5 Werkstofftechnik
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Sand erosion of solar glass: Specific energy uptake, total transmittance, and module efficiency
(2018)
Surface roughness, R Z , normal transmittance, Τ N , total transmittance, Τ T , and photovoltaic (PV) module efficiency, η S , were measured for commercial solar glass plates and PV test modules identically sandblasted with different loads of quartz sand (200 – 400 μ m), impact inclination angles, and sand particle speed. Measured data are presented versus the specific energy uptake during sand blasting, E (J/m2). Cracks, adhering particles, and scratch ‐ like textures probably caused by plastic flow phenomena could be observed after sand blasting. Their characteristic size was much smaller than that of sand particles.
After blasting and subsequent cleaning, the glass surface was still covered with adhering glass particles. These particles, cracks, and scratch ‐ like textures could not be removed by cleaning. For sand blasting with α = 30° inclination angle and E = 30 000 J/m2, normal transmittance, total transmittance, and relative module efficiency decreased by 29%, 2% and ∽ 2%, respectively. This finding indicates that diffusive transmission of light substantially contributes to PV module efficiency and that the module efficiency decrease caused by sand erosion can be better estimated from total than by normal transmittance measurements.
Borosilicate glasses (16Na2O–10B2O3–74SiO2, NBS) with water contents up to 22 mol% H2O were prepared to study the effect of water on structural relaxation using DTA, viscometry and internal friction measurements. The results show that the glass transition temperature Tg of DTA and the isokom temperature T12, of viscometry are in excellent agreement, confirming the equivalence of enthalpy and viscous relaxation for NBS glass. Combining Tg data with water speciation data demonstrates that OH groups are mainly responsible for the decrease of Tg with increasing hydration, while molecular water plays only a minor role. Internal friction spectra at 7.125 Hz confirm the decisive influence of water on mechanical relaxation. The temperature range of α-relaxation (glass transition) strongly decreases while two β-relaxation peaks (sub-Tg) progressively appear with increasing water content. A high temperature β-relaxation peak, attributed to the presence of OH groups, shifts from 670 to 450 K as total water content increases from 0.01 to 5 wt%. A low temperature β-relaxation peak, attributed to molecular water, appears at 380 K and 330 K in glasses containing 3 and 5 wt% H2O, respectively. These findings suggest that relaxation mechanism of different hydrous species at low temperature may contribute to fatigue of stressed glasses.
Sintered bioactive glass scaffolds of defined shape and porosity, e.g. made via additive manufacturing, must provide sufficient bioactivity and sinterability. As higher bioactivity is often linked to high corrosion and crystallization tendency, a certain compromise between sintering ability and bioactivity is therefore required. Groh et al. developed a fluoride-containing bioactive glass (F3), which allows fiber drawing and shows a bioactivity well comparable to that of Bioglass®45S5.
To study whether and to what extent the sinterability of F3 glass powder is controlled by particle size, coarse and fine F3 glass powders (300-310µm and 0-32µm) were prepared by crushing, sieving and milling. Sintering, degassing and phase transformation during heating were studied with heating microscopy, vacuum hot extraction (VHE), DTA, XRD, and SEM.
For the coarse glass powder, sintering proceeds slowly and is limited by surface crystallization of primary Na2CaSi2O6 crystals. Although the crystallization onset of Na2CaSi2O6 is shifted to lower temperature, full densification is attained for the fine powder. This finding indicate that certain porosity might be tuned via particle size variation. Above 900°C, intensive foaming is evident for the fine powder. VHE studies revealed that carbon species are the main foaming source.
A novel method to generalize kinetic data of viscous crack healing in glasses is proposed. The method assumes that crack healing progress is proportional to the healing time, t, and indirect proportional to viscosity, n. This way, crack length and crack width data, normalized to the initial crack length and plotted versus t/n, allow to compare crack healing progress for different cracks and healing temperatures in a master curve. Crack healing experiments conducted in this study demonstrate the applicability of this method for a commercial microscope slide glass.
Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Statistical analysis of Vickers induced subcritical crack growth in soda-lime silicate glasses
(2018)
Studies on Vickers induced subcritical crack growth are controversially discussed since the stresses that drive the crack growth are distributed three dimensionally within the material and cannot be retraced by available methods. Hence, empirical approaches are used to calculate mechanical material parameters such as the stress intensity factor KI. However, the results of these approaches show large deviations from those measured by standardized techniques such as double cantilever beam (DCB) or double cleavage drilled compression (DCDC). Yet, small specimen sizes and low specimen quantities can prevent the execution of DCB and DCDC measurements. Here we present an approach that is based on a statistical analysis of Vickers induced radial cracks. For this purpose more than 150 single radial cracks were analyzed. The cracks were generated in a commercial soda-lime silicate glass. The experiments were performed in a glovebox purged with dry nitrogen gas to minimize the influence of atmospheric water on crack growth. The temporally resolved evolution of the radial cracks was monitored in-situ using an inverted microscope equipped with a camera system directly below the Vickers indenter. An automated image analysis software was used to determine the crack length over time. The data show that the crack propagation and thereby the crack velocities are not uniformly but statistically distributed. These findings allow, using the statistical mean value of the distributions in combination with DCB data, a precise formulation of KI for each measured crack length.
The presence of water in the surrounding atmosphere of a propagating crack has a major influence on the subcritical crack growth. While these external phenomena are well understood, there is still a lack of knowledge on the influence of structurally bound water on crack propagation. Thus, our recent study aims on the analysis of crack propagation in water bearing soda-lime silicate glasses with up to 8 wt.% water. The samples were synthesized in an internally heated pressure vessel at 0.5 GPa. Since this preparation route limits the sample sizes, standard test geometries allowing for the determination of stress intensity factors, such as double cantilever beam, are not feasible. Thus, radial cracks in the hydrous glasses were initiated by Vickers indentation and crack growth was simultaneously captured with a camera system. An automated image analysis algorithm was used for the analysis of the crack length of each single video frame. To minimize influences by atmospheric water, all experiments were conducted in a glovebox purged with dry N2. About 150 cracks per glass composition were analyzed to provide statistical significance of the Vickers-induced SCCG. The results show that structurally bound water has a major influence on SCCG by means of crack lengths, growth rates and time of crack initiation.
Glasses with compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x= 0, 2, 4, 8) were prepared using a conventional melt quenching technique, and the crystallization behavior of ferroelastic β′-Gd2 MoO4)3 Crystals was examined to clarify the mechanism of self-powdering phenomenon and to design bulk crystallized glasses. It was found that the self-powdering phenomenon appeared significantly during the crystallization at temperatures near the crystallization peak temperature, but the phenomenon is suppressed in the crystallization at temperatures much higher than the glass transition temperature. It was also found that the substitution of TeO2 for B2O3 in the base glasses suppresses the self-powdering phenomenon and consequently bulk crystallized glasses were obtained in the glass with x=8 mol%. The densities at room temperature of the base glasses are d =4.755–4.906 g/cm3, being much higher than the value of d=4.555 g/cm3 for β′-Gd2(MoO4)3 crystal. It is proposed that the stresses in the inside of crystals induced by large density differences (i.e., large molar volume differences) between the glassy phase and crystals might be relaxed effectively in the glasses containing TeO2 with weak TeeO bonds and fragile character.
Der Vortrag gibt eine Einführung in die Methode der Vakuumheißextraktion und beschreibt die Anwendungsmöglichkeiten der an der BAMN betriebenen Anlage.
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.
Wasser in Silicatglas
(2018)
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 tailored mechanical, thermal, electrical and optical properties and complex shape. Its wide and precise adjustability makes this class of materials a key component for advanced technologies. Processing of glass or composite powders often allow even more flexibility in materials design. At the same time, however, processing can have substantial effects on the glass powder surface and sinterability. Thus, mechanical damage and surface contamination can strongly enhance surface crystallization, which may retard or even fully prevent densification. Whereas sintering and concurrent crystallization have been widely studied, partially as cooperative effort of the TC7 of the ICG, and although glass powder sintering is predominantly applied for glasses of low crystallization tendency, sintering is also limited by gas bubble formation or foaming. The latter phenomenon is much less understood and can occur even for slow crystallizing glass powders. The lecture illustrates possible consequences of glass powder processing on glass sintering, crystallization and foaming.
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.
All in all, practicing professionals as well as researchers can read this book with pleasure and great benefit. It presents a comprehensive collection of data and practical examples manifested in about 100 graphs, 80 schemes of processes and devices, a manifold of images showing the microstructure of alloys or details of components and several phase diagrams. Tables containing data on commercially available coatings, alloys, compositions of corrosive salts, function of constituents of coatings add further important pieces of information. Thus, this book is a valuable source of information for anyone engaged in work with or research on high temperature coatings.
Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C
(2018)
Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far.
For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide.
Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents.
In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS.
The hydrogen tightness of high-pressure hydrogen storage is a Basic criterion for long-term storage. The H2 permeation coefficients of epoxy resin and a glass lacquer were determined to enable the geometric optimization of a glass capillary storage. It was found that the curing conditions have no significant influence on the H2 permeation coefficient of resin.
The H2 permeation coefficient of epoxy resin is only about three orders of Magnitude greater than that of borosilicate glass. This suggests that the initial pressure of 700 bar takes about 2.5 years to be halved in capillary array storage. Therefore, a high-pressure hydrogen storage tank based on glass capillaries is ideally suited for long-term storage in mobile applications.
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.