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Neue niedrig sinternde Mikrowellenkeramik für Anwendungen in der mobilen Kommunikationstechnik
(2003)
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.
High-power optical multimode fibers are essential components for materials processing and surgery and can limit the performance of expensive systems due to breakdown at the end faces. The aim of this paper is the determination of laser-induced damage thresholds (LIDT) of fibers (FiberTech) and preforms (Heraeus Suprasil F300). Preforms served as models. They were heated up to maximum temperatures of 1100, 1300 and 1500°C and cooled down to room temperature at rates of 10 K min-1 (oven) and ~105 K min-1 (quenched in air) to freeze in various structural states simulating different conditions similar to a drawing process during the production of fibers. Single- and multi-pulse LIDT measurements were done in accordance with the relevant ISO standards. Nd:YAG laser pulses with durations of 15 ns (1064 nm wavelength) and 8.5 ns (532 nm) at a repetition rate of 10 Hz were used. For the preforms, LIDT values (1-on-1) ranged from 220 to 350 J/cm² (1064 nm) and from 80 to 110 J/cm² (532 nm), respectively. A multi-pulse impact changed the thresholds to lower values. The LIDT (1064 nm wavelength) of the preforms can be regarded as a lower limit for those of the fibers.
The sintering of Low Temperature Co-fired Ceramics prepared from alumoborosilicate
glass- and Al2O3 powders of similar small particle size was studied by dilatometry, heating microscopy,
microstructure analysis, glass- and effective viscosity measurements. The steric effect of
Al3O3 inclusions was studied using a gnon-reactiveh model composite. With increasing Al3O3 volume
fraction (Φ ≤ 0.45), sintering decelerates and its final stage shifts to higher temperature. The
attainable shrinkage is reduced as Al2O3 particle clusters bearing residual pores become more frequent.
The kinetics of sintering could be described formally superposing the weighed contributions
of differentially sized and randomly composed glass-crystal particle clusters and assuming a sintering
rate controlled by the effective matrix viscosity, which increases with Φ and with progressive
wetting of Al2O3 particles during densification. The "reactive" model composite shows significant
dissolution of Al2O3 into the glass, which has two opposed effects on sintering: reducing Φ and increasing
glass viscosity. For the present case (Φ = 0.25), the latter effect dominates and sintering is
retarded by Al2O3 dissolution. Crystallization of wollastonite starts after full densification. Dissolution
of Al2O3 was found to promote the subsequent growth of anorthite.
Optical multimode fibers are applied in materials processing (e.g. automotive industry), defense, aviation technology, medicine and biotechnology. One challenging task concerning the production of multimode fibers is the enhancement of laser-induced damage thresholds. A higher damage threshold enables a higher transmitted average power at a given fiber diameter or the same power inside a thinner fiber to obtain smaller focus spots.
In principle, different material parameters affect the damage threshold. Besides the quality of the preform bulk material itself, the drawing process during the production of the fiber and the preparation of the fiber end surfaces influence the resistance. Therefore, the change of the laser-induced damage threshold of preform materials was investigated in dependence on a varying thermal treatment and preparation procedure.
Single and multi-pulse laser-induced damage thresholds of preforms (F300, Heraeus) were measured using a Q-switched Nd:YAG laser at 1064 nm wavelength emitting pulses with a duration of 15 ns, a pulse energy of 12 mJ and a repetition rate of 10 Hz. The temporal and spatial shape of the laser pulses were controlled accurately.
Laser-induced damage thresholds in a range from 150 J cm-2 to 350 J cm-2 were determined depending on the number of pulses applied to the same spot, the thermal history and the polishing quality of the samples, respectively.
Multilayer ceramic devices based on low-temperature co-fired ceramics (LTCC) materials provide a very promising technology. Most LTCC tapes available today contain considerable fractions of glass powders to lower the sintering temperature. However, the glassy phases offer more possibilities to set a proper sintering behavior, on the one hand, and to tailor the desired properties of the final LTCC substrate, on the other. The exploitation of demixing and subsequent crystallizing glass compositions was shown on an example of a low-permittivity (4.4)low-loss (1.5 × 103) LTCC with a high quartz content. In another LTCC material, undesired demixing could be restricted and the crystal phase anorthite could be triggered by partial dissolution of alumina in the liquid phase during sintering. To estimate the effect of silver diffusion in the latter material, the surroundings of a pure silver via were studied. A silver-contaminated range of 50 µm was detected. Using model glasses containing silver oxide, a strong influence of dissolved silver on viscosity and crystallization behavior of the liquid phase was demonstrated. The dielectric properties of the sintered substrates were not degraded.
High-power optical multimode fibers are essential components for materials processing
and surgery and can limit the reliability of expensive systems due to breakdown at the end faces.
The breakdown threshold of fibers is determined by intrinsic materials properties and parameters of
the technology applied. The aim of this paper is the identification of technological parameters that
are crucial for the fiber quality.
Fibers were drawn from preforms of Heraeus SWU with core material F300 and a low amount of
OH-. Both, the cladding (fluorine doped SiO2) to core diameter ratio (CCDR) and the drawing speed
were varied. CCDR values between 1.05 and 1.4 were used. Afterwards, the laser-induced damage
thresholds (LIDT) of the fibers were determined. For comparison, also samples from preforms,
which underwent different thermal treatments above the transition temperature, were tested with
respect to their damage resistivity. Single and multi pulse LIDT measurements were done in
accordance with the relevant ISO standards. Nd:YAG laser pulses with durations of 15 ns (1064 nm
wavelength) and 8.5 ns (532 nm) at a repetition rate of 10 Hz were utilized. For the fibers, LIDT
values (1-on-1, 1064 nm and 532 nm) increased with growing CCDR and with decreasing drawing
velocities.