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Organisationseinheit der BAM
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.
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.
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 and a low modulus of elasticity for the application as support material for thin-film sensors. 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 sensors were mounted on a strain gauge beam arrangement and load curves and creep behavior were evaluated. The accuracy of the assembled load cells correspond to accuracy class C6. That qualifies the load cells for the use in automatic packaging units and confirms the applicability of the LTCC substrates for fabrication of accurate strain gauges. To facilitate the deposition of thin film sensor structures onto the LTCC substrates, the pressure-assisted sintering technology has been refined. By the use of smooth setters instead of release tapes substrates with minimal surface roughness were fabricated. Metallic thin films deposited on these substrates exhibit low surface resistances comparable to thin films on commercial alumina thin-film substrates. The presented advances in material design and manufacturing technology are important to promote the development of high performance thin-film strain gauges.
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.