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Glaskeramische Komposite, deren Herstellung von Glas- und kristallinen Pulvern ausgeht, bieten vielfältige Möglichkeiten, Werkstoffeigenschaften, wie z.B. Sinterverhalten, thermische Dehnung, mechanische Eigenschaften, chemische Beständigkeit, dielektrische Eigenschaften und Oberflächenqualität für spezielle Anwendungszwecke gezielt einzustellen. Glaskeramische Kompositpulver können zu Folien verarbeitet werden, aus denen mittels der LTCC (Low Temperature Co-fired Ceramics)- Technologie keramische Multilayer hergestellt werden, die insbesondere für das Electronic Packaging von Mikrosystemen eingesetzt werden. Problematisch ist die beim freien Sintern der LTCC-Multilayer auftretende laterale Schwindung, die von relativ hohen Schwindungstoleranzen begleitet ist. Zur Vermeidung der lateralen Schwindung werden Zero Shrinkage-Techniken eingesetzt. Eine neue Möglichkeit Zero Shrinkage beim Sintern von LTCC-Multilayern zu erreichen, besteht in der Anwendung eines self-constrained Laminates. Hierbei wird ein Multilayer eingesetzt, der aus zwei unterschiedlichen Folienarten für innere und äußere Lagen mit deutlich verschiedenen Sintertemperaturen (ΔT > 50 K) aufgebaut wird. Die Entwicklung von LTCC -Werkstoffen, die als innere Lagen eines self-constrained Laminates zur Verringerung der lateralen Sinterschwindung auf nahezu Null eingesetzt werden können, war Gegenstand der vorliegenden Arbeit. Es wurden hierfür LTCC - Werkstoffe aus dem Stoffsystem CaOLa2O3-Al2O3-B2O3 untersucht, die bei Temperaturen unterhalb 800 °C dicht gesintert werden können. Ausgehend von der Entwicklung geeigneter Gläser auf der Basis von Calciumlanthanborat- sowie Calciumlanthanalumoboratgläsern wurden glaskeramische Komposite unter Zusatz von Korundpulver hergestellt. Die Komposite kristallisieren während des Brennprozesses nahezu vollständig. Aus der Glasphase kristallisiert Lanthanborat aus und aufgrund der festkörperchemischen Reaktion der calciumboratreichen Restglasphase mit dem Korund bilden sich vor allem Calciumalumoborat bzw. Calciumalumoboratoxid. Die Anteile an neuen Phasen bestimmen die thermischen und dielektrischen Eigenschaften der Werkstoffe. Die wichtigsten der sich bildenden kristallinen Phasen der Komposite, Lanthanborat und Calciumalumoboratoxid wurden separat hergestellt und charakterisiert. Das Sinter- und Kristallisationsverhalten sowie die thermischen und dielektrischen Eigenschaften der glaskeramischen Komposite wurden in Abhängigkeit von den entwickelten Gläsern, dem Volumenverhältnis von Glas- und kristalliner Komponente im Kompositpulver und der Brenntemperatur untersucht. Die entwickelten LTCC-Werkstoffe wurden bzgl. ihrer thermischen Eigenschaften an einen zuvor ausgewählten LTCC-Werkstoff für die äußeren Lagen eines self-constrained Laminates angepasst. Erzielt wurden die Eigenschaftswerte: TEC: ca. 5 x 10-6/K, εr: ca. 7 und tan δ: ≤ 1 x 10-3. Zur Überprüfung der Anwendbarkeit wurde der entwickelte LTCC- Werkstoff als innere Lagen in einem LTCC-Multilayer verarbeitet. Dadurch konnte die laterale Schwindung des Multilayers beim Sintern auf < 0,4 % verringert werden.
Glaskeramische LTCC-Folien und multilayer-Technologie für Mikrosysteme / intelligente Sensoren
(2003)
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.
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.
Alumina sols were prepared using a modified
Yoldas procedure, thus resulting in sols with high solids
content, excellent long term stability and small particle size.
PH-value ranged between 3.7 and 0.6. Sols were characterised
using rheological, UV-vis transmission and particle
size measurements. Depending on NO3-/Al molar ratio as
well as solids content, sols vary. Analysis of reduced viscosities
indicate the formation of chainlike polymeric species
above a critical solids fraction.
Presented are results of an inter-laboratory study (ILS) for measurements of the particle size distribution of fine powders in wet dispersion by laser diffraction. In this proficiency test 32 participants from four countries took part. They utilized 13 different devices from 7 manufacturers.
Three commercial powders (glass spheres and two silicon carbide powders) showing a median diameter of about 30, 10 and 1 µm (volume distribution), respectively, were chosen for the procedure. A homogeneity study was carried out after the units had been separated and bottled.
All participants received their test samples including a description of the standard operating procedures based on ISO 13320:2009 – to ensure that experiments were performed in a consistent manner. Results were calculated using the Mie Theory. The general means and the precision of the results were estimated in accordance with ISO 5725-2:2002.
The evaluation showed excellent values of repeatability standard deviation. Values of 4 to 21?% of the reproducibility standard deviation of the results were found in the particle size range above 1 µm. Much larger deviation between the labs was detected in the case of smaller particles. Differences in the design of the analyzers were unambiguously identified as the main reason for the large deviations.
Resolution of capacitive sensors can be improved enormously by replacement of the dielectric material between the capacitor plates (e.g. air-dielectric) by a dielectric fluid with high permittivity. High dielectric liquid dispersions of ceramic micro and nano powders should be qualified as dielectric fluid with longtime shelf life.
For this purpose it was necessary to produce stabilized ceramic suspensions with high particle concentration and to investigate sedimentation processes of the particles. Characterization of particles was done by use of zeta potential measurement, gas adsorption measurements (BET), density measurement with gas pycnometer as well as particle sizing by ultrasound spectroscopy and by use of an optical centrifuge.
Shelf life of optimized electrostatic and steric stabilized ceramic suspension was investigated by use of an optical centrifuge, a LUMISizer 651 MW (LUM Ltd.) with STEP technology and front tracking analysis. Two different wave lengths – NIR (865 nm) and blue light (470 nm) were available for examination. Centrifugation measurements with different rotation speed were used to study the rheological behavior and the sedimentation process. By this way it was possible to achieve accelerated stability determination. Measured values could be used to simulate the sedimentation process under gravity acceleration and to predict shelf life for suspensions with different dispersants.