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Eingeladener Vortrag
- nein (432) (entfernen)
Thermoelectric generators can be used for energy harvesting by directly transforming a temperature gradient into a voltage. Multilayer generators based on ceramic multilayer technology are an interesting alternative to conventional π-type generators. They exhibit several advantages like high filling factor, possibility of texturing, co-firing of all materials in one single-step, and reduction of production costs due to the high possible degree of automation. But, co-firing of promising oxide thermoelectric materials, Ca3Co4O9 (p-type) and CaMnO3 (n-type), is very challenging due to the large difference in sintering temperature (300 K).
In this work we show the material development of Ca3Co4O9, CaMnO3, and insulation for multilayer generators co-fired under uniaxial pressure at 900 °C. The materials are tailored regarding their sintering behavior, electrical performance and coefficients of thermal expansion. Tape-casting and pressure assisted sintering are applied to fabricate textured Ca3Co4O9. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10 and the power factor by the factor of 20. The combination of sintering additives and uniaxial pressure is used to decrease the sintering temperature of CaMnO3 to 900 °C while maintaining acceptable thermoelectric properties.
Different generator designs (unileg and pn-type) were fabricated and analyzed regarding microstructure and thermoelectric performance. A lower level of complexity is beneficial for co-firing and performance. The unileg demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%).
Glass fiber reinforced polymer (GFRP) materials in practical applications have to endure cyclic mechanical loading in a wide temperature range (e.g. aircraft applications, automotive, wind turbine blades). In this study the static strength and fatigue behavior of GFRP was investigated in a temperature range from 213 K to 343 K. Therefor the coefficients of thermal expansion of the composite as well as the matrix are measured in this temperature interval. The inverse laminate theory was extended and used to calculate the inter fiber-failure effort for a virtual UD-layer according to the layer wise strength approach. The experimentally determined results are compared with the micro-mechanical model according to Krimmer, which has been enhanced to include the effect of temperature and fiber-perpendicular failure modes. A correlation between matrix effort, the dilatational strain energy of the matrix and the damage state of the specimen is demonstrated. It is shown that a fatigue life assessment can be performed with the aid of a temperature-independent master fatigue curve, as it was similar done for the fatigue behavior of CFRP and GFRP to very high load cycles at room temperature.
Dissolved water decisively influences numerous thermally activated relaxation phenomena in glasses like stress relaxation, sub-critical crack growth, internal friction, viscosity, sintering, and crystallization. Thermoanalytical methods can essentially help for better understanding of these phenomena. The lecture introduces the Vacuum Hot Extraction method (VHE) and illustrates its possibilities for measuring water content, degassing and mobility. As another thermoanalytical method, the Dynamic Mechanical Themoanalysis (DMA), allowing to study the effect of dissolved water on the internal friction in glasses, is introduced.
Due to their unique physico-chemical properties, nanoparticles are well established in research and industrial applications. A reliable characterization of their size, shape, and size distribution is not only mandatory to fully understand and exploit their potential and develop reproducible syntheses, but also to manage environmental and health risks related to their exposure and for regulatory requirements. To validate and standardize methods for the accurate and reliable particle size determination nanoscale reference materials (nanoRMs) are necessary. However, there is only a very small number of nanoRMs for particle size offered by key distributors such as the National Institute of Standards and Technology (NIST) and the Joint Research Centre (JRC) and, moreover, few provide certified values. In addition, these materials are currently restricted to polymers, silica, titanium dioxide, gold and silver, which have a spherical shape except for titania nanorods. To expand this list with other relevant nanomaterials of different shapes and elemental composition, that can be used for more than one sizing technique, we are currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance for the material and life sciences.
The relaxation of macroscopic residual stresses in laser powder bed fused stainless steel 316L
(2021)
The processing of stainless steel 316L using the additive manufacturing process Laser Powder Bed Fusion (LPBF) can widen its field of application due to a strong increase in Yield strength, without making major compromises on the ductility nor its outstanding corrosion and oxidation properties. Furthermore, improved designs that either reduce the weight or optimise the function of a part can be obtained using LPBF. These benefits are however counterbalanced by the proneness of LPBF to inducing high Residual Stresses (RS) during manufacturing. The characterisation and monitoring of these RS are of paramount importance for the wider acceptance of the LPBF process. This study focuses on the relaxation of the initial macroscopic RS present in an LPBF 316L as-built prism that undergoes various routes of manufacturing steps to achieve different specimen geometries and stress relieving treatments. The RS are determined using Angle-Dispersive (AD) and Time-of-Flight (TOF) neutron diffraction. The results reveal high tensile RS close to the surfaces and compressive RS near the centre of the as-built parts. The reduction in size and change of geometry heavily impact the stress ranges of the remaining RS, with lower stress ranges in cylindrical shaped compared to rectangular shaped specimens. Also, the application of different stress relieving heat treatments showed that heat-treating temperatures above 800 °C are necessary to obtain a strong relaxation in LPBF 316L.
The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al.
In this study, the influence of aging and mean stress on fatigue of the aluminium-alloy EN AW-2618A is investigated. Therefore axial fatigue tests are carried out on smooth specimens. The experiments show that the fatigue life decreases with increasing mean stress. Furthermore, the tests with the overaged specimens demonstrate that the number of cycles to failure is decreasing with increasing aging time.
Sulfur and water have a fundamental impact on the corrosion rate and potential failure of materials. It is therefore necessary to understand the mechanisms, rates, and potential means of transport, as well as the reactions of these elements with an alloy. This work investigates the effect of water vapor in the initial stages of SO2 corrosion of an ferritic model alloy containing 9 wt% Cr and 0.5 wt% Mn.
The exposure experiments were studied at 650°C in situ under laboratory conditions using energy-dispersive x-ray diffraction analysis. Two separate experiments were run, one with a 99.5% Ar + 0.5% SO2 atmosphere and one with a 69.5% Ar + 0.5% SO2 + 30% H2O atmosphere. With a wet atmosphere, the alloy formed a scale with decreasing oxygen content towards the scale–alloy interface. Sulfides were identified above and below a (Fe, Cr)3O4 layer in the inner corrosion zone. In contrast to this, the overall scale growth was slower in a dry SO2 atmosphere.
As more industrial interests focusing on using salt caverns and repurposed gas or petroleum reservoirs for alternative fuel storage, i.e. CO2/H2, the question raises whether microorganisms may impact the infrastructure, gas purity and storage condition over time.
Environments with high salinity (> 1.5 Meq of NaCl) are resided by halophiles (salt-loving microorganisms). To compensate for the intensive osmotic stress, they have resorted to two main adaptation strategies: 1) production of compatible solutes and 2) accumulation of intracellular KCl. Microbial community analysis of several high salinity environments revealed a number of recurring genera, including Halomonas and Halanaerobium. However, the impact of halophiles on the overall integrity and stability of the storage facilities remain largely unknown.
To evaluate the suitability and stability of saline storage facilities, several model halophilic microorganisms, such as members of Halomonas, will be selected as testing subjects. First, the impact of halophiles on the infrastructure will be determined using an integrative approach by combining a number of techniques, including electrochemistry, TOF-SIMS, SEM/FIB/EDS and FIB-TEM. Second, the abilities of halophiles to alter the fuel composition (i.e. increase/decrease the fractions of H2) will be monitored using gas chromatography by growing them under high pressure.
As a result of climate change and the accompanying mandatory shift to renewable energy resources, microorganisms will continue to play an important role in the energy sector, both to their benefit and detriment. Thus, it is important to achieve a certain level of understanding regarding the activities and mechanisms of halophiles prior to large-scaled excursions.
Wind turbine rotor blades commonly fail before their projected 20-year lifespan largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production. A potential repair alternative to restoring the mechanical properties of such lightweight fiber reinforced polymer (FRP) structures is to locally patch these areas with scarf joints. This type of repair allows for a smoother load distribution across the joint, and is favored especially on structures where minor aerodynamic contour changes are key. The effects of such repairs on the structural integrity, however, is still largely unknown. Building upon an understanding of the static load failure mechanism of GFRP scarf joints, presented at the ICCS23 Joint Event in 2020, the influence of the fiber orientation mismatch between parent and repair materials of 1:50 scarf joints on the failure mechanism of monolithic glass FRP specimens under cyclic fatigue load were examined in this study. Specimens with various layups were produced with the vacuum-assisted resin infusion (VARI) process using biaxial E-glass non-crimp fabric (NCF). The patch layers were then joined directly to the parent structure with the VARI using biaxial E-glass NCF with half the areal weight of the parent side to allow for better drapability. This mimics the soft-to-hard patch style utilized in wind turbine blade shell field repairs. The specimens were tested under uniaxial fatigue load, during which they were periodically monitored for damage onset. A comparison of the +45/-45° and 0/90° layups allowed for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. In addition to the tensile strength and stiffness property recovery assessment, a grayscale analysis using in-situ camera images determined the damage state leading to failure in each region across the scarf joint, which varied in the parent material versus scarf joint region, providing insight to the critical regions in this composite structure under cyclic loading.
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable materials data space is therefore crucial in the digital transformation of an industrial branch.
A great challenge in establishing a materials data space lies in the complexity and diversity of materials science and engineering. It must be able to handle data from different knowledge areas over several magnitudes of length scale.
The Platform MaterialDigital (PMD) is expected to network a large number of repositories of materials data, allowing the direct contact of different stakeholders as materials producers, testing labs, designers and end users. Following the FAIR principles, it will promote the semantic interoperability across the frontiers of materials classes. In the frame of a large joint initiative, PMD
works intensively together with currently near 20 research consortia in promoting this exchange (www.material-digital.de).
In this presentation we will describe the status of our Platform MaterialDigital. We will also present in more detail the activities of GlasDigital, one of the joint projects mentioned above dealing with the digitalization of glass design and manufacturing.
(https://www.bam.de/Content/EN/Projects/GlasDigital/glasdigital.html)
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable
materials data space is therefore crucial in the digital transformation of an industrial branch.
A great challenge in establishing a materials data space lies in the complexity and diversity of materials science and engineering. It must be able to handle data from different knowledge areas over several magnitudes of length scale.
The Platform MaterialDigital (PMD) is expected to network a large number of repositories of materials data, allowing the direct contact of different stakeholders as materials producers, testing labs, designers and end users. Following the FAIR principles, it will promote the semantic
interoperability across the frontiers of materials classes. In the frame of a large joint initiative, PMD works intensively together with currently near 20 research consortia in promoting this exchange (www.material-digital.de).
In this presentation we will describe the status of our Platform MaterialDigital. We will also present in more detail the activities of GlasDigital, one of the joint projects mentioned above dealing with the digitalization of glass design and manufacturing.
(https://www.bam.de/Content/EN/Projects/GlasDigital/glasdigital.html)
Texturing of calcium cobaltite for thermoelectric applications by pressure assisted sintering
(2021)
Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite (CCO) is considered as a promising thermoelectric p-type oxide for energy harvesting applications at temperatures above 500 °C. The properties and morphology of single-crystal CCO are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties of the grains can be assigned to the poly-crystalline parts.
In this study, the combination of tape casting and pressure-assisted sintering is used to texture and densify large scale components (50 cm²). Thereby, the influence of powder preparation and applied pressure during sintering on texturing and thermoelectric properties is investigated.
The analysis of XRD pole figures revealed that tape casting already leads to highly textured CCO. By pressure variation during sintering, the microstructure of CCO can be tailored either toward maximum power factor as required for energy harvesting or toward maximum figure of merit as required for energy recovery. Low pressure lead to a porous microstructure and maximum figure of merit and higher pressure to full densification and maximum power factor. The electrical and thermal conductivity of CCO seem depending on both texture and sinter density.
Additive manufacturing methods such as laser powder bed fusion (LPBF) allow geometrically complex parts to be manufactured within a single step. However, as an aftereffect of the localized heat input, the rapid cooling rates are the origin of the large residual stress (RS) retained in as-manufactured parts. With a view on the microstructure, the rapid directional cooling leads to a cellular solidification mode which is accompanied by columnar grown grains possessing crystallographic texture. The solidification conditions can be controlled by the processing parameters and the scanning strategy. Thus, the process allows one to tailor the microstructure and the texture to the specific needs. Yet, such microstructures are not only the origin of the mechanical anisotropy but also pose metrological challenges for the diffraction-based RS determination. In that context the micromechanical elastic anisotropy plays an important role: it translates the measured microscopic strain to macroscopic stress. Therefore, it is of uttermost importance to understand the influence of the hierarchical microstructures and the texture on the elastic anisotropy of LPBF manufactured materials.
This study reveals the influence of the build orientation and the texture on the micro-mechanical anisotropy of as-built Inconel 718. Through variations of the build orientation and the scanning strategy, we manufactured specimens possessing [001]/[011]-, [001]-, and [011]/[111]-type textures. The resulting microstructures lead to differences in the macroscopic mechanical properties. Even further, tensile in-situ loading experiments during neutron diffraction measurements along the different texture components revealed differences in the microstrain response of multiple crystal lattice planes. In particular, the load partitioning and the residual strain accumulation among the [011]/[111] textured specimen displayed distinct differences measured up to a macroscopic strain of 10 %. However, the behavior of the specimens possessing [001]/[011]-and [001]-type texture was only minorly affected. The consequences on the metrology of RS analysis by diffraction-based methods are discussed.
With this presentation, the push-out technique is explained. The focus of the experimental work is on the characterization of the fiber-matrix interface of short fiber reinforced composites. The reinforcing component was glass fibers and the matrix polymer was PA6.6 and PPA.
It is demonstrated for the first time that the push-out technique ca be applied on injection molded short fiber PMC and is sensitive to the mechanical interface properties. Further studies are planned on the influence of multiple processing, the temperature and humidity.
Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) should contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications.
Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused.
Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) is supposed to contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications.
Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts within the joint project PMD in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused. Furthermore, the presentation includes a live demonstration of queries possibly performed to query data that was uploaded in the PMD triple store.
Extensometer sind seit Jahrzehnten im Einsatz und bilden die Basis für eine präzise Dehnungsmessung in werkstoffmechanischen Versuchen. Jedoch ist die Temperaturstabilität von Extensometern häufig noch nicht ausreichend beachtet worden, um Fehler verursacht durch Temperaturschwankungen zu minimieren. Dieses wird derzeit nicht nur in Deutschland, sondern auch international zunehmend diskutiert. Datenblätter von Extensometern sind teils unvollständig besonders hinsichtlich von Temperatureinflüssen. Extensometer für den Einsatz bei höheren Temperaturen sollen z.B. laut Normen für dehnungsgeregelte Ermüdungsversuche mit Luft oder Wasser aktiv gekühlt werden. Jedoch schreiben die Normen keine Temperatur-Toleranzen für Extensometer vor. Dehnungsfehler verursacht durch Temperaturschwankungen am Extensometer bleiben meist verborgen, da die Temperatur des Extensometers standardmäßig gar nicht gemessen wird. Die Ursache von Einflüssen zur Temperaturstabilität von Extensometern wird erläutert. Ein einfaches Rechenbeispiel zeigt die Empfindlichkeit von Extensometern gegenüber Temperaturschwankungen und die Auswirkungen auf den Dehnungsfehler. Lösungsmöglichkeiten zur Optimierung werden aufgezeigt. Der Anwender von Extensometern soll sensibilisiert werden, um der Temperaturstabilität von Extensometern sowohl hinsichtlich Herstellerspezifikationen als auch bei der Anwendung von Extensometern im Prüflabor mehr Aufmerksamkeit zu schenken, um letztlich die Qualität von Versuchsergebnissen zu verbessern. Empfehlungen an Extensometerhersteller werden formuliert. Dieses Thema wird zukünftig auch in Prüfnormen mehr Aufmerksamkeit geschenkt werden. Es werden Maßnahmen zur Verbesserung der Temperaturstabilität von Extensometern Einzug in Prüfnomen finden, um letztlich verlässlichere Versuchsergebnisse zu erhalten. Es ist beabsichtigt, eine Verbesserung der Temperaturstabilität von Extensometern z.B. bei der nächsten Revision der Prüfnormen ISO 12106 und ISO 12111 für dehnungsgeregelte LCF- und TMF-Versuche zu berücksichtigen.
Ceramic springs combine attractive properties for applications in machinery, metrology, and sensor technology. They are electrically insulating, non-magnetic, provide a linear stress-strain behavior, and are stable at high temperatures and in corrosive environments. Generally, the precise dimensioning of a ceramic spring with respect to the spring constant is challenging. Different models are described, but many of these calculations do not match the actual spring properties. We demonstrate a reliable approach for the dimensioning and manufacturing of helical compression springs with a rectangular winding cross-section. Based on the German standard DIN 2090, which is referring to metallic springs, the spring constant can be calculated based on shear modulus, diameter, height, widths, and number of windings. Different ceramic springs were produced by milling of sintered hollow cylinders of zirconia, alumina and silicon nitride. The experimental spring constants are in very good agreement with the calculated values. Spring constants of zirconia springs were varied over three orders of magnitude between 0.02 N/mm and 5 N/mm by purposeful adaption of the spring geometry. The combination of dimensioning based on DIN 2090 and precise hard machining offers a reliable technology for the fabrication of tailored ceramic springs for special applications.
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with light into the volume of a ceramic powder compound, its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP), and other volumetric methods for the additive manufacture of filigree structures within the volume of ceramic slurries.
Recherche verschiedener jeweils nationaler/internationaler Regelwerke
und Prozeduren für die Systematische Schadensanalyse
• Literaturrecherche zu Methoden der systematischen interdisziplinären Schadensanalyse
• Vergleich der Regelwerke VDI 3822, ASTM, ASM sowie der Methoden
• Anwendung der Regelwerke/Prozeduren und Methoden am Beispiel
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. For silicate glasses we found a good correlation between the calculated surface energy of crystal faces and oriented surface nucleation. Surface energies were estimated assuming that crystal surfaces resemble minimum energy crack paths along the given crystal plane. This concept was successfully applied by Rouxel in calculating fracture surface energies of glasses. Several oriented nucleation phenomena can be herby explained assuming that high energy crystal surfaces tend to be wetted by the melt. This would minimize the total interfacial energy of the nucleus. Furthermore, we will discuss the evolution of the microstructure and its effect on the preferred crystal orientation.
Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Corresponding phenomena are discussed hypothetically or even controversial, and related studies are restricted to very few glasses. In this talk the state of the art on mechanisms of surface nucleation are summarized. On one hand, mechanical damaged surfaces show high nucleation activity, at which the nucleation occurs at convex tips and edges preferentially. On the other hand, solid foreign particles are dominant nucleation sites at low damaged surfaces. They enable nucleation at temperatures even far above Tg. The nucleation activity of the particles is substantially controlled by their thermal and chemical durability. But no systematic studies on initially oriented crystal growth or nucleation from defined active nucleation sites have been pursued, so far. Therefore, the main objective of a just started project is to advance the basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. We shall answer the question whether preferred orientation of surface crystals is the result of oriented nucleation or caused by other orientation selection mechanisms acting during early crystal growth. In both cases, crystal orientation may be caused by the orientation of the glass surface itself or the anisotropy and orientation of active surface nucleation defects. As a first attempt we focused on possible reorientation of separately growing surface crystals during early crystal growth. First results show clear evidence that separately growing crystals can reorient themselves as they are going to impinge each other.
A summery of previous research regarding surface crystallization is given as well as results regarding thecurrent DFG project are presented.
Overview about the surface initiated microstructure formation in glass surfaces. Samples which are exposed to a temperature treatment, can develop a crystalline microstructure above Tg at the surface. These separated crystals can be preferably oriented towards the surface of the sample. First experiments about the origin of these orientation phenomenon as well as the potentially causing mechanisms are presented and discussed within the presentation.
Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited. (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv).
Corrosion rates increase with increasing water content.
(0.2 – 20 mm/a).
Condensation of acids and therefore droplet formation is always possible, even at low water contents.
A low SO2 content within the CO2-stream might be more important than a low water content.
Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications.
Low alloyed steels showed better corrosion behavior. (predictable uniform corrosion)
For direct contact with saline aquifer fluids only high alloyed steels shall be used.
Ambient water influences sub-critical crack growth (SCCG) from microscopic surface flaws, leading to stress corrosion at the crack tip. The complex influence of humidity accelerating slow crack propagation (region I) is well studied only for dry commercial NCS glass (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG water-bearing glasses. For this purpose, water-bearing silicate glasses of 8 wt% total water were synthesized at 0.5 GPa and compared to dry glasses. SCCG was measured in double cantilever beam geometry. For dry glasses, 3 trends in crack velocity vs. stress intensity, KI, curve were found. The slope in region I increases in the order NCS < NBS < BaCS < NZnS < NAS glass. The velocity range of region II, reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among these glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam0.5. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg internal friction peak caused by molecular water, and makes the glasses more prone to SCCG. The observed trends will be discussed in terms of the effects of Youngs Modulus on the strain energy release rate and energy dissipation related to mechanical glass relaxation phenomena.
Environmental conditions are known to influence sub-critical crack growth (SCCG) that are released from microscopic flaws at the glass surface, leading to stress corrosion phenomena at the crack tip. The processes at the crack-tip are complex and water has been identified as a key component governing SCCG at low crack velocities (region I). In particular, the influence of humidity accelerating crack propagation is well studied for industrial soda-lime silicate glasses, which are practically free (< 1000 ppm) of dissolved water. To shed light on the corrosion process, the situation at the crack-tip is reversed in the present study as dissolved water in larger fractions is present in the glass and crack propagation is triggered in dry environment. For this purpose, water-bearing silicate glasses of up to 8 wt% total water were synthesized in an internally heated pressure vessel at 0.5 GPa and compared to dry glasses of standard glass manufacturing. SCCG was measured using the double cantilever beam technique and by Vickers indentation. For dry glasses, three trends in the crack growth velocity versus stress intensity curve were found. The slope in region I limited by environmental corrosion increases in the order sodium aluminosilicate < sodium borosilicate ≲ sodium lead silicate. The velocity range of region II reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For hydrous glasses, it is found that those of low Tg are more prone to SCCG. As water strongly decreases Tg, it promotes SCCG. First results indicate that molecular water has a dominating influence on SCCG.
Environmental conditions are known to influence sub-critical crack growth (SCCG) that starts from microscopic flaws at the glass surface, leading to stress corrosion phenomena at the crack tip. The processes at the crack tip are complex and water has been identified as a key component governing SCCG at low crack velocities (region I). In particular, the influence of humidity accelerating crack propagation is well studied for dry industrial soda-lime silicate glasses (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG in water-bearing glasses. For this purpose, water-bearing silicate glasses of up to 8 wt% total water were synthesized in an internally heated pressure vessel at 0.5 GPa and compared to dry glasses. SCCG was measured using the double cantilever beam technique. For dry glasses, three trends in the crack growth velocity versus stress intensity, KI, curve were found. The slope in region I, limited by environmental corrosion, increases in the order soda-lime silicate < sodium borosilicate < barium calcium silicate < sodium zinc silicate < sodium aluminosilicate glass. The velocity range of region II, reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among these glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg relaxation peak caused by molecular water, and makes the glasses more prone to SCCG. The observed trends will be discussed in terms of the effects of Youngs Modulus on strain energy release rate and energy dissipation related to glass relaxation phenomena.
Study of Polyaniline/Silicon Dioxide based Coating on Carbon Steel in Artificial Geothermal Brine
(2021)
By using the available resources in Indonesia, such as silicon dioxide and marine coating base, the PANI/SiO2 modified alkyd coating was able to protect carbon steel in a deaerated artificial geothermal water. The screening of coatings shows that the modification by adding individual pigment was not sufficient to protect carbon steel even during a short-term exposure, indicated by the discoloration after only seven days of exposure. Electrochemical tests indicated that there was no significant change in the Ecorr between the coated and uncoated carbon steel at room temperature. At 150 °C, the coated carbon steel has a lower potential than that of carbon steel, indicating that the coating is protecting carbon steel cathodically or slowing down the corrosion reaction. Finally, a long-term exposure test confirmed that the PANI/SiO2 modified coating successfully protects the carbon steel in the Sibayak artificial geothermal water up to 150 °C for 6 months.
Lock-in- and flash thermography are standard methods in active thermography. They are widely used in industrial inspection tasks e.g. for the detection of delaminations, cracks or pores. The requirements for the light sources of these two methods are substantially different. While lock-in thermography requires sources that can be easily and above all fast modulated, the use of flash thermography requires sources that release a very high optical energy in the very short time.
By introducing high-power vertical cavity surface emitting lasers (VCSELs) arrays to the field of thermography a source is now available that covers these two areas. VCSEL arrays combine the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination range of flash lamps or LEDs and can thus potentially replace all conventional light sources of thermography.
However, the main advantage of this laser technology lies in the independent control of individual array areas. It is therefore possible to heat not only in terms of time, but also in terms of space. This new degree of freedom allows the development of new NDT methods. We demonstrate this approach using a test problem that can only be solved to a limited extent in active thermography, namely the detection of very thin, hidden defects in metallic materials that are aligned vertically to the surface. For this purpose, we generate destructively interfering thermal wave fields, which make it possible to detect defects within the range of the thermal wave field high sensitivity. This is done without pre-treatment of the surface and without using a reference area to depths beyond the usual thermographic rule of thumb.
The main deference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which moves from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Investigation of temperature dependent solid solution strengthening in single phase multicomponent alloys with medium and high entropy using creep testing was performed. Creep tests carried out on single phase SX CrCoNi , CrMnFeCoNi and pure Ni from 700 to 1200 °C excluding oxidation, grain boundaries and multiphase effects. It was found that the influence of solid solution strengthening of CrCoNi and CrMnFeCoNi increases by decreasing temperature (1200 to 700 °C), and dislocation forests occur in CrCoNi and CrMnFeCoNi in comparison to pure Ni.
Dry pressing of ceramic materials requires homogeneously soft granules with good flowability to allow rapid die filling and to avoid packing defects. Spray-drying granulation appears to be the best method for obtaining granules with high flowability in industrial scale. But, strength reducing internal microstructural defects caused by spray-dried granules with hollow and hard shells are often observed using nano and/or multi-component starting powders.
Using the example of a ZTA composite, the potential of slurry optimization, ultrasound atomization and infrared drying for better granule properties and compaction behavior were investigated. Starting granules produced in a conventional spray dryer (Niro, Denmark) with a two fluid nozzle showed typical defects like large central pores and dimples.
The early step of slurry preparation already possesses an essential optimization possibility in the form of stability adjustments. Granule compaction was clearly improved upon a specific reduction in slurry stability. The second optimization opportunity to improve the granule quality was the atomization step. Implementation of an ultrasound atomizing unit into the conventional spray dryer positively affected granule size distribution and therefor flowability and as well granule yield. But, a combination of both process optimizations delivered the best sinter bodies with highest density and strength due to further reduction in maximum size and fraction of pores.
As last step of a spray drying process, the drying is the focus of further investigations. A current setup implying a spray dryer prototype utilizes stacked infrared heater in a countercurrent setup delivering a further increase in granule yield and enduring spraying process stability.
Ziel von fraktographischen Untersuchungen ist die Auswertung von makroskopischen und mikroskopischen Bruchflächenmerkmalen und daraus resultierend die Bestimmung des Bruchmechanismus eines Bauteils aus einem Schadensfall. Die Grundlage für die Bewertung von Bruchmerkmalen stammt dabei aus zuvor durchgeführten eigenen Vergleichsversuchen und aus der Literatur. Eine fraktographische Analyse kann sehr aufwändig sein und setzt in jedem Fall erhebliches Erfahrungswissen voraus. Im IGF-Vorhaben „iFrakto“ wird Software entwickelt, die auf Basis von digitalisiertem Expertenwissen, Machine Learning und unter Zuhilfenahme von Topographie-Daten anhand von REM-Aufnahmen Bruchmerkmale und Bruchmechanismen quantitativ bestimmt, s. Abbildung. Solche Software soll mittelfristig direkt am REM oder bei der nachfolgenden Auswertung wissensbasierte Vorschläge für die Bewertung von Bruchflächen liefern. Als Grundlage hierfür wurden Ringversuche unter Fraktograph/inn/en durchgeführt, um die Wissensbasis zu schaffen, die praxisrelevanten Anforderungen an solche Software abzufragen und erste Praxistests durchzuführen. Die bisherigen Ergebnisse werden vorgestellt und die Relevanz der Auswertestrategie und unterschiedlicher Sensordaten bewertet.
Efficient studies of scarce or expensive materials require material saving processes. Therefore, a high yield concept for small batch preparation of ready-to-press powder is exemplarily presented for yttria stabilized nano-zirconia (d50 < 50 nm).
The concept involves small batch preparation in an ultrasound resonator, dispersant selection based on zeta potential measurements, evaluation of slurry stability using an analytical centrifuge, and preparation of ready-to-press powder by freeze drying.
Freeze drying offers key advantages. Process efficiency and high yield above 95 % are independent of sample size. The dried product does not require further mechanical treatment like milling or grinding. Side effects like migration of additives are avoided.
An optimized freeze drying process tolerates slurries with moderate stability. Thus, efforts for slurry development can be reduced. Generally, identifying a suitable dispersing agent requires only 3-5 zeta potential measurements. Slurry stability is rechecked using an analytical centrifuge, which also accounts for steric stabilization. An ultrasound resonator is used to disperse the powder without contamination, which becomes critical for small batches.
The described route is exemplarily presented for the development of an additive recipe for nano-sized zirconia powder, targeting for good pressing behavior and high green density. Therefore, a variety of binding and lubricating agents were tested.
Following the presented route, 80 g zirconia powder were sufficient to conduct a study including slurry development and five sample sets with varying composition, each set comprising five discs (d = 20 mm and h = 2 mm).
Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductive and osteoinductive properties. However, resorption of modern materials for bone grafting (hydroxyapatite (HA) and tricalcium phosphate (TCP)) is reported, in some cases, to be not enough, this is why the search for more soluble compounds compared to HA and TCP looks very perspective. A possible way to increase ceramics solubility leads to partial substitution of Ca2+ -ions in Ca3(PO4)2 by alkali cations, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as the increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in the sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making the study of sintering of the ceramics mentioned above highly important.
To control Ca3(PO4)2 - CaKPO4 - CaNaPO4 based ceramic microstructure it is necessary to know possible phase transformations in the system and the way to manage microstructure by sintering schedule or sintering process.
In this work, an isothermal section for phase diagram of Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system is studied with several techniques. According to the XRD of quenched samples, this phase triangle has four single-phase areas at 1200˚C (Figure 1). It was shown that single-phase CaK0.6Na0.4PO4 cannot be sintered to full-dense ceramics by conventional sintering regardless time-temperature schedule. Two-step sintering technique, beneficial in the case of HA-ceramics, was unsuccessful in all cases of calcium-alkali phosphate compositions. However, field-assisted sintering techniques like, e.g. Spark Plasma Sintering (SPS), can overcome this problem due to significant impact on grain boundary diffusion. In connection with this fact, grains grow much slower retaining sintering process in a pore control regime. In this work CaK0.6Na0.4PO4 low-porous ceramics was also fabricated by FAST-methods of sintering. Moreover, other alternative sintering techniques, such as reaction sintering, may be useful in accelerating ions diffusion but stopping excessive grain growth.Strength properties of ceramics were evaluated by B3B-testing, micro- and nanoindentation techniques. Fracture toughness also becomes higher with potassium content increase, guiding porosity level.
Resorption properties of sintered ceramics were studied in different solutions with pH=5 and 7.4.
Acknowledgements. The research of sintering processes in calcium phosphate materials were funded by RFBR according to the research project № 18-33-00974.
Since decades electric contacts based on silver metallization pastes are key components of photovoltaics and advanced microelectronics. For the metallization of commercial Si solar cells, high conductive silver glass pastes are cost effectively applicated by screen printing. Nevertheless, silver pastes are still one of the most crucial and expensive none Si materials in solar cells. Ever shorter time to market as well as increasing demands on reduced Ag consumption and line width require the targeted development of silver-glass-pastes with increased sinter ability and electrical conductivity. As a main difficulty, however, the liquid phase sintering of silver glass pastes is poorly understood so far.
In the present study, the influence of different network modifier in alkali-zinc-borate paste glasses on liquid phase sintering of silver-glass-pastes was investigated. Low melting X2O-ZnO-B2O3 glasses with X = Na, Li and Rb (abbr. LZB, NZB, and RZB) were utilized to prepare silver-glass-composites containing 30 %Vol glass. Shrinkage behavior of the silver-glass-composites compared with that of pure silver and pure glass powder compacts was studied with heating microscopy. The powder compacts were uniaxially pressed and heated at 5 K/min to the glass softening temperature. Glass transformation temperature and viscosity of the glasses were respectively measured with dilatometry and rotational viscometry. The thermal behavior of the pure glasses was analyzed with thermal analysis. Additionally, the contact angle of glass on pure silver foil was determined by means of heating microscopy between room temperature and 830 °C.
Thermal analysis of the alkali-zinc-borate-glasses under study has shown transformation temperatures between 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB). For all glasses crystallization was found to start approximately at about 550 °C. However, different peak areas hint on a different degree of crystallization. Conformingly, the sintering behavior, measured in terms of area shrinkage, significantly differed for the silver-pastes under study. For silver-pastes with NZB or LZB-glass, sintering starts at 464 °C for NZB Ag pastes and at 451 °C for LZB Ag pastes and ends at 597 °C for NZB Ag paste and at 594 °C for LZB Ag paste. The sintering of the RZB Ag paste proceeds between 426 °C and 703 °C. The final densification was retarded possibly due to crystallization or swelling. The low sinter onset at 426 °C seems to correlate with the good wetting behavior of the RZB glass. Thus, the lowest apparent contact angle between the just densified powder compact sintered at a silver substrate was found for this glass. Moreover, microstructure analyses of the various composites indicate differences in silver dissolution and reprecipitation.
High conductive silver-glass-metallization-pastes are key components in photovoltaics and advanced microelectronics. However, the underlying mechanisms of liquid phase sintering as silver dissolution, diffusion and reprecipitation are poorly understood so far.
In the current work, the influence of different network modifier in alkali-zinc-borate paste-glasses on liquid phase sintering of silver-glass-composites was studied. Therefore, silver-glass-composites containing 30 vol% glass were prepared, using low melting X2O-ZnO-B2O3 glasses with X = Na, Li, and Rb (NZB, LZB, and RZB). Glass transition temperature, viscosity, glass-silver wetting, crystallization and sintering behavior was studied by means of thermal analysis, dilatometry, heating microscopy and microscopy.
Similar glass transition temperatures of 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB) were found by means of thermal analysis for glasses under study. Also, all glasses have a similar crystallization onset at about 550 °C, even though exhibiting with a different degree of crystallization.
Despite these similarities, however, the sintering behavior, measured in terms of area shrinkage, significantly differs for the composites. This finding indicates a different degree of silver dissolution. Assuming that dissolved silver reduces the viscosity, this effect could explain why glass crystallization starts at lower temperature in the composites. For example, the crystallization peak of LZB at 629 °C measured for pure glass powder compacts was decreased to 586 °C for the composite. Confirmatively, microstructure analyses indicate different degrees of silver dissolution, as e.g. revealed by different amount of silver precipitates within the residual glass phase, and reprecipitation. Best silver dissolution appeared for the RZB glass. Nevertheless, the final densification of RZB was retarded probably due to swelling and crystallization.
Today, more than 12% of the primary energy is lost in the form of waste heat. Thermoelectric generators (TEGs) can convert waste heat directly into electrical power by utilizing the Seebeck effect. The performance of such a generator is defined by a dimensionless figure of merit ZT of the thermoelectric pairs and the resistance R of the metallic contacts between these pairs. The figure of merit of thermoelectric oxides is considerably smaller compared to semiconductors. Still, thermoelectric oxides like calcium cobaltite (Ca3Co4O9) are attractive for applications at elevated temperatures in air. In contrast to the established π-type architecture of common TEGs, tape casting and multilayer technology may be applied for cost-effective manufacturing of oxide TEGs. Promising demonstrations of multilayer TEGs have been published in the last years. Still, the development of reliable and scalable manufacturing processes and proper material combinations is necessary. The aim of our project is to evaluate the feasibility of low temperature co-fired ceramics (LTCC) technology for a practical manufacturing of oxide multilayer TEGs of Ca3Co4O9 (p-type) and calcium manganate (CaMnO3, n-type). Ca3Co4O9 exhibits an undesired phase decomposition at 926 °C. Because of that, the application of sintering strategies and interconnect concepts well known from LTCC technology is a promising approach. We present results of pressure-assisted sintering of Ca3Co4O9 multilayer at 900 °C and axial pressures of up to 7.5 MPa. Ca3Co4O9 was produced by solid state reaction of CaCO3 and cobalt(II,III)oxide at 900 °C. Green tapes were prepared by a doctor-blade process, manually stacked and laminated by uniaxial thermocompression. Sintering was conducted in a LTCC sintering press between SiC setter plates. The thickness shrinkage was recorded by an in-situ technique. After sintering under 7.5 MPa, the microstructure of the single phase material shows a high density of 95 % and an advantageous alignment of the platelet grains. This results in good electrical conductivity and a comparatively high ZT of 0.018 at room temperature. However, the lowering of CaMnO3 sintering temperature from above 1200 °C to below 920 °C remains a challenge. To select a proper metal paste for interconnections of an oxide TEG, several pastes have been investigated regarding contact resistance of internal and external (soldered) connections in a preliminary study. Commercial pastes containing Ag, Au, Au/Pt, Ag/Pd, and Ag/Pd/Bi were manually applied and post-fired on sintered test bars of Ca3Co4O9 and CaMnO3 at 900 °C for 2 h. All tested pastes formed mechanically stable metallization after firing. For resistance measurement, 4-wire method and a custom-made probe head were used. The contacts on Ca3Co4O9 exhibit significantly (2-sample t-test, α = 5%) higher resistance compared to contacts on CaMnO3. Pure silver paste exhibits the lowest resistance for internal contacts on both materials, lower than 5 mΩ on CaMnO3. Ag/Pd/Bi paste resulted in conspicuously high variance of resistance. EDX analyses clarified an enrichment of Bi in the thermoelectric material near the interface and thereby the formation of an oxide layer with probably high electrical resistance. The thickness of that layer varies with the thickness of metallization. In conclusion, the use of Bi containing pastes is not advisable. Pure Ag paste shows the best results regarding resistance and solderability.
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites or glass bonded ceramics with properties and complex shape. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
The lecture focuses on the mechanisms of non-desired gas bubble formation and foaming during the sintering of glass powder compacts. It is shown that foaming is driven by carbon gases and that carbonates, encapsulated in micropores or mechaniacally dissolved beneath the glass surface, provide the major foaming source.
Single crystal superalloys usually contain pores of sizes 5-10 micro-m after casting and heat treatment. These pores can be reduced under compression by combined creep and diffusion in a subsequent treatment called Hot Isostatic Pressing (HIP). The paper presents a methodology to simulate pore shrinkage under HIP conditions in two dimensions (2D).
At the scale of the pores, which is also the scale of the sub-grains (<50 micro-m) the dislocation sources cannot be assumed to be homogeneously distributed. Thus, the applicability of classical crystal plasticity is questionable. In this case, the transport of dislocations under an applied stress from the location where they are nucleated must be explicitly modelled. This is done by solving the transport equations for the dislocation densities and the elasticity equations in 2D. The dislocations are assumed to be nucleated at Low Angle Boundaries. They glide or climb through the sub-grains with a stress dependent velocity.
The transport equations are solved by the Flux-Corrected Transport method, which belongs to the predictor-corrector class of algorithms. In the first step, an artificial diffusion is introduced, which suppresses spurious oscillations of the solution. In a second step, the solution is corrected in such a way that no additional extremes appear and that the extremes do not grow. The algorithm is validated by simulating the transport of simple distributions with a constant velocity field.
With the dislocation velocities and the computed dislocation densities, the inelastic shear rate at the slip system level is computed by integrating the Orowan equation. In the 2D-setting, three slip systems are considered. The contributions of these slip systems are summed up to obtain the total inelastic strain rate. Dislocation glide and climb and the coupling of climb with vacancies diffusion are considered.
The resolution of the equilibrium equations from the inelastic strains turned out to be prone to numerical instabilities. As an alternative, the stresses are directly computed from the distribution of geometrically necessary dislocations following the method presented in. The resulting boundary value problem is solved by the Least-Square Finite Element method.
Examples of simulations are presented for a representative region under creep tension and for a pore shrinking under external pressure.
Substitution of lead oxide in low-melting glasses, e.g., for application in silver metallization pastes, is a current research goal. This work is focused on the investigation of silver diffusion in alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb). In addition, the redox state of silver (Ag) and thus the type of diffusing silver species were studied. For this purpose, a metallic silver coating was applied on glass cubes by means of sputtering. Heat treatment of the samples was performed close to the glass transition temperatures at 470 °C for 2 h under air and nitrogen atmosphere. Coating thickness was 1.8 µm after heat treatment, measured by a white light interferometer.
Silver diffusion profiles were measured by means of secondary neutral mass spectrometry. The silver diffusion coefficients are in the range of ~10-14 cm2/s and indicate no significant differences depending on the type of alkali ions in the glass. Dissolved Ag+-ions and [Agm]n+-clusters in the glasses were differentiated using fluorescence spectroscopy.
Precipitated metallic silver particles in the sodium containing glass were observed by means of transmission electron microcopy. Their mean particle diameter was ~6 nm.
In many late-breaking research fields as in photovoltaics, microelectronics, nuclear waste glasses or at least mirror glasses silver diffusion in glasses is relevant to the issues of high-level functionality and recycling. The present study is focused on silver diffusion in innovative, low-melting alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) potentially usable for silver metallization-pastes in solar cells. The glasses were coated with a thin metallic silver layer and heat treatments in air and nitrogen close to Tg at 470 °C for 2 h were performed. After heat treatment under air and nitrogen atmospheres the coating thickness, measured by a white light interferometer, was about 1.8 µm thick. Silver depth profiles determined by means of secondary neutral mass spectrometry (SNMS) indicate the fastest silver diffusion to a depth of 3.5 µm for Li2O-ZnO-B2O3 (LZB) glass. Nevertheless, the influence of the different alkali ions on the silver diffusion is small. The oxygen availability determines the silver diffusion into the glasses. The oxygen promotes the oxidation of the silver layer enabling Ag+ to diffuse into the glass and to precipitate as Ag0. Both species were detected by x-ray absorption spectroscopy (XAS). The precipitated metallic silver particles in Na2O-ZnO-B2O3 (NZB) glass have a mean size of 5.9 nm ± 1.2 nm diameter, which was determined using transmission electron microscopy (TEM). Phase separation in zinc-rich and zinc-poor phases with a mean diameter of 75 nm ± 20 nm occurred in NZB glass after heat treatment. Ion diffusion of the glasses into the silver layer was suggested by EDX-line scans.
Network modifier ions can decisively influence properties and structure of low melting alkali-zinc-borate glasses and thus cause complex effects on the liquid phase sintering of silver-glass metallization pastes. This effect was studied for X2O-ZnO-B2O3 (X = Li, Na, Rb) glasses for silver-glass metallization pastes. Viscosity and the glass transition temperature, Tg, were measured with rotational viscometry and dilatometry. Dried model pastes with 30 vol% LZB, NZB or RZB glass were prepared for sintering studies by means of heating microscopy measuring the silhouette area shrinkage of uniaxially pressed powder compacts during heating at 5 K/min. For comparison, the silhouette area shrinkage of pure glass and silver powder compacts were determined. Glass-silver wetting was investigated during heating of bulk glass cylinders placed on silver substrates. Glass RZB turned out to have the lowest viscosity among the glasses under study. Its glass transformation temperature, Tg, was found at 444 °C and it caused the lowest sintering onset for its glass and paste powder compacts. Slightly increased values of Tg were found for NZB and LZB (468 °C and 466 °C, respectively) and a slightly retarded sintering was found for both paste powder compacts. These results indicate that liquid phase sintering of silver-glass pastes under air atmosphere is mainly influenced by glass viscosity.