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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.
LTCC-Modules with integrated ferrite layers - Strategies for material development and co-sintering
(2009)
The integration of passive components (resistors, capacitors, inductors) into LTCC modules is a challenging task in multilayer ceramics technology. We report on multilayer assemblies consisting of combined layers of ferrite and dielectric LTCC tapes. Ni-Cu-Zn ferrites with maximum shrinkage at 900°C were processed to green tapes and laminated with dielectric LTCC tapes. Cosintering at 900°C led to multilayers with different defects such as incomplete densification of the ferrite layers, cracks, and warpage. Since ferrite tapes do not really allow compositional changes without deterioration of magnetic properties, the dielectric tape was modified with the following objectives: (i) matching of the shrinkage curves of dielectric and ferrite materials, (ii) adjusting the coefficients of thermal expansion to avoid cracking during cooling, and (iii) controlling of interface reactions. Using this concept we fabricated dense and defect-free multilayers consisting of dielectric and ferrite layers. However, compositional changes of the individual ferrite tapes require the development of a specific dielectric tape material with tailored properties.
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.
Synthetic molecular systems undergoing structure and property changes as a response to external stimuli offer a series of relevant functions. Their direct use in solution, immobilized at surfaces, or integrated into adequate matrices, allow for the elaboration of nano-carriers, molecular electronic memory circuits, adaptive systems, artificial muscles, or healable materials, among others. Reversible systems are commonly generated by utilizing molecular switches as responsive bi-stable molecules. Of particular interest are switches controlled by non-invasive triggers, especially light, which can display high spatial and temporal resolution. Photoswitches were used to change properties, such as conductance and basicity, based on light-induced alteration of the molecular geometry, that is, their dimensions and shape. In nature, light-induced geometrical modifications of molecular systems lead to primary biological functions, such as the visual perception in vertebrates, or proton pumping in some bacteria, two examples that nicely illustrate the potential of photo-inducing structural modifications in organic systems.
We studied sintering of LTCC-type glass matrix composites (GMCs) consisting of small glass and alumina particles of equal size. Primarily, crystals act as rigid inclusions, decelerating the densification rate. In later stages, they also dissolve, partially increasing the viscosity. Release of alumina finally induces crystallization of alumosilicates, which enables post-firing stability. To study both effects, two model GMCs were prepared: an α-Al2O3 + barium alumoborosilicate glass (BABS)GMC, which shows neither significant dissolution nor crystallization, and an α-Al2O3 + calcium alumoborosilicate glass (CABS)GMC, which dissolves readily and promotes crystallization. The kinetics of shrinkage for both GMC were modeled by utilizing Frenkel theory for the early stage and MackenzieShuttleworth theory for the late stage, assuming that sintering is superimposed by the weighted contributions of triparticle glasscrystal clusters, their random occurrence (ideal mixing), and a shrinkage rate controlled by the GMC effective viscosity. In agreement with modeling, the experimental results showed that the shrinkage rate of BABSGMC decreases progressively for crystal volume fractions Φ > 0.15. The attainable shrinkage is reduced by up to 8% for Φ = 0.45. For the CABSGMC with Φ = 0.25, a reduction of Φ to 0.20 was evident due to partial α-Al2O3 dissolution. This effect was found able to increase the sintering temperature by ~5060 K.
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%.
We have studied the integration of Ni-Cu-Zn ferrite spinels as well as substituted hexagonal Co2Y-and M-type ferrites into LTCC (Low Temperature Ceramic Co-firing) modules. The cofiring behavior and the magnetic properties of these materials were investigated and evaluated for multilayer applications. Ni-Cu-Zn ferrites exhibit permeabilities of µ=300–500 for operating frequencies in the MHz range. Cu-substituted Y-type ferrites Ba2Co2-x-yZnxCuyFe12O22 in combination with sintering additives display sufficient shrinkage and densification at 900°C. A permeability of µ=10 is observed; however, substituted Co2Y-type ferrites do not exhibit long-term stability at 900°C. Co/Ti-substituted M-type ferrites BaFe12-2yCoyTiyO19 (y=1.2) with planar magneto-crystalline anisotropy exhibit excellent soft magnetic behavior. Using sintering additives, complete densification is reached at 900°C and a permeability of µ=15 and a resonance frequency of larger than 1?GHz are observed. Integration of ferrite multilayer inductor components into LTCC modules using free and constrained cofiring technologies is demonstrated.