Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (18)
- Beitrag zu einem Tagungsband (8)
- Sonstiges (1)
- Forschungsbericht (1)
Schlagworte
- LTCC (13)
- Ferrite (6)
- Co-firing (4)
- XPS (3)
- Coefficient of thermal expansion (CTE) (2)
- Cofiring (2)
- Datenmanagement (2)
- Inclusions (2)
- Modeling (2)
- NEXAFS (2)
- Shrinkage (2)
- Sintering (2)
- Strain gauge (2)
- Thin-film substrate (2)
- 2D (1)
- 2D Materials (1)
- AFM (1)
- Aggregation (1)
- Azoverbindungen (1)
- Bifunctional 2D nanomaterials (1)
- Big Data (1)
- Calcium peroxide (1)
- Capacitor (1)
- Ceramics (1)
- Constrained sintering (1)
- Dental (1)
- Dielectric materials (1)
- Digitalisierung (1)
- EOS (1)
- EPMA (1)
- Electroceramics (1)
- Ferrite integration (1)
- Ferrites (1)
- Fertigungsprozess (1)
- Fracture toughness (1)
- Glas Matrix Composites (1)
- Glass matrix composites (1)
- Graphene (1)
- Graphene oxide (1)
- Graphene template (1)
- Grenzflächenreaktion (1)
- Hexagonal ferrites (1)
- IGUS (1)
- Integrated inductors (1)
- Interface (1)
- Keramik (1)
- Keramische Multilayer (1)
- LTCC modules (1)
- Micro-XRF (1)
- Microfocus x-ray source (1)
- Multilayer (1)
- Multilayer ceramic technology (1)
- Multilayer inductors (1)
- Multivalency (1)
- Nanostrukturen (1)
- New and emerging technologies and materials (1)
- Ni-Cu-Zn ferrites (1)
- Passive components and circuits (1)
- Permeability (1)
- Photochromie (1)
- Polyglycerol (1)
- Polymere (1)
- Power law (1)
- Pressure-assisted sintering (1)
- Round robin (1)
- SEM (1)
- Sensorik (1)
- Shrinkage behavior (1)
- Silver conductors (1)
- Silver diffusion (1)
- Sintering Kinetics (1)
- Sintering kinetics (1)
- Sodium nitrate (1)
- Sodium perborate monohydrate (1)
- Solid oxidizer test (1)
- Thick films (1)
- Transformer (1)
- Triazine (1)
- United Nations (1)
- Virus inhibition (1)
- Windenergie (1)
- X-ray-diffraction (1)
- Zirconia (1)
Organisationseinheit der BAM
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.
The classification of solid oxidizers according to the regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and accepted by all international organisations for the transport of dangerous goods as ADR, IMO, IATA) and in future also according to the GHS (Globally Harmonized System of Classification and Labelling of Chemicals) is performed on the basis of the results of the UN test O.1 (UN test O.1 ―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Dangerous Goods – Manual of Tests and Criteria, see [1]). This test was introduced into the UN Manual of Tests and Criteria in 1995 as a replacement for a similar test from 1986. Even if the UN O.1 test as described in the current 5th revised edition of UN Manual of Tests and Criteria gives some improvements compared to the old test, which had had many deficiencies, there are still some problems left with this test in terms of e.g. repeatability or reproducibility of test results, how to handle compacted or multilayer formulations like tablets, toxicity and partly significantly varying particle size distribution within defined fractions of 150 μm to 300 μm of the reference oxidizer potassium bromate (KBrO3). For this reason the IGUS EOS working group installed an ad-hoc working group in 2002 assigned with the task to propose solutions for the existing problems. The appropriateness of such proposed solutions has to be proved by the method of interlaboratory (round robin) tests before they are presented for the adoption to the UN Committee of Experts on the TDG and on the GHS with a proposal of a completely revised test procedure.
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.
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.
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.
Scanning electron microscopes are usually equipped with energy-dispersive X-ray detectors for electron probe microanalysis. This widespread analytical method allows investigators to determine the elemental composition of specimens with a spatial resolution of about 1 µm. However, owing to the electron-specimen interaction, the emitted spectra reveal, in addition to characteristic lines, also a high level of continuous bremsstrahlung background. As a result, elements with low concentrations cannot be identified. The minimum detection limit can be diminished by two orders of magnitude if the characteristic lines are excited as fluorescence by an additional x-ray source. In this case, the emergence of bremsstrahlung is considerably reduced. Combining a high-brilliance microfocus x-ray tube with efficient polycapillary optics enables one to realize an experimental arrangement for performing local fluorescence analysis at the same point where the electron beam hits the sample. The polycapillary optics under consideration focuses the emitted x-radiation onto focal spots between 30 and 100 µm in diameter. Count rates of several thousands cps have been achieved. Elemental maps have been obtained by means of the motorized specimen stage of the microscope. Copyright © 2005 John Wiley & Sons, Ltd.
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 p=900 were developed which can be fully densified at the Standard LTCC sintering temperature of 900 °C. Successful co-firing of this ferrite with dielectric tapes requires the adaptation of the shrinkage behavior of the materials as well as the thermal expansion during the cooling period - especially in the temperature range below the transformation point of the glassy 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 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 by EDX measurements. Compared to pure ferrite laminates the permeability of co-sintered Ni-Cu-Zn ferrite layers is drastically reduced to 400, i.e. a decrease of more than 50 %.
To investigate the origin of this permeability reduction, Ni-Cu-Zn ferrite laminates were sintered separately, and in combination with alumina release tapes or dielectric tapes, respectively. SEM and EDX analysis of co-fired laminates reveal differences in the ferrite grain growth behavior. Ferrite laminates with homogeneous microstructure and grain size up to 50 pm exhibit large permeability. 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 high permeability and volume fraction of large ferrite grains. Regions of fine and coarse grains inside the ferrite layers show different bismuth concentration; the Bi-content is larger in regions of fine ferrite grains.
Further miniaturization of electronic packaging calls for integration of magnetic functional components into LTCC modules. For integration of magnetic function into LTCC, low fired MnZn- and NiCuZn-ferrites which can be fully densified at the standard LTCC sintering temperature of 900°C were developed. To co-fire these ferrite tapes with dielectric tapes the sintering shrinkage and the coefficient of thermal expansion of ferrite and dielectric tapes must be matched. For each ferrite material a new LTCC dielectric material was designed. The embedded ferrite tapes into new LTCC dielectric tapes can be sufficiently densified during co-firing at 900°C without any cracking. Compared to separately sintered ferrites the permeability of embedded ferrite tapes is reduced. For embedded NiCuZn ferrites permeabilities between 230 and 570 (at 2 MHz) according to the thickness of the embedded ferrite layer were measured. For embedded MnZn ferrites a permeability of 300 was measured.
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 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.
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.
Dieses Strategiepapier zielt darauf ab, Akteuren und Entscheidungsträgern den Status der Digitalisierung in der keramischen Fertigung, erfolgreiche Best-Practice-Beispiele aber auch die Herausforderungen nahezubringen, die es nun anzugehen gilt. Es ist die Vision, die Keramikfertigung durchgehend zu digitalisieren und alle Schritte des Produktkreislaufs lückenlos über die gesamte Wertschöpfungs- und Nutzungskette zu vernetzen: also eine Keramikindustrie 4.0 zu etablieren. Das Strategiepapier erfasst zunächst die Spezifität der keramischen Fertigung und nimmt eine Analyse des gegenwärtigen Standes der Digitalisierung in der keramischen Industrie vor, auch anhand einiger ausgewählter Beispiele aus der industriellen Praxis. Auf Basis der wesentlichen Bausteine für eine Fertigungsdigitalisierung werden schließlich die Chancen für Keramikproduzenten sowie der erforderliche Forschungs- und Entwicklungsbedarf aufgezeigt.
LTCC-modules with integrated ferrite layers - Strategies for material development and co-sintering
(2008)
Silver in LTCC - Interfacial reactions, transport processes and influence on properties of ceramics
(2009)
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.
Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes.
While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique.
Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section.
As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width.
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.