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Topper, Brian; Tagiara, Nagia S.; Herrmann, Andreas; Kamitsos, Efstratios I.; Möncke, Doris
Yttrium and rare-earth modified lithium orthoborates: glass formation and vibrational activity. - In: Journal of non-crystalline solids, ISSN 0022-3093, Bd. 575 (2022), 121152

Glass formation and structure-property relations were explored in highly modified borate glasses containing high loads of rare-earth elements, whose crystalline analogues display a trigonal to tetrahedral borate phase transition (BO33- -> BØ2O23-, where Ø and O- indicate bridging and non-bridging oxygen atoms). The resulting borate networks are completely depolymerized, where borate anions are crosslinked to rare-earth and modifier cations via ionic bonds. The borate structure was found to be based on a single structural unit, BO33- triangles, whose fundamental vibrations are all active in both the Raman and infrared. The local environment of the rare-earth ions in orthoborate glasses was studied with far infrared spectroscopy and, in some cases, by using terbium as a probe ion. A linear correlation was obtained between the effective force constant in the far infrared and the field strength of the rare-earth cation.



https://doi.org/10.1016/j.jnoncrysol.2021.121152
Herrmann, Andreas; Tsekrekas, Elizabeth; Möncke, Doris; Clare, Alexis G.
Luminescence-site symmetry correlations in Dy3+ doped alkali-alkaline earth orthoborates of the type XZBO3 with X = Li, Na, K and Z = Mg, Ca, Ba. - In: Journal of luminescence, ISSN 0022-2313, Bd. 241 (2022), 118429, S. 1-12

A systematic investigation of the luminescence properties of Dy3+ doped alkali-alkaline earth orthoborates of the stoichiometric composition XZBO3 with X = Li, Na, K and Z = Mg, Ca, Ba was conducted. XRD diffractograms show that the compounds LiMgBO3, LiCaBO3, LiBaBO3, NaMgBO3, NaCaBO3, NaBaBO3, and KMgBO3 could be produced in high purity. Relatively intense luminescence was observed only for the phases LiCaBO3, NaMgBO3, NaCaBO3 and NaBaBO3. Micro Raman investigations show that the Dy3+ luminesence mainly originates from the orthoborate phase in these samples. Photo-luminescence spectroscopy of LiCaBO3, NaCaBO3 and NaBaBO3 shows the typical Dy3+ emission with the prominent emission peak in the yellow spectral range around 575 nm. A second, but much less intense peak is observed at around 485 nm (cyan). The luminescence emission spectrum of Dy3+:NaMgBO3 is much different: here, the highest emission intensity is observed at about 485 nm. It is proposed that the Dy3+ ions occupy the Na positions in this crystal phase which has a much higher symmetry than the alkaline earth positions in the other examined crystal phases. This is supported by broadened and more split up peaks in the excitation and emission spectra of Dy3+:NaMgBO3 suggesting a much stronger local crystal field at the rare earth position in this compound. The results are additionally compared to spectroscopic data of different well known Dy3+ doped crystalline compounds and Dy3+ and Eu3+ doped alkali-alkaline earth orthoborates from other publications, which offer further insight into the relation between the crystallographic sites of the doped rare earth ions and their luminescence.



https://doi.org/10.1016/j.jlumin.2021.118429
Benisch, Michael F.; Liebl, Johannes; Bogner, Werner; Fähnle, Oliver; Rädlein, Edda
Impact analysis of temperature and humidity effects on polishing. - In: EOS Annual Meeting (EOSAM 2021), (2021), 03011, S. 1-3

The polishing process for optical glass is one with intertwined chemical and mechanical processes. The aim of the present study is to verify whether control of these factors can be used to improve the efficiency of the polishing process.



https://doi.org/10.1051/epjconf/202125503011
Weigel, Christoph; Brokmann, Ulrike; Hofmann, Meike; Behrens, Arne; Rädlein, Edda; Hoffmann, Martin; Strehle, Steffen; Sinzinger, Stefan
Perspectives of reactive ion etching of silicate glasses for optical microsystems. - In: Journal of optical microsystems, ISSN 2708-5260, Bd. 1 (2021), 4, S. 040901-1-040901-22

We provide a review of the latest research findings as well as the future potential of plasma-based etching technology for the fabrication of micro-optical components and systems. Reactive ion etching (RIE) in combination with lithographic patterning is a well-established technology in the field of micro- and nanofabrication. Nevertheless, practical implementation, especially for plasma-based patterning of complex optical materials such as alumino-silicate glasses or glass-ceramics, is still largely based on technological experience rather than established models. Such models require an in-depth understanding of the underlying chemical and physical processes within the plasma and at the glass-plasma/mask-plasma interfaces. We therefore present results that should pave the way for a better understanding of processes and thus for the extension of RIE processes toward innovative three-dimensional (3D) patterning as well as for the processing of chemically and structurally inhomogeneous silicate-based substrates. To this end, we present and discuss the results of a variety of microstructuring strategies for different application areas with a focus on micro-optics. We consider the requirements for refractive and diffractive micro-optical systems and highlight potentials for 3D dry chemical etching by selective tailoring of the material structure. The results thus provide first steps toward a knowledge-based approach to RIE processing of universal dielectric glass materials for optical microsystems, which also has a significant impact on other microscale applications.



https://doi.org/10.1117/1.JOM.1.4.040901
Weigel, Christoph; Brokmann, Ulrike; Rädlein, Edda; Strehle, Steffen
Maskless pattern transfer into photostructurable glasses by deep plasma etching. - In: MikroSystemTechnik, (2021), S. 419-421

Westphalen, Jasper;
Implementierung eines Moduls zur großflächigen In-Line Blitzlampentemperung von gesputterten ITO-Schichten. - Ilmenau : Universitätsverlag Ilmenau, 2021. - 1 Online-Ressource (x, 109 Seiten). - (Werkstofftechnik aktuell ; Band 22)
Technische Universität Ilmenau, Dissertation 2020

Die Blitzlampentemperung (Flash Lamp Annealing - FLA) zählt zu den Kurzzeittemperverfahren (Rapid Thermal Annealing - RTA), da die Erwärmung und Abkühlung der Schicht im Bereich von Millisekunden liegen. Die mit Hilfe von Blitzlampen durchgeführte Temperung dient zur oberflächennahen Erwärmung von Festkörpern. Hierbei handelt es sich um einen thermischen Prozess, der Materialeigenschaften verändern kann. Durch die Blitzlampentemperung kann der Schichtwiderstand von transparenten leitfähigen Oxidschichten (Transparent Conductive Oxides - TCO) reduziert und die Transmission im sichtbaren Wellenlängenbereich erhöht werden. In der vorliegenden Forschungsarbeit wird das Prozessverhalten von dynamischen FLA-Prozessen bei Indium-Zinn-Oxid (ITO) Schichten experimentell dargelegt. Dazu wurde der Einfluss von verschiedenen Prozessparametern wie Energiedichte und Pulszeit des Xenonlichtblitzes erforscht. Erste Versuche zur Untersuchung des Einflusses der Blitzwiederholrate und der Geschwindigkeit des Substrates ließen sich erfolgreich durchführen. Die Herstellung aller Schichten erfolgte am Fraunhofer-Institut für Organische Elektronik, Elektronenstrahl- und Plasmatechnik (FEP) in der In-Line Sputteranlage ILA 750. Für die Blitzlampentemperung wurde das Lampensystem Xenon Flash Lamp Modul FLA 2x360w der Firma ROVAK GmbH genutzt. Das Modul ist Bestandteil der Beschichtungsanlage ILA 900 am Fraunhofer FEP und erlaubt sowohl die statische als auch die dynamische FLA-Behandlung von Substraten bis zu einer Größe von 600 mm x 1200 mm. Die unterschiedlichen Einstellungen der Blitze ließen sich optisch vermessen. Für ITO-Schichten mit einer Schichtdicke von 150 nm konnte nach der FLA-Behandlung ein Widerstand von 14 [Ohm] erreicht werden. Für die Transmission im sichtbaren Wellenlängenbereich wurden 87 % erzielt. Diese Werte sind vergleichbar mit einer konventionellen Temperung von ITO-Schichten im Ofen. Erfolgreich ließ sich zeigen, dass der FLAProzess an eine bestehende In-Line Prozessanlage implementiert werden kann.



https://doi.org/10.22032/dbt.49068
Strugaj, Gentiana; Herrmann, Andreas; Rädlein, Edda
AES and EDX surface analysis of weathered float glass exposed in different environmental conditions. - In: Journal of non-crystalline solids, ISSN 0022-3093, Bd. 572 (2021), 121083

To characterize the influence of environmental conditions on glass weathering, two different float glasses were subjected to a six-month outdoor experiment that took place in Durres (seacoast, Albania), Ilmenau (rural, Germany) and Pristina (urban, Kosovo), three sites with largely different environmental conditions. Atmospheric deposits and meteorological conditions led this study to receive information about different weathering behaviour of two types of float glasses. Typical glass degradation effects and reaction products at the glass surface are shown and the impact of weathering and air quality parameters on the formation of reaction products and degradation is discussed. Surface changes have been localized using optical microscopy. Further investigations for receiving chemical information on the contaminations include Auger electron spectroscopy (AES) and scanning electron microscopy (SEM/EDX). Surface analyses indicate a high amount of weathering products such as chlorides, sulphates and carbonates followed by severe delamination effects for both types of glass exposed in Durres and Pristina. In contrast to this, low levels of soiling and degradation for the samples exposed in Ilmenau were detected.



https://doi.org/10.1016/j.jnoncrysol.2021.121083
Zekri, Mohamed; Herrmann, Andreas; Erlebach, Andreas; Damak, Kamel; Rüssel, Christian; Sierka, Marek; Maâlej, Ramzi
The structure of Gd3+-doped Li2O and K2O containing aluminosilicate glasses from molecular dynamics simulations. - In: Materials, ISSN 1996-1944, Bd. 14 (2021), 12, 3265, insges. 18 S.
Im Titel sind "3+" hochgestellt und "2" tiefgestellt

Understanding the atomic structure of glasses is critical for developing new generations of materials with important technical applications. In particular, the local environment of rare-earth ions and their distribution and clustering is of great relevance for applications of rare earth-containing glasses in photonic devices. In this work, the structure of Gd2O3 doped lithium and potassium aluminosilicate glasses is investigated as a function of their network modifier oxide (NMO-Li2O, K2O) to aluminum oxide ratio using molecular dynamics simulations. The applied simulation procedure yields a set of configurations, the so-called inherent structures, of the liquid state slightly above the glass transition temperature. The generation of a large set of inherent structures allows a statistical sampling of the medium-range order of the Gd3+ ions with less computational effort compared to other simulation methods. The resulting medium-range atomic structures of network former and modifier ions are in good agreement with experimental results and simulations of similar glasses. It was found that increasing NMO/Al ratio increases the network modifier coordination number with non-bridging oxygen sites and reduces the overall stability of the network structure. The fraction of non-bridging oxygen sites in the vicinity of Gd3+ ions increases considerably with decreasing field strength and increasing concentration of the network modifier ions. These correlations could be confirmed even if the simulation results of alkaline earth aluminosilicate glasses are added to the analysis. In addition, the structure predictions generally indicate a low driving force for the clustering of Gd3+. Here, network modifier ions of large ionic radii reduce the probability of Gd-O-Gd contacts.



https://doi.org/10.3390/ma14123265
Thieme, Christian; Herrmann, Andreas; Kracker, Michael; Patzig, Christian; Höche, Thomas; Rüssel, Christian
Microstructure investigation and fluorescence properties of europium-doped scheelite crystals in glass-ceramics made under different synthesis conditions. - In: Journal of luminescence, ISSN 0022-2313, Bd. 238 (2021), 118244, S. 1-8

https://doi.org/10.1016/j.jlumin.2021.118244
Reiß, Stephanie; Hopfeld, Marcus; Romanus, Henry; Pfeifer, Kerstin; Krischok, Stefan; Rädlein, Edda
Chemical changes of float glass surfaces induced by different sand particles and mineralogical phases. - In: Journal of non-crystalline solids, ISSN 0022-3093, Bd. 566 (2021), 120868

Particles play an important role in the storage, transportation and natural weathering of glasses, but their influence on glass degradation is little studied. In this work, the influence of main sand components is investigated. Feldspar exhibits the strongest leaching rate for the network former Na, while quartz has the lowest. The leaching rate of natural sands is in between. Based on these findings, a model describing the leaching mechanism was developed: Hereby, hydroxyl groups adhering on sand grains adsorb network modifiers by substituting their hydrogen by network formers from the glass surface. The amount of available hydroxyl groups determines the leaching rate. This model is supported by loss on ignition performed for the sands, which might be a suitable method to roughly estimate their leaching rates. The adsorption of network modifiers suppresses carbonate formation, dendritic growth and Mg diffusion in the glass surface region. Pimple-like crystal growth is observed.



https://doi.org/10.1016/j.jnoncrysol.2021.120868