KIc and bulk mol% Y2O3 content, whether using only our measurements or including literature data, challenging some established relationships. A linear relationship between KIc and the fraction of the transformable t-phase was established within the range of 30–70 vol%.
Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale
(2020)
Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation.
Recent advances in the development of high gauge factor thin films for strain gauges prompt the research on advanced substrate materials. A glass ceramic composite has been developed in consideration of a high coefficient of thermal expansion (9.4 ppm/K) and a low modulus of elasticity (82 GPa) for the application as support material for thin-film sensors. In the first part, constantan foil strain gauges were fabricated from this material by tape casting, pressure-assisted sintering, and subsequent lamination of the metal foil on the planar ceramic substrates. The accuracy of the assembled load cells corresponds to accuracy class C6. That qualifies the load cells for the use in automatic packaging units and confirms the applicability of the low-temperature co-fired ceramic (LTCC) substrates for fabrication of accurate strain gauges. In the second part, to facilitate the deposition of thin-film sensor structures to the LTCC substrates, pressure-assisted sintering step is modified using smooth setters instead of release tapes, which resulted in fabrication of substrates with low average surface roughness of 50 nm. Titanium thin films deposited on these substrates as test coatings exhibited low surface resistances of 850 Ω comparable to thin films on commercial alumina thin-film substrates with 920 Ω. The presented material design and advances in manufacturing technology are important to promote the development of high-performance thin-film strain gauges.
Integration of magnetic functional components in LTCC circuit boards calls for co-firing of dielectric and ferrite tapes. Ni-Cu-Zn ferrites with permeability of µ = 900 were fully densified at the standard LTCC sintering temperature of 900°C. Co-firing of this ferrite with dielectric tapes requires the adaptation of the shrinkage behavior of the materials as well as the thermal contraction during the cooling period – especially in the temperature range below the transformation point of the glass phase of the dielectric tape. To match these preconditions, a new dielectric LTCC material with steep sintering curve and high thermal expansion coefficient was designed. Sintered multilayer laminates composed of Ni-Cu-Zn ferrite and tailored dielectric tapes are free of cracks and possess no open porosity. No significant interdiffusion between the ferrite and dielectric tapes was found using microprobe analysis. Pure ferrite laminates show homogeneous microstructure with large grains up to 50 µm in diameter. However, growth of ferrite grains does not take place near the interface between ferrite and release or dielectric tapes. There is a strong correlation between permeability and volume fraction of large ferrite grains. Compared to pure ferrite laminates the permeability of co-sintered Ni-Cu-Zn ferrite layers is drastically reduced to 400, that is a decrease of more than 50%.
The sintering behavior of sub-micron Ni0.30Cu0.20Zn0.52Fe1.98O3.99 ferrite with and without Bi2O3 addition was studied. Ferrites with 0.5 wt% Bi2O3 exhibit enhanced shrinkage at T < 900 °C with significant grain growth. Additive-free ferrite powders also sinter to high density at 900 °C, however, grain growth is very limited. Both ferrites exhibit a permeability of µ = 400–450. Multilayers consisting of ferrite and low-k dielectric LTCC layers were prepared by co-firing at 900–915 °C. The shrinkage and thermal expansion characteristics of ferrite and LTCC tapes are similar. However, the permeability of integrated ferrite layers, made from ferrite tapes with Bi2O3 additive, significantly drops after co-firing with LTCC layers compared to separately fired monolithic ferrite multilayers. Contrarily, the permeability of integrated, Bi2O3-free ferrite layers, co-fired with dielectric tapes, is identical to that of monolithic ferrite multilayers. This finding is an important step toward ferrite integration into complex LTCC multilayer architectures.
Implementation of Ba0.6Sr0.4TiO3-ZnO-B2O3 based tunable microwave phase shifters in LTCC technology
(2017)
Tunable dielectric Ba0.6Sr0.4TiO3-ZnO-B2O3 thick-films were analyzed regarding their integration potential into the LTCC technology. Therefore, tunable loaded line phase shifters based on metal-insulator-metal varactors with single- and double- printed BST thick-films were fabricated and co-sintered inside a four layer LTCC module. Microstructural and chemical investigations showed a sufficient compatibility and adhesion between the silver, BST composite and LTCC layers and a resulting morphology depending on the processing route. The microwave characterization of the LTCC-embedded phase shifters revealed comparable results to phase shifters with the same design on alumina substrates.
2D nanomaterials have garnered widespread attention in biomedicine and
bioengineering due to their unique physicochemical properties. However, poor functionality, low solubility, intrinsic toxicity, and nonspecific interactions at biointerfaces have hampered their application in vivo. Here, biocompatible polyglycerol units are crosslinked in two dimensions using a graphene-assisted strategy leading to highly functional and water-soluble polyglycerols nanosheets with 263 ± 53 nm and 2.7 ± 0.2 nm average lateral size and thickness, respectively.
A single-layer hyperbranched polyglycerol containing azide functional
groups is covalently conjugated to the surface of a functional graphene template through pH-sensitive linkers. Then, lateral crosslinking of polyglycerol units is carried out by loading tripropargylamine on the surface of graphene followed by lifting off this reagent for an on-face click reaction. Subsequently, the polyglycerol nanosheets are detached from the surface of graphene by slight acidification and centrifugation and is sulfated to mimic heparin sulfate proteoglycans. To highlight the impact of the two-dimensionality of the synthesized polyglycerol sulfate nanosheets at nanobiointerfaces, their efficiency with respect to herpes Simplex
virus type 1 and severe acute respiratory syndrome corona virus 2 inhibition is compared to their 3D nanogel analogs. Four times stronger in virus Inhibition suggests that 2D polyglycerols are superior to their current 3D counterparts.2D nanomaterials have garnered widespread attention in biomedicine and bioengineering due to their unique physicochemical properties. However, poor functionality, low solubility, intrinsic toxicity, and nonspecific interactions at biointerfaces have hampered their application in vivo. Here, biocompatible polyglycerol units are crosslinked in two dimensions using a graphene-assisted strategy leading to highly functional and water-soluble polyglycerols nanosheets with 263 ± 53 nm and 2.7 ± 0.2 nm average lateral size and thickness, respectively.
A single-layer hyperbranched polyglycerol containing azide functional groups is covalently conjugated to the surface of a functional graphene template through pH-sensitive linkers. Then, lateral crosslinking of polyglycerol units is carried out by loading tripropargylamine on the surface of graphene followed by lifting off this reagent for an on-face click reaction. Subsequently, the polyglycerol nanosheets are detached from the surface of graphene by slight acidification and centrifugation and is sulfated to mimic heparin sulfate proteoglycans. To highlight the impact of the two-dimensionality of the synthesized polyglycerol sulfate nanosheets at nanobiointerfaces, their efficiency with respect to herpes Simplex virus type 1 and severe acute respiratory syndrome corona virus 2 inhibition is compared to their 3D nanogel analogs. Four times stronger in virus Inhibition suggests that 2D polyglycerols are superior to their current 3D counterparts.
Low-κ dielectric LTCC was developed, to realize successful co-firing with NiCuZn ferrite tapes. A critical high-temperature process in the production of highly integrated LTCC modules is the migration of silver from inner conductors into the LTCC glass phase. Intensive silver migration causes strong deformation of LTCC multilayers during firing in air.
Silver migration into the LTCC glass phase depends on oxygen content of the sintering atmosphere and can be minimized by sintering in nitrogen atmosphere. However, partial decomposition of NiCuZn-ferrite and formation of cuprite was observed during sintering in nitrogen and, consequently, the permeability of the ferrite decreases. As shown by a combined XRD/thermogravimetric study the co-firing of LTCC modules with silver metallization and integrated ferrite layer demands precise adjustment of oxygen partial pressure.