TY - JOUR A1 - Tielemann, Christopher A1 - Busch, R. A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Avramov, I. A1 - Müller, Ralf T1 - Oriented surface nucleation in diopside glass N2 - Es wird die Texturbildung in kristallisierendem Diopsidglas im Zusammenhang mit der Oberflächenbeschaffenheit der unbehandelten Probe untersucht. Zudem wird der diskutiert, dass es sich bei der Texturbildung in Gläsern höchstwahrscheinlich um ein Nukleationsphänomen handelt welches auf die richtungsabhängige Grenzflächenenergie der kristallisierenden Phase zurückzuführen ist. N2 - Oriented surface crystallization on polished diopside glass surfaces has been studied with scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy and laser scanning microscopy. An orientation preference of [001] parallel to the glass surface was detected for separately growing diopside crystals even as small as 700 nm in size. This finding shows that crystal orientation occurs in the outermost surface layer without crystal-crystal interaction and indicates that the crystal orientation is a result of oriented nucleation. Depending on surface preparation, monomodal crystal orientation distributions with [100] perpendicular to the surface or bimodal distributions with [100] and [010] perpendicular to the glass Surface were detected. It was also shown that the degree of crystal orientation increases with decreasing Surface roughness. The observed orientation of diopside crystals could be explained in terms of the interfacial energies of different crystal faces. KW - Surface energy KW - Glass ceramic KW - Glass KW - EBSD KW - Diopsid PY - 2021 UR - https://www.sciencedirect.com/science/article/pii/S002230932100020X DO - https://doi.org/10.1016/j.jnoncrysol.2021.120661 SN - 0022-3093 VL - 562 PB - Elsevier B.V. AN - OPUS4-53073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Rouxel, T. A1 - Behrens, H. A1 - Deubener, J. A1 - Müller, Ralf T1 - Vacuum crack growth in alkali silicate glasses N2 - Crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young´s moduli and the theoretical fracture surface energy estimated from chemical bond energies. Data analysis reveals significant deviations from this intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture. KW - Silicate glass KW - Brittle fracture KW - Crack growth KW - Calculated intrinsic fracture toughness PY - 2021 DO - https://doi.org/10.1016/j.jnoncrysol.2021.121094 SN - 0022-3093 VL - 572 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-53144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Sintering of silver‑alkali zinc borate glass‑composites N2 - 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. T2 - Technology Crossover Extravaganza, HiTEC/CICMT/APEPS CY - Online meeting DA - 26.04.2021 KW - Silver-glass-metallization-paste KW - Sintering KW - Crystallization KW - Alkali ions KW - Sintering atmosphere PY - 2021 AN - OPUS4-52872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Sintering and Foaming of Silicate Glass Powders N2 - 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. T2 - Sandanski Workshop Sinter crystallization 27th-29th September 2021 PROJECT “THEORY AND APPLICATIONS OF SINTER-CYSTALLIZATION” DN 19/7 CY - Online meeting DA - 27.10. 2021 KW - Sintering KW - Non-desired foaming PY - 2021 AN - OPUS4-53772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten T1 - 3D printing of crystallizing bioactive glasses N2 - Artificial bone replacement by individual customized three-dimensional resorbable bioactive glass has not yet been widely established in the clinical use. This is mainly due to the antagonism of sintering ability and suitable bioactivity. Competitive crystallization often prevents the generation of dense sintered bodies, especially for additive manufactured 3D structures. Previous studies of the fluoride-containing glass F3 have shown its potential to combine both sintering ability and suitable bioactivity. Furthermore, the occurring sintering blockade by surface crystallization of Na2CaSi2O6 was tunable by glass particle size. In this study the glasses F3, F3-Cu with 1 mol% CuO added at the expense of CaO and the well-known 13-93 were chosen to determine the influence of surface crystallization on 3D printed sinter bodies. For this purpose, grain size fractions in range of smaller 32 µm to 315 µm in fraction size of 6-20 µm were sieved from jaw crushed glass frit as well as glass cubes were cut from casted blocks for all glasses. Sintering behavior of both pressed and printed powder compacts was observed via heating microscopy. Crystallization was determined by DTA and crystallization progress was monitored on fractured sinter bodies and polished cubes via electron and laser scanning microscopy as well as with diffractometry. Depending on grain size the formation of crystalline support framework along former grain boundaries shows the capability to stabilize fully densified sinter bodies before softening. Beside of this, the generation of complex hierarchic porosity was possible as well. T2 - ICG Berlin 2022 CY - Berlin, Germany DA - 03.07.2022 KW - Bioactive Glass KW - Crystallization KW - Sintering KW - 3D printing PY - 2022 AN - OPUS4-55253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Flüssigphasensinterung von Silber-Glas Dispersionen N2 - Silber-Glas Wechselwirkungen spielen eine wichtige Rolle zum Beispiel in Glas-haltigen Silberpasten, die in der Photovoltaik oder Mikroelektronik verwendet werden. Um ein besseres Verständnis der Vorgänge zu erhalten, werden niedrig-schmelzende, bleifreie X2O ZnO B2O3 Gläser (X = Li, Na, K und Rb, Abk.: LZB, NZB, KZB and RZB) zur Untersuchung der Pasten verwendet. Raman und Infrarot Spektroskopie zeigen, dass die Glasstruktur weitgehend vergleichbar ist, aber Unterschiede in der Bildung von Pentaboratgruppen in LZB und NZB oder Diboratgruppen in KZB und RZB auftreten. Die Anzahl an vierfach koordinierten Bor-Ionen (N4) sinkt mit zunehmendem Alkaliionenradius. Die Verringerung von N4 führt zu einer niedrigeren Glasübergangstemperatur in der Reihe LZB (472 °C) < NZB (465 °C) < KZB (460 °C) < RZB (449 °C). Zur Herstellung der Pasten wurde kommerzielles Silber-Pulver mit 30 Vol.-% Glas und Organik gemischt. Das Sinterverhalten der gepressten Pulver wurde mittels Erhitzungsmikrospie untersucht. Der Sinterbeginn der Pasten ist vergleichbar und korrespondiert mit den geringen Unterschieden der Viskosität bei vergleichbarer Partikelgröße der Gläser. In den Ag-KZB- und Ag-RZB-Pasten ist die Schwindung durch die stärker einsetzende Kristallisation im Vergleich zu LZB und NZB verzögert. T2 - AK Glasig-kristalline Multifunktionswerkstoffe CY - Aachen, Germany DA - 17.02.2022 KW - Sintern KW - Silber KW - Glas KW - Diffusion KW - Gefüge PY - 2022 AN - OPUS4-55735 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Liquid phase sintering of alkali zinc borate glass-bearing silver pastes for applications in photovoltaics and microelectronics N2 - Liquid phase sintering of glass bearing silver pastes used in photovoltaics and microelectronics is poorly understood. In particular, the role of different network modifiers acting in the glass component and the question of the most suitable atmospheric oxygen level during sintering are still under considerable debate. To tackle these issues, low-melting and lead-free X2O-ZnO-B2O3 glasses with X = Li, Na, K and Rb (LZB, NZB, KZB and RZB) were prepared. Infrared spectroscopy showed that the glass structure was similar to each other, while an increase of tetrahedrally coordinated boron with increasing field strength of the alkali was evident. In turn, the glass transition temperature (from differential thermal analysis) increased in the order: RZB (449 °C) < KZB (460 °C) < NZB (465 °C) < LZB (472 °C). Powders of each glass were mixed with organics to receive silver-glass-pastes containing 30 vol% glass and these were subjected to heating microscopy in air. Although similar onset temperatures of sintering were recorded for Ag-NZB and Ag-LZB glass pastes, and for Ag-RZB paste and KZB-Ag-paste, respectively, differences in the crystallization behavior and final densification were observed between the former and the latter group. These were translated in terms of differences in silver dissolution and reprecipitation among the two groups. Further, running the experiments in nitrogen gas showed that sintering of all pastes was considerably hampered. The slow-down of the sinter kinetics was found to be in line with the assumed lower oxidation and dissolution of silver ions into the glass-forming liquid. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Silver metallization paste KW - Sintering KW - Glass KW - Alkali zinc borate glasses KW - Viscosity KW - Structure PY - 2022 AN - OPUS4-55728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - In situ observation of silver precipitation in sodium zinc borate glass-forming melts N2 - Melting of Na2CO3-ZnO-B2O3 batches containing up to 16.8 wt% AgNO3 (5 mol% Ag2O in the target glass composition) was observed in situ by means of hot stage microscopy. In all batches metallic silver precipitation took place as most of the silver nitrate was reduced to metallic silver before Ag+ ions could be dissolved in the evolving borate melts. In turn, only traces of Ag+ (<300 ppmw) were dissolved in the sodium zinc borate glass melts under study. It is assumed that the oxidation to Ag+ was limited due to poor availability of reducible oxygen in the glass melts and presence of Na2O being a stronger base than Ag2O. Thus, the precipitated metallic silver formed droplets of different sizes. The larger droplets (d > 20 µm) were already settled at the bottom of the container and remained constant in size upon dwelling for 1 h at 1050 °C of about one hour and the subsequent cooling (45 K/min) to room temperature, whereas the smaller droplets (d < 20 µm) were mobile in the borate melt due to Marangoni and Stokes motion. For the latter droplets, coalescence was observed in situ. A growth of larger droplets at the expense of smaller ones, i.e., Ostwald ripening was also expected but could not be studied with the used experimental equipment. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Glass melt KW - Silver KW - Sodium zinc borate glass KW - Hot stage microscopy KW - Precipitation PY - 2022 AN - OPUS4-55732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan T1 - Surface-Initiated Microstructure Formation in Glass Ceramics N2 - 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. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Glass KW - Oriented surface crystallization KW - Surface energy KW - Bond energy KW - Nucleation mode PY - 2022 AN - OPUS4-56070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tielemann, Christopher T1 - Oriented Surface Crystallization N2 - 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. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Glass KW - Surface energy KW - Crystal orientation PY - 2022 AN - OPUS4-56074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina T1 - Vacuum crack growth in silicate glasses N2 - Although the slow crack growth in glass is dominated by stress-corrosion phenomena, it also should reflect the underlaying intrinsic fracture behavior controlled by glass chemistry and structure. To investigate such underlaying phenomena, crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young’s moduli and theoretical fracture surface energy. Data analysis reveals slight correlation with the packing density and significant deviations from the intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Oxide glass KW - Fracture toughness KW - Fracture surface PY - 2022 AN - OPUS4-56485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Chen, Y.-F. A1 - Contreras Jaimes, A. T1 - Datengetriebener Workflow für die beschleunigte Entwicklung von Glas (GlasDigital) N2 - Das Projekt GlasDigital wurde im allgemeinen vorgestellt, sowie die einzelnen Zwischenstände der verschiedenen Arbeitspakete aller Projektpartner präsentiert. Die allgemeine Porjektvorstellung ist auf deutsch. Die Zwischenstände der Arbeitsinhalte sind auf englisch. T2 - PMD Vollversammlung CY - Berlin, Germany DA - 03.11.2022 KW - Oxidglas KW - Robotische Glasschmelzanlage KW - ML KW - Ontologie KW - Digitaler Zwilling KW - Bildanalyse PY - 2022 AN - OPUS4-56491 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kilo, M. T1 - Glass Screening for the systematic development of new glasses N2 - Die technischen Möglichkeiten der robotischen Glasschmelzanlage der BAM werden vorgestellt. T2 - 26th International Conference on Glass CY - Berlin, Germany DA - 04.07.2022 KW - Material Digital PY - 2022 AN - OPUS4-56280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina T1 - Data-driven Workflow for Accelerated Glass Development (GlasDigital) N2 - As part of a joint project involving the Fraunhofer Institute for Silicate Research (ISC), the Friedrich Schiller University of Jena, the Clausthal University of Technology and the Federal Institute for Materials Research and Testing (BAM), digital tools are to be created for the development of new types of glass materials. Current processes for the production of glasses with improved properties are usually very cost- and energy-intensive due to the low degree of automation and are subject to long development cycles. The use of robotic synthesis processes in combination with self-learning machines is intended to overcome these problems in the long term. The development of new types of glass can then not only be accelerated considerably, but also be achieved with much less effort. In this talk, data generation via a robotic high-throughput glass melting system is presented, which should be the experimental basis for the ontology developed within the project GlasDigital. T2 - Materials Science and Engineering Congress (MSE 2022) CY - Darmstadt, Germany DA - 27.09.2022 KW - Oxidglas KW - Robotische Glasschmelzanlage PY - 2022 AN - OPUS4-56489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenbusch, Ivo A1 - Arai, Marylyn Setsuko A1 - Rizzo, Fabio A1 - de Camargo, Andrea S. S. A1 - Ravoo, Bart Jan T1 - A host–guest approach to ratiometric pH sensing using upconversion nanoparticles N2 - A new pH nanosensor based on β-NaYF4:Yb3+/Tm3+ upconversion nanoparticles functionalized with cyclodextrin and a pH-sensitive adamantane-modified nitrobenzoxadiazole dye (NBD-Ad). KW - Host-guest materials KW - Upconversion nanoparticles KW - Ratiometric optical sensors KW - pH sensing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637722 DO - https://doi.org/10.1039/d5na00145e SN - 2516-0230 VL - 7 IS - 13 SP - 4142 EP - 4151 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea Simone Stucchi T1 - Optical and Spectroscopic Properties of Glasses N2 - Optical glasses have given us the eyes to unveil the microscopic and the macroscopic worlds through microscope and telescope lenses, they have revolutionized the way we communicate through fiber optics and portable device screens, as well as given us new perspectives for sustainable energy harvesting conversion and generation. To meet the demands of ever-growing markets, the compositional design of new glasses requires full characterization of thermal, mechanical, electric, and optical properties. Particularly, the characterization of optical properties is not only relevant for optical/luminescent applications but is also essential for the tailored design of some medical and dental materials such as restorative resins, implants and prothesis. In this seminar we will introduce the fundaments on the optical properties of materials, with particular focus on glasses, and the techniques to characterize them. T2 - 3rd Sao Carlos School on Glasses and Glass-Ceramics CY - Sao Carlos, Brazil DA - 10.03.2025 KW - Optical properties KW - Glasses PY - 2025 AN - OPUS4-63773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea Simone Stucchi T1 - Structure and photophysics of RE ion doped gallium phosphofluoride glasses containing silver nanostructures: Effects of heat treatment and femtosecond direct laser writing. N2 - Gallium fluoride phosphate glasses are interesting hosts for emissive rare-earth (RE) dopants. Despite featuring low refractive index, they present high energy radiation resistance and a wide optical transmission range (350 to 1700 nm) enabling observation of important RE3+ emissions in the visible to near-infrared spectral range. In a previous, NMR-based structural study of the system xGa(PO3)3–(40-x)GaF3–20BaF2–20ZnF2–20SrF2 (x = 5 - 25 mol%), we verified that the network structure of these glasses is dominated by P-O-Ga linkages with no P-O-P linkages and that Ga is mainly six-coordinated in a mixed fluoride/phosphate environment. For Eu3+ doped samples, the photophysical properties strongly suggest changes in the ion´s ligand distribution toward a fluoride-dominated environment at low P/F, which translates into improved radiative emissions. To extend the studies to other RE doped glasses, and glasses containing Ag nanostructures (and their influence on RE emission), we selected the composition 25Ga(PO3)3 – 20ZnF2 – 30BaF2 - (25 – x - y)SrF2 – xAgNO3 - yNdF3, where x = 0, 1, 3, 5, 10 mol% and y = 0 or 1 mol%. The glasses were synthesized through the conventional melt-quenching technique and fully characterized from the thermal, structural, and microstructural viewpoints. By appropriate heat-treatment, the presence of both Ag nanoclusters (Ag-NCs, < 10 nm) and larger nanoparticles was confirmed by TEM in agreement with the observation of broad emission bands in the visible spectrum. Excited state lifetime measurements evidence the presence of non-radiative energy transfer processes between the Ag species to Nd3+ ions but there is no direct evidence of plasmon enhancement effects. In samples singly doped with silver, direct laser writing experiments using a femtosecond laser were also performed which induced localized growth of Ag-NCs associated to a variation in the refractive index. Preliminary results indicate the potential of the DLW technique for tailoring optical glass properties. T2 - 27th International Congress on Glass 2025 CY - Kolkata, India DA - 20.01.2025 KW - Gallium phosphofluoride glass KW - Structure-property correlation KW - Femtosecond direct laser writting KW - Neodymium PY - 2025 AN - OPUS4-63774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Composition-structure-property relationships of ternary borate glasses N2 - Since the pioneer work of Krogh-Moe [1] in the 1960’s the structure clarification of borate glasses is of interest for many generations. In the present contribution the composition–structure–property relationships of Me2O–ZnO–B2O3, Me = Li (LZB), Na (NZB), K (KZB), Rb (RZB), CaO–ZnO–B2O3 (CaZB), and Li2O–PbO–B2O3 (LPbB) glasses are investigated. Non-toxic, highly polarizable zinc oxide potentially substitutes harmful lead oxide in glasses for applications e.g., in photovoltaics and microelectronics. Glass structure was analyzed using Raman and infrared spectroscopy, and the glass properties were measured using dilatometry (Tg, viscosity data, coefficient of thermal expansion) and rotational viscometry (high-temperature viscosity) [2,3]. The spectroscopic results show that alkali and calcium ions largely balance out the negative charges of BO4-units, while zinc and lead ions mainly stabilize the non-bridging oxygen atoms (NBO). The type of network modifier ion directs formation of the BO4-containing groups and the number of BO4-units (N4). Thus, i.) BO4-containing pentaborate was assigned in LZB, NZB and CaZB glasses, and ii.) diborate in KZB and RZB glasses. Simultaneous presence of pentaborate and diborate was only detected in LPbB. The combination of modifier’s properties, i.e., lower Lewis’s basicity (Rb+ > Li+), higher field strength (Rb+ < Li+), lower polarizability (Rb+ > Li+), and steric effects with increasing size (Rb+ > Li+) [4], leads to slightly increasing N4 in the series RZB (0.36) ≈ KZB < NZB (0.37) < LZB ≈ CaZB (0.39). This increase in N4 results in an increase in the atomic packing density 0.519 (RZB) – 0.584 (LZB) and thus in the Young’s Modulus 38.1 GPa (RZB) – 92.5 GPa (LZB) and in the glass transition temperature (Tg) 444 °C (RZB) – 467 °C (LZB) in the alkali series. In reverse order the coefficient of thermal expansion decreases from 12·10-6 K-1 (RZB) – 8.54·10-6 K-1 (LZB) with increasing N4. Ca2+ in CaZB enhances the viscosity (Tg: 580 °C) compared to Li+ in isocompositional LZB due to higher coordination. On the other hand, Pb2+ in LPbB decreases the viscosity (Tg: 399 °C) compared to Zn2+ in LZB with similar molar fractions. T2 - 98th Glass-Technology Conference of the German Society of Glass Technology (DGG) CY - Goslar, Germany DA - 26.05.2025 KW - Borate glasses KW - Structure-property relationship PY - 2025 AN - OPUS4-63771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xie, Zhuocheng A1 - Atila, Achraf A1 - Guénolé, Julien A1 - Korte-Kerzel, Sandra A1 - Al-Samman, Talal A1 - Kerzel, Ulrich T1 - Predicting grain boundary segregation in magnesium alloys: An atomistically informed machine learning approach N2 - Grain boundary (GB) segregation substantially influences the mechanical properties and performance of magnesium (Mg). Atomic-scale modeling, typically using ab-initio or semi-empirical approaches, has mainly focused on GB segregation at highly symmetric GBs in Mg alloys, often failing to capture the diversity of local atomic environments and segregation energies, resulting in inaccurate structure-property predictions. This study employs atomistic simulations and machine learning models to systematically investigate the segregation behavior of common solute elements in polycrystalline Mg at both 0 K and finite temperatures. The machine learning models accurately predict segregation thermodynamics by incorporating energetic and structural descriptors. We found that segregation energy and vibrational free energy follow skew-normal distributions, with hydrostatic stress, an indicator of excess free volume, emerging as an important factor influencing segregation tendency. The local atomic environment’s flexibility, quantified by flexibility volume, is also crucial in predicting GB segregation. Comparing the grain boundary solute concentrations calculated via the Langmuir-McLean isotherm with experimental data, we identified a pronounced segregation tendency for Nd, highlighting its potential for GB engineering in Mg alloys. This work demonstrates the powerful synergy of atomistic simulations and machine learning, paving the way for designing advanced lightweight Mg alloys with tailored properties. KW - Machine learning KW - Grain boundary segregation KW - Magnesium alloys KW - Atomistic simulation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638499 DO - https://doi.org/10.1016/j.jma.2025.03.021 SN - 2213-9567 VL - 13 IS - 6 SP - 2636 EP - 2650 PB - Elsevier B.V. AN - OPUS4-63849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - An overview of structural, physical and thermal properties of low melting zinc and lead borate glasses N2 - Low melting zinc borate glasses awake interest to replace lead borate glasses in the silver metallization pastes for solar cells or microelectronics. In the current study, characteristic properties of alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) were compared to an earth alkali zinc borate glass (CaO-ZnO-B2O3). Additionally, zinc oxide is partially substituted by lead oxide or cooper oxide in the borate glasses (Li2O-PbO-B2O3, Na2O ZnO CuO-B2O3). The alkali zinc borate glasses indicate less differences in Raman spectra, and thus in structural properties, in comparison to the Ca and Pb ions influence. LPbB (Tg = 401 °C) has a lower viscosity than LZB (Tg = 468 °C) and CaZB has the highest glass transition temperature (Tg = 580 °C). The Angell plot for the alkali zinc borate glasses shows a high fragility m = 80. Besides Tg, the density measured by means of the Archimedean principle, molar volume, and coefficient of thermal expansion (CTE) of the glasses were investigated. Trends could be found according to alkali ions or intermediate oxides. The density increases with decreasing alkali ion size from KZB (2.632 g/cm3) to LZB (2.829 g/cm3) and increases from LZB to LPbB (3.764 g/cm3). CTE ranges between 7.09 10-6 K-1 for CaZB and 11.5 10 6 K 1 for KZB and RZB. The differential thermal analysis (DTA) and X ray diffraction (XRD) indicate crystallization of various crystalline phases during heating with 5 K/min in most cases. T2 - 94. Glastechnische Tagung CY - Online meeting DA - 10.05.2021 KW - Borate glasses KW - Glass structure KW - Viscosity KW - Young´s Modulus KW - Alkali ions PY - 2021 AN - OPUS4-52867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Viscous crack healing in soda–lime–magnesium–silicate–ZrO2 glass matrix composites N2 - AbstractThe present study investigates the influence of the crystal volume content on viscous crack healing in glass ceramic glass sealants. To ensure constant microstructure during healing, soda–lime–magnesium silicate glass matrix composites with varied volume fractions of ZrO2 filler particles were used. Crack healing was studied on radial cracks induced by Vickers indentation, which were stepwise annealed to monitor the healing progress by confocal laser scanning microscopy. Confirming previous studies, healing of radial cracks in pure glass was found delayed by global flow phenomena like crack widening and crack edge and tip rounding to minimize the sample surface. With increasing ZrO2 filler content, these global flow phenomena were progressively inhibited whereas local flow phenomena like sharp crack tip healing could still occur. As a result, crack healing was even accelerated by filler particles up to a maximum filler content of 17 vol% whereas crack healing was fully suppressed only at 33 vol% filler content. KW - Crack healing KW - Glass matrix composite KW - Solid oxide fuell cell KW - Vickers identation KW - Viscosity PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607860 DO - https://doi.org/10.1111/jace.20002 SN - 0002-7820 SP - 1 EP - 12 PB - Wiley AN - OPUS4-60786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gogula, Shravya A1 - Bornhöft, H. A1 - Wondraczek, L. A1 - Sierka, M. A1 - Diegeler, A. A1 - Müller, Ralf A1 - Deubener, J. T1 - Optical Real-Time Castability Evaluation for High-Throughput Glass Melting N2 - A novel optical real-time method for evaluating the castability of glass forming melts for laboratory furnaces is presented. The method is based on the analysis of top view images of the melt surface inside the crucible during melting after being subjected to a small mechanical impulse. In this way, the melt surface is excited to oscillate. The difference in contrast between two images taken in quick succession scales with the viscosity, with a larger diffe­rence occurring at lower viscosities. The method is designed as an instrument for the in-line evaluation of the castability for a high-throughput glass melting system as part of the joint project “GlasDigital” in the framework of the German Platform Material Digital initiative but is applicable to other laboratory furnaces as well. KW - Optical Real-Time Castability Check KW - Image Analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618659 DO - https://doi.org/10.52825/glass-europe.v2i.1359 VL - 2 SP - 83 EP - 93 AN - OPUS4-61865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Boccaccini, A. R. A1 - Müller, Ralf T1 - Sintering and Crystallization of Fluoride-Containing Bioactive Glass F3 N2 - The fluoride-containing bioactive glass F3 with nominal composition (mol%) 44.8 SiO2 - 2.5 P2O3 - 36.5 CaO - 6.6 Na2O - 6.6 K2O - 3.0 CaF2 is a highly promising candidate for bone replacement applications. Its strong crystallization tendency, however, requires a thorough understanding of the interplay between glass powder particle size, surface crystallization, and sintering. Therefore, this study characterizes the sintering and crystallization of bulk specimens and various particle size fractions by differential thermal-analysis, laser scanning, electron microscopy, X-ray diffraction, and Infrared spectroscopy. Particle size fractions < 56 µm were found to fully densify, while crystals growing from the glass particle surface retard sintering of coarser fractions. Small amounts of a non-stoichiometrically calcium phosphosilicate (Ca14.92(PO4)2.35(SiO4)5.65) occurs as the primary crystal phase followed by combeite (Na4Ca4[Si6O18]) as a temporarily dominating phase. The surface crystallization of both pha­ses was found to be mainly responsible for sinter retardation. During later stages of crystallization, additional phases such as cuspidine (Ca4F2Si2O7) and silicorhenanite (Na2Ca4(PO4)2SiO4) occur, but finally monoclinic wollastonite (CaSiO3) forms as the dominant phase. KW - Bioactive Glass KW - Sintering KW - Crystallization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632482 DO - https://doi.org/10.52825/glass-europe.v3i.2564 SN - 2940-8830 VL - 3 SP - 105 EP - 124 AN - OPUS4-63248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal friction and energy dissipation during fracture in silicate glasses N2 - To obtain a deeper insight into the nature of energy dissipation during fracture, the internal friction of 13 borosilicate, aluminosilicate, soda-lime, and lead-containing glasses, for which inert crack growth data are known, was measured using dynamic mechanical thermal analysis. For asymmetrically bent glass beams, the loss tangent, tan δ, was determined between 0.2 and 50 Hz at temperatures between 273 K and the glass transition temperature, Tg. It was found that the area under the tan δ vs T·Tg−1 curve correlates with the crack growth exponent, n, in the empirical v = v0·KIn relation between crack growth velocity, v, and stress intensity, KI, which indicates that n correlates with the degree of energy dissipation of sub-Tg relaxation phenomena. KW - Glass KW - Internal friction KW - Crack growth PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631582 DO - https://doi.org/10.1063/5.0255432 SN - 0021-9606 VL - 162 IS - 19 SP - 1 EP - 9 PB - AIP Publishing AN - OPUS4-63158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pan, Z. A1 - Waurischk, Tina A1 - Duval, A. A1 - Müller, Ralf A1 - Deubener, J. A1 - Krishnan, N. M. A. A1 - Wondraczek, K. A1 - Wondraczek, L. T1 - Precise Real‐Time Measurement of Liquid Viscosity Using Digital Video Data N2 - Quantitative knowledge of liquid viscosity is of fundamental importance in many areas of materials synthesis and processing. However, the determination of viscosity often relies on specialized experimental equipment, offline experimentation, or invasive procedures, in particular when required in extreme conditions such as at high temperature, high pressure, and in confined or corrosive environments. Here, this study proposes and validates a fast and simple method that mimics the intuitive perception of liquid flow within a quantitative framework. For this, this study employs digital video observation to derive quantitative values of the shear viscosity of liquids, with high precision and rapid acquisition rates. The technique involves capturing liquid dynamics after minor mechanical stimulation. Processed imaging data are indexed by similarity and referenced to a digital database generated with a finite element model, from which values of viscosity are obtained in line. The approach is tested on water at room temperature and on a high‐temperature glass melt. Covering a viscosity range of four orders of magnitude, both yield convincing agreement with tabulated reference data at low computational cost. KW - Image analyses KW - Liquids KW - Materials discovery KW - Similarity analyses KW - Viscosities PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634606 DO - https://doi.org/10.1002/aisy.202500297 SN - 2640-4567 SP - 1 EP - 12 PB - Wiley AN - OPUS4-63460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Kiefer, P. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. T1 - Crack Growth in Hydrous Soda-Lime Silicate Glass N2 - Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water. KW - Internal friction KW - Soda-lime silicate glass KW - Water content KW - Stable crack growth KW - DCB geometry KW - Stress intensity factor PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506829 DO - https://doi.org/10.3389/fmats.2020.00066 VL - 7 SP - Articel 66 AN - OPUS4-50682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Maiwald, M. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Automated Analysis of Slow Crack Growth in Hydrous Soda-Lime Silicate Glasses N2 - To explore the impact of ambient and structural water on static fatigue, the initiation and growth of 3279 Vickers induced median radial cracks were automatically recorded and analyzed. We find that humidity is more efficient in initiating cracks and promoting their growth than water, which is dissolved in the glass structure. In particular for slow crack growth (< 3x10-6 m s-1), tests in dry nitrogen showed a considerable decrease in the crack growth exponent with increasing water content of the glasses. On the other hand, if tests were performed in humid air, the crack growth exponent was independent of the water content of the hydrous glasses, while stress intensity decreased slightly. These observations indicate that water promotes the processes at the crack-tip regardless of its origin. However, ambient water is more efficient. KW - Indentation fracture toughness KW - Slow crack growth KW - Automated analysis KW - Hydrous glass KW - Vickers indentation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513085 DO - https://doi.org/10.3389/fmats.2020.00268 VL - 7 SP - 268 AN - OPUS4-51308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. A1 - Marzok, Ulrich A1 - Reinsch, Stefan T1 - Hydrogen Permeation Through Glass N2 - Physical storage of gaseous hydrogen under high-pressure in glassy micro-containers such as spheres and capillaries is a promising concept for enhancing safety and the volumetric capacity of mobile hydrogen storage systems. As very low permeation through the container wall is required for storage of compressed hydrogen, development of glasses of minimal hydrogen permeability is needed. For this purpose, one has to understand better the dependence of hydrogen permeability on glass structure. The paper points out that minimizing the accessible free volume is as one strategy to minimize hydrogen permeability. Based on previously measured and comprehensive literature data, it is shown that permeation is independently controlled by ionic porosity and network modifier content. Thus, ionic porosity in modified and fully polymerized networks can be decreased equally to the lowest hydrogen permeability among the glasses under study. Applying this concept, a drop of up to 30,000 with respect to the permeation of hydrogen molecules through silica glass is attainable. KW - Ionic porosity KW - hydrogen storage KW - Glass KW - Permeability KW - Solubility KW - Diffusivity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513927 DO - https://doi.org/10.3389/fmats.2019.00342 VL - 6 SP - Article 342 AN - OPUS4-51392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf T1 - Alkali and alkaline earth zinc and lead borate glasses: Sintering and crystallization N2 - Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices. KW - Alkali zinc borate glasses KW - Lead borate glasses KW - Viscosity KW - Sintering KW - Crystallization KW - Fragility PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556128 DO - https://doi.org/10.1016/j.nocx.2022.100116 SN - 2590-1591 VL - 15 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-55612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Sintering and foaming of bioactive glasses N2 - Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming. VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas. KW - Bioactive Glass KW - Crystallization KW - Foaming KW - Sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552454 DO - https://doi.org/10.1111/jace.18626 SN - 0002-7820 SP - 1 EP - 11 PB - Wiley online library AN - OPUS4-55245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deubener, J. A1 - Behrens, H. A1 - Müller, Ralf T1 - An overview on the effect of dissolved water on the viscosity of soda lime silicate melts N2 - In this review article, the impact of dissolved water on the viscous properties of soda lime silicate melts is addressed against the background of the upcoming switch from natural gas to hydrogen combustion. This change will lead to an increase in the total water content of the glasses by up to 0.4 mol%. In order to better define possible influences of water speciation, water-rich glasses were synthesised under increasing pressure up to the kbar range. It is shown that a distinction must be made between the influence of dissolved OH-groups and H2Omolecules in order to accurately reflect the dependence of isokom temperatures on water content. In addition, an increase of one order of magnitude in the tolerance to higher deformation rates was observed for the range of expected increased water contents during isothermal deformation processes, which is based on the timetemperature superposition principle, i.e. congruent flow curves were determined under isokomal conditions. KW - Water in glass KW - Viscosity KW - Soda lime silicate glass KW - Shear thinning KW - Nydrogen melting PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587276 DO - https://doi.org/10.1016/j.nocx.2023.100195 VL - 19 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-58727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gomes Fernandes, Roger A1 - Al-Mukadam, Raschid A1 - Bornhöft, Hansjörg A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Selle, Susanne A1 - Deubener, Joachim T1 - Viscous Sintering of Acid Leached Glass Powders N2 - The process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down. KW - Glass powder KW - Viscous sintering KW - Acid-leaching KW - Sinter retardation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589008 DO - https://doi.org/10.52825/glass-europe.v1i.681 VL - 1 SP - 37 EP - 53 AN - OPUS4-58900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Viscous healing of Vickers indentation–induced cracks in glass N2 - AbstractViscous healing of cracks induced by the Vickers indentation in a soda lime magnesium silicate, a soda borosilicate, and a soda aluminosilicate glass (NAS) was studied by laser scanning microscopy. Plots of the crack length, width, and depth normalized to the initial crack length versus time over viscosity merge into single master curves of each of these quantities for each glass. Despite glass properties do not differ strikingly from each other, however, these master curves strongly differ among the glasses. This finding was attributed to a different interplay of various crack healing phenomena. Lateral cracks were found to be responsible for the bulging of the sample surface around the Vickers imprint, which in turn promotes radial crack widening as the main cause of healing delay. The most rapid healing of lateral cracks was observed in NAS in which bulging and crack widening were least pronounced. KW - Crack healing KW - Glass KW - Vickers indentation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587295 DO - https://doi.org/10.1111/jace.19245 SN - 0002-7820 VL - 106 IS - 10 SP - 5795 EP - 5805 PB - Wiley AN - OPUS4-58729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. T1 - Hydrogen Permeability of Tectosilicate Glasses for Tank Barrier Liners N2 - The permeation of hydrogen gas was studied in meta-aluminous (tectosilicate) glass powders of Li2O×Al2O3×SiO2 (LAS), Na2O×Al2O3×SiO2 (NAS) and MgO×Al2O3×SiO2 (MAS) systems by pressure loading and vacuum extraction in the temperatures range 210–310 °C. With this method, both the solubility S and the diffusivity D were determined, while the permeability was given by the product SD. For all glasses, S was found to decrease with temperature, while D increased. Since the activation energy of diffusion of H2 molecules exceeded that of dissolution, permeation increased slightly with temperature. When extrapolated to standard conditions (25 °C), the permeability of tectosilicate glasses was found to be only 10-22–10-24 mol H2 (m s Pa)-1, which is 8–10 magnitudes lower than most polymers. Thin glass liners of these compositions are expected to be the most effective barrier for tanks of pressurised hydrogen. KW - Hydrogen permeation KW - Aluminosilicate glasses KW - Hydrogen storage tank KW - Glass liner PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587284 DO - https://doi.org/10.52825/glass-europe.v1i.425 VL - 1 SP - 1 EP - 11 AN - OPUS4-58728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheffler, Franziska A1 - Fleck, Mirjam A1 - Busch, Richard A1 - Casado, Santiago A1 - Gnecco, Enrico A1 - Tielemann, Christopher A1 - Brauer, Delia S. A1 - Müller, Ralf T1 - Surface Crystallization of Barium Fresnoite Glass: Annealing Atmosphere, Crystal Morphology and Orientation N2 - Controlled oriented crystallization of glass surfaces is desired for high precision applications, since the uppermost crystal layer significantly influences the properties of the material. In contrast to previous studies, the data presented here deal with separated crystals growing at defect-free surfaces in four atmospheres with different degrees of humidity (ambient/dry air, argon and vacuum). A glass with the composition 2 BaO–TiO2–2.75 SiO2 was heat-treated at 825 °C until fresnoite (Ba2TiSi2O8) grew to a significant size. The crystal growth rate is found to increase with increasing humidity. The morphology of the crystals changes from highly distorted dendrites in the driest atmosphere (vacuum) to circular/spear-head-shaped crystals in the wettest atmosphere (ambient air), which we attribute to a decrease in viscosity of the glass surface due to water uptake. The least distorted crystals appear in the form of depressions of up to 6 µm. This has an influence on the observed crystal orientation, as measured by electron backscatter diffraction (EBSD). The pulled-in crystals change the orientation during growth relative to the flat glass surface due to an enrichment in SiO2 at the crystal fronts. This confirms that the orientation of crystals is not fixed following nucleation. KW - Fresnoite KW - Surface crystallization KW - Crystal growth KW - Crystal morphology KW - Crystal orientation KW - EBSD PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587230 DO - https://doi.org/10.3390/cryst13030475 VL - 13 IS - 3 SP - 1 EP - 17 PB - MDPI AG CY - Basel AN - OPUS4-58723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Ralf A1 - Behrens, Harald A1 - Ageo-Blanco, Boris A1 - Reinsch, Stefan A1 - Wirth, Thomas T1 - Foaming Species and Trapping Mechanisms in Barium Silicate Glass Sealants N2 - Barium silicate glass powders 4 h milled in CO2 and Ar and sintered in air are studied with microscopy, total carbon analysis, differential thermal Analysis (DTA), vacuum hot extraction mass spectroscopy (VHE-MS), Fourier-transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary-ion mass spectrometry (TOF-SIMS). Intensive foaming of powder compacts is evident, and VHE studies prove that foaming is predominantly caused by carbonaceous species for both milling gases. DTA Shows that the decomposition of BaCO3 particles mix-milled with glass powders occurs at similar temperatures as foaming of compacts. However, no carbonate at the glass surface could be detected by FTIR spectroscopy, XPS, and TOF-SIMS after heating to the temperature of sintering. Instead, CO2 molecules unable to rotate identified by FTIR spectroscopy after milling, probably trapped by mechanical dissolution into the glass bulk. Such a mechanism or microencapsulation in cracks and particle aggregates can explain the contribution of Ar to foaming after intense milling in Ar atmosphere. The amount of CO2 molecules and Ar, however, cannot fully explain the extent of foaming. Carbonates mechanically dissolved beneath the surface or encapsulated in cracks and micropores of particle aggregates are therefore probably the major foaming source. KW - Milling KW - Foaming KW - Glass powder KW - Sintering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531227 DO - https://doi.org/10.1002/adem.202100445 SN - 1438-1656 VL - 24 IS - 6 SP - 2100445-1 EP - 2100445-13 AN - OPUS4-53122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf A1 - Deubener, J. T1 - Silver dissolution and precipitation in an Na2O–ZnO–B2O3 metallization paste glass N2 - Thermally stimulated interactions between silver and glass, that is, silver dissolution as Ag+ and precipitation as Ag0 were studied in two glass series of molar target composition xAg2O–(19 − x)Na2O–28ZnO–53B2O3 with x = 0, 0.1, 0.5, 5 and (19Na2O–28ZnO–53B2O3)+yAg2O with y = 0.01, 0.05. These act as model for low-melting borate glasses being part of metallization pastes. The occurrence of metallic silver precipitates in melt-quenched glass ingots demonstrated that silver dissolved only in traces (< 0.01 mol%) in the glasses. The dissolved silver was detected by means of Raman spectroscopy and energy-dispersive X-ray spectroscopy. Increasing x in the batch could not lead to a significant increase of the silver ion fraction in the glass as possible in binary silver borate glasses. In situ observation of heated AgNO3 mixed with the base glass frit in a hot stage microscope showed that Ag0 precipitation occurs already at the solid state. At higher temperatures, small droplets of liquid silver were found to move freely within the melt, whereas coalescence caused a stepwise increase of their size. These results contribute to the understanding of formation of silver precipitates in metallization pastes described in the literature. KW - Silver metallization paste KW - Batch reactions KW - Borate KW - Glass forming melts KW - Glass manufacturing KW - Raman spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559433 DO - https://doi.org/10.1111/ijag.16613 SN - 2041-1286 SP - 1 EP - 11 PB - Wiley Online Library AN - OPUS4-55943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Silver - alkali borate glass pastes N2 - 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. T2 - GLASS MEETING 2020 CY - Online meeting DA - 07.12.2020 KW - Silver-glass metallization paste KW - Sintering KW - Alkali ions KW - Viscosity KW - Silver precipitates PY - 2020 AN - OPUS4-52871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - GlasDigital: Data-driven workflow for accelerated glass development N2 - lasses stand out by their wide and continuously tunable chemical composition and large variety of unique shaping techniques making them a key component of modern high technologies. Glass development, however, is still often too cost-, time- and energy-intensive. The use of robotic melting systems embedded in an ontology-based digital environment is intended to overcome these problems in future. As part of the German research initiative MaterialDigital, the joint project GlasDigital takes first steps in this direction. The project consortium involves the Fraunhofer ISC in Würzburg, the Friedrich Schiller University Jena (OSIM), the Clausthal University of Technology (INW), and the Federal Institute for Materials Research and Testing (BAM, Division Glasses) and aims to combine all main basic components required for accelerated data driven glass development. For this purpose, a robotic high throughput glass melting system is equipped with novel inline sensors for process monitoring, machine learning (ML)-based, adaptive algorithms for process monitoring and optimization, novel tools for high throughput glass analysis and ML-based algorithms for glass design, including software tools for data mining as well as property and process modelling. The talk gives an overview how all these tools are interconnected and illustrates their usability with some examples. T2 - HVG-DGG Fachausschuss I CY - Jena, Germany DA - 03.11.2023 KW - Glass KW - Robotic melting KW - Ontologie KW - Simulation KW - Workflow KW - Data Space PY - 2023 AN - OPUS4-60383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Ya‐Fan A1 - Arendt, Felix A1 - Bornhöft, Hansjörg A1 - de Camargo, Andréa S. S. A1 - Deubener, Joachim A1 - Diegeler, Andreas A1 - Gogula, Shravya A1 - Contreras Jaimes, Altair T. A1 - Kempf, Sebastian A1 - Kilo, Martin A1 - Limbach, René A1 - Müller, Ralf A1 - Niebergall, Rick A1 - Pan, Zhiwen A1 - Puppe, Frank A1 - Reinsch, Stefan A1 - Schottner, Gerhard A1 - Stier, Simon A1 - Waurischk, Tina A1 - Wondraczek, Lothar A1 - Sierka, Marek T1 - Ontology‐Based Digital Infrastructure for Data‐Driven Glass Development N2 - The development of new glasses is often hampered by inefficient trial‐and‐error approaches. The traditional glass manufacturing process is not only time‐consuming, but also difficult to reproduce with inevitable variations in process parameters. These challenges are addressed by implementing an ontology‐based digital infrastructure coupled with a robotic melting system. This system facilitates high‐throughput glass synthesis and ensures the collection of consistent process data. In addition, the digital infrastructure includes machine learning models for predicting glass properties and a tool for extracting patent information. Current glass databases have significant gaps in the relationships between compositions, process parameters, and properties due to inconsistent studies and nonconforming units. In addition, process parameters are often omitted, and even original literature references provide limited information. By continuously expanding the database with consistent, high‐quality data, it is aimed to fill these gaps and accelerate the glass development process. KW - Digitalisation KW - Data-driven glass development KW - Ontology PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625844 DO - https://doi.org/10.1002/adem.202401560 SN - 1527-2648 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-62584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Fast crack healing in glass-matrix composites with rigid filler percolation frameworks N2 - To ensure the durability of solid oxide fuel cell sealants, the understanding of the microstructural influence on viscous crack healing is essential. To this end, the effect of microstructure with respect to the spatial distribution of filler particles on viscous crack healing was studied with confocal laser scanning microscopy in glass-matrix composites (GMCs) made by mix-milling and sintering of sodalime magnesium silicate glass and Φ ≈ 6 vol% ZrO2 chemically inert rigid filler particles. This way, no change in Φ occurred during the crack healing treatments studied on Vickers indentation-induced radial cracks in polished GMC surfaces. Different microstructures were mimicked using different ZrO2 particle sizes for mix-milling. Unlike coarse ZrO2 particles, similar in size to the glass particle, fine ZrO2 particles, much smaller than the glass particles, form a rigid percolation framework (RPF) of ZrO2 filler particles around the former glass particles or glass particle agglomerates. For this RPF microstructure, crack healing was observed more readily as crack healing retardation phenomena like large-scale crack widening and crack tip rounding were strongly reduced, whereas narrow cracks could still heal locally within the glassy regions. KW - Crack healing KW - Glass matrix composite KW - Rigid percolation frameworks KW - Vickers indentation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625921 DO - https://doi.org/10.1111/jace.20386 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley AN - OPUS4-62592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Kiefer, P. A1 - Deubener, J. A1 - Fechtelkord, M. T1 - Water in Alkali Aluminosilicate Glasses N2 - To understand the influence of water and alkalis on aluminosilicate glasses, three polymerized glasses with varying ratios of Na/K were synthesized [(22. 5-x)Na2O-xK2O-22.5 Al2O3-55 SiO2 with x = 0, 7.5, and 11.25]. Subsequently, these glasses were hydrated (up to 8 wt% H2O) in an internally heated gas pressure vessel. The density of hydrous glasses linearly decreased with water content above 1 wt%, consistent with the partial molar volume of H2O of 12 cm3/mol. Near-infrared spectroscopy revealed that hydroxyl groups are the dominant species at water content of <4 wt%, and molecular water becomes dominating at water content of >5 wt%. The fraction of OH is particularly high in the pure Na-bearing glass compared to the mixed alkali glasses. 27Al magic angle spinning-NMR spectroscopy shows that aluminum is exclusively fourfold coordinated with some variations in the local geometry. It appears that the local structure around Al becomes more ordered with increasing K/Na ratio. The incorporation of H2O reinforces this effect. The differential thermal analysis of hydrous glasses shows a significant mass loss in the range of glass transition already during the first upscan, implying the high mobility of water in the glasses. This observation can be explained by the open structure of the aluminosilicate network and by the low dissociation enthalpy of H2O in the glasses (≈ 8 kJ/mol). The effect of the dissolved H2O on the glass transition temperature is less pronounced than for other aluminosilicate glasses, probably because of the large fraction of Al in the glasses. KW - NMR spectroscopy KW - Alkali aluminosilicate glasses KW - Water speciation KW - Glass transition KW - Infrared spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509497 DO - https://doi.org/10.3389/fmats.2020.00085 VL - 7 SP - 85 AN - OPUS4-50949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Silver in low-melting alkali zinc borate glasses N2 - Ein aktuelles Forschungsziel ist die Substitution von Bleioxid in niedrig schmelzenden Gläsern z.B. zur Anwendung in Silber-Metallisationspasten. Im Fokus steht hier die Untersuchung der Silberdiffusion in Alkali-Zink-Boratgläsern (X2O-ZnO-B2O3, X = Li, Na, K, Rb). Zudem wird der Redoxzustand des Silbers (Ag) und somit die Art der diffundierenden Silberspezies bestimmt. Hierzu wurde eine metallische Silberschicht mittels Sputterns auf Glaswürfel aufgebracht. Die Wärmebehandlung erfolgte nahe der Glasübergangstemperatur bei 470 °C über 2 h unter Luft und Stickstoffatmosphäre. Die Schichtdicke der Silberbeschichtung betrug 1.8 µm nach der Wärmebehandlung, gemessen mittels Weißlicht-Interferometer. Die Silberdiffusionsprofile wurden mittels Sekundär-Neutral-Teilchen-Massenspektrometrie gemessen. Die Diffusionskoeffizienten des Silbers liegen in der Größenordnung von ~10-14 cm2/s und unterscheiden sich nur gering in Abhängigkeit des Alkali-Ions im Glas. Mittels Fluoreszenz-Spektroskopie ließen sich gelöste Ag+-Ionen und [Agm]n+-Cluster nach der Wärmebehandlung unterscheiden. Zusätzlich konnten ausgeschiedene metallische Silber-Partikel im Natrium-enthaltenden Glas mittels Transmissionselektronenmikroskopie beobachtet werden. Diese haben einen mittleren Durchmesser von ~6 nm. N2 - 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. T2 - Living Glass Surfaces XI - Year of Glass CY - Ilmenau, Germany DA - 14.09.2022 KW - Alkali zinc borate glasses KW - Silver diffusion KW - Transmission electron microscopy KW - Fluorescence spectroscopy KW - Silver cluster PY - 2022 AN - OPUS4-55736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stargardt, Patrick A1 - Bresch, Sophie A1 - Falkenberg, Rainer A1 - Mieller, Björn T1 - Effect of Reaction Layers on Internal Stresses in Co‐Fired Multilayers of Calcium Manganate and Calcium Cobaltite N2 - A widespread recovery of waste heat requires a cost‐effective production of thermoelectric generators. Thermoelectric oxides are predestined for use at high temperatures. For manufacturing reasons, a multilayer generator design will be easily scalable and cost‐effective. To evaluate the potential of ceramic multilayer technology for that purpose, a multilayer of the promising thermoelectric oxides calcium cobaltite (Ca3Co4O9), calcium manganate (CMO, CaMnO3), and glass–ceramic insulation layers is fabricated. Cracks and reaction layers at the interfaces are observed in the microstructure. The compositions of these reaction layers are identified by energy‐dispersive X‐ray spectroscopy and X‐ray diffraction. Mechanical and thermal properties of all layers are compiled from literature or determined by purposeful sample preparation and testing. Based on this data set, the internal stresses in the multilayer after co‐firing are calculated numerically. It is shown that tensile stresses in the range of 50 MPa occur in the CMO layers. The reaction layers have only a minor influence on the level of these residual stresses. Herein, it is proven that the material system is basically suitable for multilayer generator production, but that the co‐firing process and the layer structure must be adapted to improve densification and reduce the tensile stresses in the CMO. KW - Ceramic multilayers KW - Co-firings KW - Internal stresses PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601626 DO - https://doi.org/10.1002/pssa.202300956 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-60162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aristia, Gabriela A1 - Le, Quynh Hoa A1 - Nofz, Marianne A1 - Sojref, Regine A1 - Bäßler, Ralph T1 - Study of Al2O3 Sol-Gel Coatings on X20Cr13 in Artificial North German Basin Geothermal Water at 150 °C N2 - Al2O3 has been widely used as a coating in industrial applications due to its excellent chemical and thermal resistance. Considering high temperatures and aggressive mediums exist in geothermal systems, Al2O3 can be a potential coating candidate to protect steels in geothermal applications. In this study, γ-Al2O3 was used as a coating on martensitic steels by applying AlOOH sol followed by a heat treatment at 600 °C. To evaluate the coating application process, one-, two-, and three-layer coatings were tested in the artificial North German Basin (NGB), containing 166 g/L Cl−, at 150 °C and 1 MPa for 168 h. To reveal the stability of the Al2O3 coating in NGB solution, three-layer coatings were used in exposure tests for 24, 168, 672, and 1296 h, followed by surface and cross-section characterization. SEM images show that the Al2O3 coating was stable up to 1296 h of exposure, where the outer layer mostly transformed into boehmite AlOOH with needle-like crystals dominating the surface. Closer analysis of cross-sections showed that the interface between each layer was affected in long-term exposure tests, which caused local delamination after 168 h of exposure. In separate experiments, electrochemical impedance spectroscopy (EIS) was performed at 150 °C to evaluate the changes of coatings within the first 24 h. Results showed that the most significant decrease in the impedance is within 6 h, which can be associated with the electrolyte penetration through the coating, followed by the formation of AlOOH. Here, results of both short-term EIS measurements (up to 24 h) and long-term exposure tests (up to 1296 h) are discussed. KW - Al2O3 KW - Geothermal KW - Martensitic steels KW - Behmite KW - Corrosion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525551 DO - https://doi.org/10.3390/coatings11050526 SN - 2079-6412 VL - 11 IS - 5 SP - 526 PB - MDPI CY - Basel AN - OPUS4-52555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Maaß, Robert A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal nucleation tendency and crystal surface energy obtained from bond energies and crystal lattice data N2 - We present an easy-to-apply method to predict structural trends in the internal nucleation tendency of oxide glasses. The approach is based on calculated crystal fracture surface energies derived from easily accessible diatomic bond energy and crystal lattice data. The applicability of the method is demonstrated on literature nucleation data for isochemically crystallizing oxide glasses. KW - Glass KW - Nucleation tendency KW - Fracture surface energy KW - Crystal lattice KW - Bond energy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548814 DO - https://doi.org/10.1016/j.nocx.2022.100093 SN - 2590-1591 VL - 14 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-54881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzer, Marco A1 - Johansen, Sidsel M. A1 - Christensen, Johan F.S. A1 - Smedskjaer, Morten M. A1 - Cicconi, Maria Rita A1 - de Ligny, Dominique A1 - Müller, Ralf A1 - de Camargo, Andrea S.S. A1 - Maaß, Robert T1 - Direct connection between secondary relaxation mode and fracture toughness in alkali-aluminosilicate glasses N2 - Oxide glasses are intrinsically brittle, lacking sufficient atomic-scale mechanisms that can relax mechanical stresses in the vicinity of a propagating crack. As a result, fracture is typically well-captured by considering local bond rupture at the crack tip. Here we demonstrate that barrier energies related to the low-temperature 𝛾-relaxation mode in alkali-aluminosilicate glasses are inversely related to the fracture toughness measured via standardized three-point bending fracture experiments. This holds true for both a series with varying cations (Li, Na, K) and one with varying Li concentration. The structural rationale for this finding is gained via Raman spectroscopy. The findings suggest that a fundamental structural relaxation mode measured on bulk specimens can serve as an effective guideline for fracture toughness of oxide glasses. Data for additional silicate glasses support this conclusion. KW - Fracture toughness KW - Oxide glass KW - Mechanical properties KW - Alkali-aluminosilicate glasses KW - Internal friction PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651540 DO - https://doi.org/10.1016/j.mtadv.2025.100669 SN - 2590-0498 VL - 29 SP - 1 EP - 10 PB - Elsevier Ltd. CY - Amsterdam, Niederlande AN - OPUS4-65154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzer, Marco T1 - Glass fracture surface energy calculated from crystal structure and bond-energy data N2 - Enhancing the fracture toughness is still one of the major challenges in the field of oxide glasses. To screen different glass systems for promising candidates, a theoretical expression for the fracture surface energy, G, linked to the fracture toughness, KIc, is thus of interest. Extending our earlier work on nucleation and surface energies [1], we present a simple approach for predicting the fracture surface energy of oxide glasses, G using readily available crystallographic structure data and diatomic bond energies. The proposed method assumes that G of glass equals the surface fracture energy of the weakest fracture (cleavage) plane of the isochemical crystal. For non-isochemically crystallizing glasses, an average G is calculated from the weighed fracture energy data of the constitutional crystal phases according to Conradt [2]. Our predictions yield good agreement with the glass density- and chemical bond energy-based prediction model of Rouxel [3] and with experimentally obtained G values known at present. [1] C. Tielemann, S. Reinsch, R. Maass, J. Deubener, R. Müller, J. Non-Cryst. Solids 2022, 14, 100093 [2] R. Conradt, J. Non-Cryst. Solids 2004, 345-346, 16 [3] R., Tanguy, Scripta Materialia 2017, 109-13, 137 T2 - DPG Spring Meeting of the Condensed Matter Section CY - Dresden, Germany DA - 26.03.2023 KW - Fracture Toughness KW - Oxide Glasses KW - Surface Energy PY - 2023 AN - OPUS4-58414 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Waitelonis, Jörg A1 - Birkholz, Henk A1 - Jung, Matthias A1 - Schilling, Markus A1 - v. Hartrott, Philipp A1 - Bruns, Marian A1 - Schaarschmidt, Jörg A1 - Beilke, Kristian A1 - Mutz, Marcel A1 - Nebel, Vincent A1 - Königer, Veit A1 - Beran, Lisa A1 - Kraus, Tobias A1 - Vyas, Akhilesh A1 - Vogt, Lars A1 - Blum, Moritz A1 - Ell, Basil A1 - Chen, Ya‐Fan A1 - Waurischk, Tina A1 - Thomas, Akhil A1 - Durmaz, Ali Riza A1 - Ben Hassine, Sahar A1 - Fresemann, Carina A1 - Dziwis, Gordian A1 - Beygi Nasrabadi, Hossein A1 - Hanke, Thomas A1 - Telong, Melissa A1 - Pirskawetz, Stephan A1 - Kamal, Mohamed A1 - Bjarsch, Thomas A1 - Pähler, Ursula A1 - Hofmann, Peter A1 - Leemhuis, Mena A1 - Özçep, Özgür L. A1 - Meyer, Lars‐Peter A1 - Skrotzki, Birgit A1 - Neugebauer, Jörg A1 - Wenzel, Wolfgang A1 - Sack, Harald A1 - Eberl, Chris A1 - Portella, Pedro Dolabella A1 - Hickel, Tilmann A1 - Mädler, Lutz A1 - Gumbsch, Peter T1 - Concepts for a Semantically Accessible Materials Data Space: Overview over Specific Implementations in Materials Science N2 - This article describes advancements in the ongoing digital transformation in materials science and engineering. It is driven by domain‐specific successes and the development of specialized digital data spaces. There is an evident and increasing need for standardization across various subdomains to support science data exchange across entities. The MaterialDigital Initiative, funded by the German Federal Ministry of Education and Research, takes on a key role in this context, fostering collaborative efforts to establish a unified materials data space. The implementation of digital workflows and Semantic Web technologies, such as ontologies and knowledge graphs, facilitates the semantic integration of heterogeneous data and tools at multiple scales. Central to this effort is the prototyping of a knowledge graph that employs application ontologies tailored to specific data domains, thereby enhancing semantic interoperability. The collaborative approach of the Initiative's community provides significant support infrastructure for understanding and implementing standardized data structures, enhancing the efficiency of data‐driven processes in materials development and discovery. Insights and methodologies developed via the MaterialDigital Initiative emphasize the transformative potential of ontology‐based approaches in materials science, paving the way toward simplified integration into a unified, consolidated data space of high value. KW - Semantic Interoperability KW - Data Spaces KW - Integration Workflows KW - MaterialDigital PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622952 DO - https://doi.org/10.1002/adem.202401092 SN - 1527-2648 SP - 1 EP - 25 PB - Wiley-VCH CY - Weinheim AN - OPUS4-62295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aristia, Gabriela A1 - Bäßler, Ralph A1 - Nofz, Marianne A1 - Sojref, Regine A1 - Kohl, Anka T1 - Short-term exposure tests of ɣ-Al2O3 Sol-gel coating on X20Cr13 in artificial geothermal waters with different pH N2 - The suitability of an Al2O3 coating for corrosion protection on X20Cr13 was evaluated in various artificial geothermal brines, focusing on the influence of different pH (4, 6 and 8) and their chemical compositions on the coating properties. All experiments were performed in the laboratory using autoclaves at 150 ◦C and 1 MPa in deaerated condition for 1 and 7 days. Results showed that the pH of geothermal waters is the most detrimental factor in the transformation of ɣ-Al2O3 and its protective abilities. Delaminations were found in the Coating exposed to geothermal brines with pH 4. FTIR spectra indicated a transformation of ɣ-Al2O3 to boehmite AlOOH after exposure to pH 4 and 6, and bayerite Al(OH)3 was formed after exposure to pH 8. Different Crystal structures of the hydrated Al2O3 also contribute to the stability of the coatings, observed by the SEM- EDX of the surface and cross-section of coatings. This study indicated that ɣ-Al2O3 sol-gel coating presents a promising aspect of corrosion protection in geothermal environment with a neutral pH. KW - Al2O3 KW - Corrosion KW - Coating KW - Martensitic steel PY - 2021 DO - https://doi.org/10.1016/j.geothermics.2021.102193 SN - 0375-6505 VL - 96 SP - 102193 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fotheringham, U. T1 - Digitalization of Glass Development N2 - Im Vortrag werden erste Ergebnisse aus dem vom BMFTR im Rahmen der MaterialDigital Initiative geförderten Projekt „GlasAgent“ vorgestellt, welches die Glasentwicklung mittels KI vorantreiben soll. In diesem Projekt werden mehrere Entwicklungszyklen inklusive des Recyclingprozesses durchlaufen und die Ergebnisse genutzt, um Datenbanken und Modelle zu verbessern. Mit diesen verknüpft und basierend auf der semantischen GlasDigital-Ontologie soll zukünftig ein Chatbot die Glasentwicklung schneller, präziser und nachhaltiger gestalten. T2 - PMD Vollversammlung CY - Berlin, Germany DA - 26.11.2025 KW - Glass KW - Workflow KW - Automation KW - MAP KW - Ontology KW - Simulation KW - Database PY - 2025 AN - OPUS4-65039 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzer, Marco A1 - Waurischk, Tina A1 - George, Janine A1 - Maaß, Robert A1 - Müller, Ralf T1 - Silicate glass fracture surface energy calculated from crystal structure and bond-energy data N2 - We present a novel method to predict the fracture surface energy, γ, of isochemically crystallizing silicate glasses using readily available crystallographic structure data of their crystalline counterpart and tabled diatomic chemical bond energies, D0. The method assumes that γ equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were in excellent agreement with those calculated from glass density, network connectivity and D0 data in earlier work. This finding demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces. KW - Glass KW - Fracture surface energy KW - Toughness KW - Modeling KW - Mechanical properties PY - 2023 DO - https://doi.org/10.1016/j.jnoncrysol.2023.122679 SN - 0022-3093 VL - 622 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-58767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzer, Marco T1 - A new model for predicting fracture surface energies in oxide glasses - How cleavage planes help us understand the intrinsic fracture toughness of oxide glasses N2 - The search for strong and tough oxide glasses is important for making safer, more environmentally friendly, thinner glass products. However, this task remains generally difficult due to the material’s inherent brittleness. In search for tougher glasses, fracture toughness (KIC) prediction models are helpful tools to screen for promising candidates. In this work, a novel model to predict KIC via the fracture surface energy, γ, is presented. Our approach uses readily available crystallographic structure data of the glass’s isochemical crystal and tabled diatomic chemical bond energies, D0. The method assumes that γ of a glass equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were not only in excellent agreement with those calculated with a former well-working model, but also demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces. Finally, the effectiveness of fracture toughness enhancement by chemical substitution is discussed based on our results and alternative toughening strategies will be suggested. T2 - Deparment Seminar Materials Engineering CY - Berlin, Germany DA - 15.06.2023 KW - Fracture Toughness KW - Oxide Glasses KW - Fracture Mechanics KW - Silicate Glasses KW - Phase Separation PY - 2023 AN - OPUS4-58419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzer, Marco T1 - Fracture surface energy of glasses obtained from crystalline structure and bond energy data N2 - The search for strong and tough oxide glasses is important for making safer, environment-friendlier, thinner glasses. As fracture toughness experiments in brittle materials are complicated and time-consuming , modelling glass fracture surface energy, G, and fracture toughness, KIc, is of interest for screening promising candidates. Inspired by Rouxel´s idea of preferred crack growth along cutting weakest bonds within a glass structure and a study by Tielemann et al. , which indicates a correlation between crystal fracture surface and glass-crys¬tal interfacial energies, we present a new approach for predicting G. Combining both ideas, we used diatomic bond energies and readily available crystallographic structure data for estimating G. The proposed method assumes that G of the glass equals the surface fracture energy of the cleavage plane in its respective isochemical crystal. We calculated G- values for more than 25 iso-chemical silicate systems and compared them to calculated values from Rouxel’s widely used procedure, which is well working and based on glass densities and chemical bond energies. Not only does our model yields good agreement with [3], but it also enables an estimation for glasses with unknown density and can therefore contribute to broaden the data basis for glass property modelling tools. Most interestingly, however, this agreement indicates an interesting similarity between cleavage planes in a crystal and its corresponding glass state in terms of fracture processes. T2 - DGG-USTV Joint annual meeting 2023 CY - Orleans, France DA - 22.05.2023 KW - Fracture Toughness KW - Oxide Glasses KW - Surface Energy KW - Silicate Glasses PY - 2023 AN - OPUS4-58416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Aristia, Gabriela A1 - Nofz, Marianne A1 - Bäßler, Ralph A1 - Sojref, Regine A1 - Le, Quynh Hoa T1 - Preliminary Study on Al2O3 Sol-Gel Coating for Corrosion Protection of Martensitic Stainless Steel in Artificial Geothermal Water N2 - Al2O3 coatings are often used as protective layers on steels against electrochemical and high-temperature corrosion because they are chemically inert and stable at elevated temperatures. This study presents preliminary work on the possibilities of using Al2O3 sol-gel coatings for corrosion protection of martensitic stainless steels in geothermal environments. Al2O3 sol-gel coatings were applied on UNS S42000, which is known to be susceptible to uniform and localized corrosion. The coated steel specimens were then tested in two types of artificial geothermal water, which simulate the geothermal fluids found in Sibayak (SBY), Indonesia, and North German Basin (NGB), Germany, respectively. SBY has pH 4 and 1.5 g/L of chloride ions, whereas NGB has a pH of 6 and 166 g/L of chloride ions. All experiments were carried out in autoclaves at 150 °C and 1 MPa under the deaerated condition. Evaluations were performed by investigating the surface profiles of both uncoated and coated steels before and after the corrosion test using a Laser Scanning Microscope (LSM) and Scanning Electron Microscope (SEM). Finally, Electrochemical Impedance Spectroscopy (EIS) was performed to compare the corrosion resistance of Al2O3 coated steels in SBY and NGB solutions. It was observed from the corrosion test that Al2O3 coatings are more suitable for use in the geothermal water with a higher pH. T2 - AMPP Annual International Corrosion Conference 2021 CY - Online Meeting DA - 19.04.2021 KW - Protective coating KW - Sol-gel coating KW - Geothermal KW - Martensitic steel KW - Corrosion PY - 2021 SP - 16777-01 EP - 16777-12 CY - Houston AN - OPUS4-52501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hickel, Tilmann A1 - Waske, Anja A1 - Tehranchi, Ali A1 - Bhattacharya, Biswajit A1 - Stawski, Tomasz M. A1 - Fellinger, Tim-Patrick A1 - Mehmood, Asad A1 - Witt, Julia A1 - Ozcan, Ozlem A1 - Guilherme Buzanich, Ana A1 - Kumar, Sourabh A1 - Mishra, Rajesh Kumar A1 - Holzer, Marco A1 - Stucchi de Camargo, Andrea Simone A1 - Agudo Jácome, Leonardo A1 - Manzoni, Anna A1 - Fantin, Andrea A1 - John, Elisabeth A1 - Hodoroaba, Vasile-Dan A1 - Bührig, Sophia A1 - Murugan, Jegatheesan A1 - Marschall, Niklas A1 - George, Janine A1 - Darvishi Kamachali, Reza A1 - Maaß, Robert A1 - Emmerling, Franziska T1 - Chemically complex materials enable sustainable high-performance materials N2 - Chemically complex materials (CCMats) 􀀀 including high-entropy alloys, oxides, and related multi-principal element systems 􀀀 offer a paradigm shift in materials design by leveraging chemical diversity to simultaneously optimize functional, structural, and sustainability criteria. The vastness of the compositional and structural space in CCMats propels the field into an expanding exploratory state. To reconcile functional and structural performance across this immense parameter space remains an open challenge. This Perspective evaluates the opportunities and challenges associated with harnessing chemical complexity across a broad spectrum of applications, such as hydrogen storage, ionic conductors, catalysis, magnetics, dielectrics, semiconductors, optical materials, and multifunctional structural systems. It is delineated how three central design strategies: targeted substitution (SUB), defect engineering (DEF), and diversity management (DIV) enable the reconciliation of high functional performance with long-term structural stability and environmental responsibility. Advances in computational thermodynamics, microstructure simulations, machine learning, and multimodal characterization are accelerating the exploration and optimization of CCMats, while robust data infrastructures and automated synthesis workflows are emerging as essential tools for navigating their complex compositional space. By fostering cross-disciplinary knowledge transfer and embracing data-driven design, CCMats are poised to deliver next-generation materials solutions that address urgent technological, energy, and environmental demands. KW - Chemically complex materials KW - Structural stability KW - Functional performance KW - Design strategies KW - Sustainability PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655598 UR - https://www.sciencedirect.com/science/article/pii/S1359028626000033?via%3Dihub DO - https://doi.org/10.1016/j.cossms.2026.101256 SN - 1359-0286 VL - 42 SP - 1 EP - 26 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-65559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Silver diffusion in low-melting alkali zinc borate model glasses studied by means of SNMS, TEM and XAS N2 - 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. T2 - 94. Glastechnische Tagung CY - Online meeting DA - 10.05.2021 KW - Silver diffusion KW - Alkali zinc borate glass KW - Metallic silver precipitates KW - Phase separation PY - 2021 AN - OPUS4-52861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chahal, Shweta T1 - Sustainable Synthesis of Na+ and Bi3+ - doped Cs₂AgInCl₆ Double Perovskites for Efficient White-Light Emission N2 - Double halide perovskites have emerged as promising, less-toxic alternatives to lead-based perovskites for diverse photochemical applications. Among them, Cs₂AgInCl₆ has attracted significant attention, particularly when doped with various elements, which induce self-trapped exciton (STE) states within the bandgap, resulting in efficient white-light emission and a remarkable enhancement of photoluminescence quantum yield (PL QY). While several solid-state and solution-based methods have been employed for the synthesis of double halide perovskites, many rely on toxic solvents and complex procedures, hindering scalability. In this study, we present two environmentally friendly synthesis approaches for the preparation of Cs₂AgInCl₆ doped with monovalent (Na⁺) and trivalent (Bi³⁺) cations: 1. Green solution-based method: Utilizes mild reagents and entirely replaces harsh chemicals, enabling synthesis at ambient conditions. 2. Mechanochemical approach: Employs high-energy ball milling for 62 minutes at room temperature to obtain the desired crystalline phase. These green methodologies provide sustainable and scalable alternatives to conventional routes, minimizing the environmental footprint. We systematically compare the structural and optical properties of the doped perovskites synthesized via both approaches. The resulting materials exhibit strong UV absorption, broadband white-light emission, high PL QY (up to 85%, Fig. 1), long PL lifetimes, and good thermal and environmental stability (up to 300 °C in air). These results highlight the potential of doped Cs₂AgInCl₆ double perovskites as an eco-friendly material with possible photonic applications as in white-light devices. T2 - eMRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Fluorescence KW - Advanced material KW - Perovskite KW - Synthesis KW - Characterization KW - Fluorescence quantum yield KW - Absolute KW - Integrating sphere spectroscopy KW - Sustainable synthesis KW - Lifetime KW - Photophysics PY - 2025 AN - OPUS4-64185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal friction and energy dissipation during fracture in silicate glasses N2 - To obtain a deeper insight into the nature of energy dissipation during fracture, the internal friction of 13 borosilicate, aluminosilicate, soda-lime, and lead-containing glasses, for which inert crack growth data are known, was measured using dynamic mechanical thermal analysis. For asymmetrically bent glass beams, the loss tangent, tan δ, was determined between 0.2 and 50 Hz at temperatures between 273 K and the glass transition temperature, Tg. It was found that the area under the tan δ vs T·Tg−1 curve correlates with the crack growth exponent, n, in the empirical v = v0·KIn relation between crack growth velocity, v, and stress intensity, KI, which indicates that n correlates with the degree of energy dissipation of sub-Tg relaxation phenomena. KW - Glass KW - Internal friction KW - Crack growth PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651371 DO - https://doi.org/10.1063/5.0255432 SN - 0021-9606 VL - 162 IS - 19 SP - 1 EP - 9 PB - AIP Publishing AN - OPUS4-65137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pan, Z. A1 - Waurischk, Tina A1 - Duval, A. A1 - Müller, Ralf A1 - Deubener, J. A1 - Krishnan, N. M. A. A1 - Wondraczek, K. A1 - Wondraczek, L. T1 - Precise Real‐Time Measurement of Liquid Viscosity Using Digital Video Data N2 - Quantitative knowledge of liquid viscosity is of fundamental importance in many areas of materials synthesis and processing. However, the determination of viscosity often relies on specialized experimental equipment, offline experimentation, or invasive procedures, in particular when required in extreme conditions such as at high temperature, high pressure, and in confined or corrosive environments. Here, this study proposes and validates a fast and simple method that mimics the intuitive perception of liquid flow within a quantitative framework. For this, this study employs digital video observation to derive quantitative values of the shear viscosity of liquids, with high precision and rapid acquisition rates. The technique involves capturing liquid dynamics after minor mechanical stimulation. Processed imaging data are indexed by similarity and referenced to a digital database generated with a finite element model, from which values of viscosity are obtained in line. The approach is tested on water at room temperature and on a high‐temperature glass melt. Covering a viscosity range of four orders of magnitude, both yield convincing agreement with tabulated reference data at low computational cost. KW - Glass KW - Liquid Viscosity KW - Digital Video Data KW - Finite Element Method PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651363 DO - https://doi.org/10.1002/aisy.202500297 SN - 2640-4567 VL - 7 IS - 12 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-65136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Santos Baltieri, Ricardo T1 - Luminescence Thermometry in Pure TeO₂ Glasses Doped with Er3+/Yb3+ and Eu3+: Remote Sensing Capability Across the Biological Temperature Range N2 - The development of non-contact and remote temperature sensors based on rare-earth (RE3+)-doped glasses is crucial for emerging applications in biomedical diagnostics and microscale thermal monitoring. In this study, we explore the fundamental thermometric properties of pure tellurite (TeO2) glasses doped with either Er3+/Yb3+ or Eu3+ ions in a wide range of temperature. The Er3+/Yb3+-co-doped system was analyzed through upconversion emission thermometry, particularly involving thermally coupled levels 2H11/2 and 4S3/2. The intensity ratio between these levels exhibits a clear temperature dependence from 100 K to 530 K, with an inversion near 160 K and optimal sensitivity above 250 K. At 300 K, the relative sensitivity (SR) reached 1.1% K−1, and the absolute sensitivity peaked at 6.5 × 10−3 K−1 at 460 K. Figure on the left is the Er3+ upconversion luminescence dependency on temperature, in the center is the excitation spectra of Eu3+ with temperature, and on the right is the comparison between calculated and measured temperature for Eu3+ samples. In parallel, the excitation spectra of Eu3+-doped TeO2 glasses were acquired from 100 K to 520 K, revealing three thermally responsive spectral regions. These transitions exhibited temperature-dependent intensity inversions, enabling the use of excitation-based thermometry. Notably, one of the regions provided the most accurate temperature predictions, with a relative sensitivity of 0.5% K−1 at 300 K. Both systems benefit from the high optical transparency, chemical stability, and low phonon energy of pure TeO2 glass, making them ideal candidates for remote sensing platforms, such as fiber-optic tips or implantable probes. While the Er3+/Yb3+ system provides robust upconversion emission for conventional thermometry, the Eu3+ system introduces an innovative excitation-based strategy, broadening the applicability of RE3+-doped tellurite glasses for optical thermometry. Acknowledgements This work was supported by the São Paulo Research Foundation (FAPESP – N. 2020/11038-2, 2023/05994-6, 2024/04675-7) and National Council for Scientific and Technological Development (CNPq - 304718/2023-8). T2 - Shift 2025 Conference CY - Tenerife, Spain DA - 13.10.2025 KW - Lanthanide KW - Optical thermometry KW - Energy conversion PY - 2025 AN - OPUS4-65195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meira, Maria Fernanda Cavalcante A1 - Fernandes, Gabriela Leal Peres A1 - de Camargo, Andréa Simone Stucchi A1 - Ravaro, Leandro Piaggi A1 - Arai, Marylyn Setsuko A1 - Navarro, Maria Fidela de Lima A1 - Brighenti, Fernanda Lourenção A1 - Oliveira, Analú Barros de A1 - Danelon, Marcelle ED - Stucchi de Camargo, Andrea T1 - Modification of restorative glass ionomer cement with zinc oxide nanoparticles and calcium glycerophosphate microparticles: in vitro assessment of mechanical properties and antimicrobial activity N2 - Abstract The incorporation of bioactive agents into resin-modified glass ionomer cement (RMGIC) is a promising strategy to improve its mechanical strength and biofilm control, especially for patients with active dental caries. Objective This study aimed to evaluate the effects of incorporating ZnONPs and CaGP into RMGIC on its mechanical and microbiological properties. Design Six groups were tested: 1) RMGIC (without CaGP/ZnONPs); 2) RMGIC-1.0%ZnONPs; 3) RMGIC-2.0%ZnONPs; 4) RMGIC-3.0%CaGP; 5) RMGIC-3.0%CaGP-1.0%ZnONPs; and 6) RMGIC-3.0%CaGP-2.0%ZnONPs. The compressive strength (CS), diametral tensile strength (DTS), and surface hardness (SH) were evaluated after 24 hours and 7 days. Antimicrobial and antibiofilm activity were evaluated using agar diffusion and biofilm metabolic activity (XTT) assays. Results After 24 hours, all the groups showed similar DTS values (p0.05), except for RMGIC-3.0%CaGP-1.0%ZnONPs, which showed the highest DTS value (p<0.05). Comparing 24 hours and 7 days, the DTS values of RMGIC-3.0%CaGP-2.0%ZnONPs, RMGIC-3.0%CaGP, and RMGIC-3.0%CaGP-2.0%ZnONPs were similar (p=0.360). After 24 hours, the RMGIC group showed the CS highest value, followed by RMGIC-2.0%ZnONPs (p < 0.05). After 7 days, the RMGIC-3.0%CaGP-1.0%ZnONPs group exhibited the highest CS value, approximately 15% higher than RMGIC (p<0.05). The RMGIC-1.0%ZnONPs group exhibited significantly higher SH at 24 hours (p=0.621). At 7 days, the highest SH value was observed for the RMGIC-3.0%CaGP-1.0%ZnONPs group (p<0.05). Regarding antimicrobial and antibiofilm activity, including results from biofilm metabolism assays, the RMGIC-3.0%CaGP-1.0%ZnONPs group demonstrated the most effective antimicrobial and inhibitory effects (p<0.05). Conclusion This study demonstrated that adding ZnONPs and CaGP to RMGIC enhanced its mechanical and antimicrobial and antibiofilm properties, suggesting enhanced mechanical performance and improved protection against cariogenic biofilms—critical factors for successful restorative treatments. Therefore, the addition of ZnONPs and CaGP is a promising strategy to develop advanced restorative materials that improve clinical outcomes, especially for patients with active dental caries. KW - Resin-modified glass ionomer cement KW - Phosphate KW - Zinc oxide nanoparticles KW - Biofilm KW - Mechanical properties PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652799 DO - https://doi.org/10.1590/1678-7757-2025-0356 SN - 1678-7765 VL - 33 SP - 1 EP - 14 PB - FapUNIFESP (SciELO) AN - OPUS4-65279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arai, Marylyn S. A1 - Brambilla, Gabriel V. A1 - Corrêa, Bruna Carolina A1 - Merízio, Leonnam G. A1 - Inada, Natalia M. A1 - de Camargo, Andrea S. S. T1 - A Dual-Mode “Turn-On” Ratiometric Luminescent Sensor Based on Upconverting Nanoparticles for Detection and Differentiation of Gram-Positive and Gram-Negative Bacteria N2 - Infectious bacterial diseases, intensified by antibiotic resistance, cause millions of deaths annually and pose risks beyond human health, including water and food contamination. Current diagnostics are often slow, require complex equipment, and lack specificity, highlighting the need for rapid and reliable detection methods. To address this, we developed a luminescent sensor based on NaYF4 upconverting nanoparticles (UCNPs) doped with Er3+ or Tm3+, coated with COOH-PEG4-COOH, and functionalized with vancomycin (Van) or polymyxin-B (Poly) to selectively target Gram-positive and Gram-negative bacteria, respectively. Gold nanoparticles (AuNPs) served as quenchers, enabling a ratiometric “turn-on” mechanism: upon bacterial binding, the UCNP emission, initially quenched by AuNPs, was partially restored. This allowed Differentiation through changes in the green/red (G/R) ratio for Er-UCNP@PEG4-Van and the blue/red (B/R) ratio for Tm-UCNP@PEG4-Poly. The sensor distinguished between Gram-positive and Gram-negative bacteria over a wide concentration range (0.05 to 5 × 105 CFU/mL) and showed high correlation with actual bacterial counts (r = 0.99 for S. aureus, r = 0.91 for E. coli). This platform is a potential fast, selective, and reliable tool for bacterial detection in clinical and environmental settings. KW - Lminescent sensor KW - Upconverting nanoparticles KW - Gram-positive and Gram-negative bacteria KW - Ratiometric luminescent sensors PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652785 DO - https://doi.org/10.1021/acsomega.5c07006 SN - 2470-1343 VL - 10 IS - 39 SP - 46040 EP - 46050 PB - American Chemical Society (ACS) AN - OPUS4-65278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arai, Marylyn Setsuko A1 - Machado, Thales Rafael A1 - da Silva, Beatriz Giacomelli Rodrigues A1 - Vilela, Raquel Riciati do Couto A1 - de Camargo, Andrea Simone Stucchi A1 - Zucolotto, Valtencir T1 - Biomimetic Upconverting Nanoplatforms for Glioblastoma Bioimaging and Targeted Therapy N2 - Infectious bacterial diseases, intensified by antibiotic resistance, cause millions of deaths annually and pose risks beyond human health, including water and food contamination. Current diagnostics are often slow, require complex equipment, and lack specificity, highlighting the need for rapid and reliable detection methods. To address this, we developed a luminescent sensor based on NaYF4 upconverting nanoparticles (UCNPs) doped with Er3+ or Tm3+, coated with COOH-PEG4-COOH, and functionalized with vancomycin (Van) or polymyxin-B (Poly) to selectively target Gram-positive and Gram-negative bacteria, respectively. Gold nanoparticles (AuNPs) served as quenchers, enabling a ratiometric “turn-on” mechanism: upon bacterial binding, the UCNP emission, initially quenched by AuNPs, was partially restored. This allowed differentiation through changes in the green/red (G/R) ratio for Er-UCNP@PEG4-Van and the blue/red (B/R) ratio for Tm-UCNP@PEG4-Poly. The sensor distinguished between Gram-positive and Gram-negative bacteria over a wide concentration range (0.05 to 5 × 105 CFU/mL) and showed high correlation with actual bacterial counts (r = 0.99 for S. aureus, r = 0.91 for E. coli). This platform is a potential fast, selective, and reliable tool for bacterial detection in clinical and environmental settings. KW - Glioblastoma KW - Homotypic targeting KW - Cell membrane coating KW - Upconverting nanoparticles KW - Temozolamide KW - Near infrared bioimaging KW - Drug delivery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652808 DO - https://doi.org/10.1021/acsanm.5c04567 SN - 2574-0970 VL - 10 IS - 39 SP - 1 EP - 13 PB - American Chemical Society (ACS) AN - OPUS4-65280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea A1 - Arai, Marylyn Setsuko T1 - Upconversion nanoparticles for chemical, physical and biological sensing: from functionalization to point-of-care devices N2 - Among several applications, versatile upconversion nanoparticles (UCNPs) which can convert lower-energy infrared radiation into higher-energy visible or ultraviolet light, have emerged as one of the most powerful tools in the field of chemical, physical and biological sensing. The use of UCNPs in fluorescent sensors allows non-invasive, highly sensitive, and selective detection methods, which are particularly beneficial in environments requiring minimal interference and high precision for analytes that can range from metal ions to biomolecules. In this lecture, an overview and the state of the art will be given, accompanied by examples of our recent contributions to key areas such as chronic disease diagnostics, bacterial sensing, and multifunctionally responsive nanoplatforms: (1) An Enhanced Luminescence Lateral-Flow Assay (ELLA) designed for rapid (< 15 min) and early detection of acute kidney injury biomarkers in urine samples, using a commercial cell phone camera, will be presented. The platform is based on Er³⁺- and Tm³⁺-doped UCNPs whose emissions intensities are 40-fold enhanced by an Au-coated mesoporous silica shell, enabling the accurate detection of KIM-1 and NGAL biomarkers with detection limits as low as 0.23 ng/mL; (2) Also, a multifunctional nanoplatform that combines Tm³⁺-doped UCNPs with a Cu(I) complex for applications in oxygen sensing, optical thermometry, and emission colour tuning will be presented. The platform utilizes Luminescent Resonance Energy Transfer (LRET) to achieve efficient energy transfer, enabling red emission from the Cu(I) complex while allowing the use of the UCNP’s original emissions for thermometry. The dual functionality allows sensitive O2 detection and temperature measurements, with relative sensitivities of up to 1% K⁻¹; (3) The critical challenge of rapid bacterial detection and differentiation was addressed by the development of a novel UCNP-based sensor. By functionalizing UCNPs with the antibiotics - vancomycin for Gram-(+) and polymyxin-B for Gram-(-), and using Au nanoparticles as intensity quenchers, the sensor leverages a ratiometric "turn-on" mechanism for selective detection of the bacteria, through changes in the green/red (G/R) ratio for Er-UCNP@PEG4-Van, and blue/red (B/R) ratio for Tm-UCNP@PEG4-Poly. By this approach, differentiation was possible over a wide concentration range of bacteria (0.05 to 5 x 105 CFU/mL) with high correlation with actual bacterial counts (r = 0.99 for S. aureus, r = 0.91 for E. coli); (4) Recently, we have demonstrated a water dispersable ratiometric pH-nanosensor based on host-guest interaction of Tm3+/Yb3+ co-doped UCNPs functionalized with b-cyclodextrin (b-CD) and a pH-responsive nitrobenzoxadiazol dye modified with adamantane (NBD-Ad). The sensor shows a ratiometric emission response (blue/red) over a pH range of 8.0 – 11.0 with high reproducibility, excellent reusability and selectivity, even in the presence of interferents. Together, the presented examples highlight the versatility and potential of UCNPs to develop novel sensors, offering measurable advances in diagnostics, environmental monitoring, and beyond. T2 - Shift2025 - Spectral shaping for biomedical and energy applications CY - Tenerife, Spain DA - 13.10.2025 KW - Upconverting nanoparticles KW - Fluorescent sensors KW - Point-of-care devices PY - 2025 AN - OPUS4-65282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea T1 - Enhanced emission of Nd3+ by localized silver nanocluster growth via direct laser writing in Ga-fluoride phosphate glasses N2 - Gallium fluoride phosphate glasses are promising materials for optical applications in the visible to near infrared spectra due to their wide transmission window and ability to accommodate optically active dopants. In this study, melt quenched glasses in the compositional system 25Ga(PO₃)₃–20ZnF₂–30BaF₂–(25–x–y)SrF₂–xAgNO₃–yNdF₃ (x = 0 -10 mol%, y = 0 or 1 mol%) were studied and fully characterized by conventional and spectroscopic techniques to understand the interaction of silver species and Nd³⁺ ions. In Ag+ doped samples, the observation of a broad emission band in the visible spectrum evidences the overlapping presence of Ag⁺, Ag nanoclusters (NCs), and [Ag₂]²⁺ species. In the sample doped with 10 mol% Ag⁺, the development of a dark yellow color and alterations in the emission profile suggest the formation of Ag nanoparticles. In an attempt to control and increase the formation of Ag nanoclusters in a localized way, the glasses with 3 and 5 mol% Ag+ were subjected to direct laser writing (DLW) with femtosecond laser pulses at variable inscription intensities and scan speeds. As expected, the approach led to localized growth of Ag-NCs with precise spatial control and as a consequence, the Nd³⁺ emissions in the NIR region (e.g. at1060 nm) were significantly enhanced in laser-structured regions as compared to unmodified areas, evidencing efficient energy transfer from silver species to Nd³⁺ ions. These results demonstrate that DLW, applied for the first time in these glasses, enables precise spatial control over silver nanocluster formation, offering a viable route to process optical glasses for photonic applications. T2 - XXIII - B-MRS Meeting CY - Salvador, Brazil DA - 28.09.2025 KW - Fluoride phosphate glasses KW - Direct laser writting KW - Neodymium KW - Silver nanoclusters PY - 2025 AN - OPUS4-65281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shasmal, Nilanjana T1 - Effects of Direct femtosecond laser writing on chloroborosilicate glasses doped with Eu3+/Eu2+ and CdS quantum dots N2 - Femtosecond (fs) direct laser writing (DLW) is a promising technique for developing nano-inhomogeneous materials with advanced optical properties and for fabricating novel photonic devices such as integrated waveguides, ultrafast optical switches, phase plates, and 3D optical memory. In this study, DLW was applied to chloroborosilicate glasses that were singly and co-doped with Eu and CdS quantum dots (QDs). The glasses were laser-treated within a very narrow range of experimental conditions, resulting in laser-inscribed sites exhibiting enhanced emission, similar to the glass-ceramics crystallized from the as-prepared glass. In the regions crystalized by DLW a significant reduction of Eu3+ to Eu2+ was verified by photoluminescence spectroscopy. However, the characteristics of the emission bands of Eu2+ changed markedly in the laser-treated sites as compared to the emission spectra of the same glass crystallized by heat treatment. A considerable redshift and splitting of the emission band were observed, attributed to changes in the surrounding environment of the rare earth (RE) ions which was, in turn, attributed to an alteration in the coordination number of Ba2 + and/or Eu2+ as a result of the high-power laser treatment. Although there was an issue with homogeneity of the glass in the micro-level, which restricts some of the aspects of the DLW, these findings suggest the potential for structural modifications through laser treatment, which could be harnessed to create new functionalities for advanced optical applications. T2 - ICG 2025 (27th International Congress on Glass) CY - Kolkata, India DA - 20.01.2025 KW - Femtosecond direct laser writing KW - DLW KW - CdS quantum dots KW - Eu/CdS co-doped glass PY - 2025 AN - OPUS4-65285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abel, Andreas A1 - Rosalie, Julian A1 - Reinsch, Stefan A1 - Zapala, Pawel A1 - Michels, Heiner A1 - Skrotzki, Birgit T1 - Influence of Mo and B additions in intermetallic near-Fe3Al alloys on microstructure and mechanical properties N2 - Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms. KW - Materials Chemistry KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials KW - General Chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585284 DO - https://doi.org/10.1016/j.intermet.2023.108074 VL - 163 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-58528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chahal, Shweta A1 - Xiao, Boyu A1 - Grant, Jessica A1 - Furniss, David A1 - Farries, Mark A1 - Phang, Sendy A1 - Neate, Nigel A1 - Robertson, Lorelei A1 - Roe, Martin A1 - Barney, Emma A1 - Seddon, Angela B. T1 - Ce3+-doped chalcogenide glass fibre for laser beyond 4 microns wavelength: Glass material-integrity N2 - The 4-μm wavelength barrier encountered for mid-infrared fibre lasing based on heavy metal fluoride glasses has been overcome. We reported, in 2021, the first continuous wave, mid-infrared fibre laser operating beyond 4 μm at room temperature in a fibre with a Ce3+-doped selenide-chalcogenide core. Defects, such as crystallites in the core glass, could cause unwanted light-scattering, diminishing fibre laser efficiency. It is important to identify such optical loss mechanisms and eradicate them. Here, we report on investigating the material nano-structure of a chalcogenide-glass lasing fibre which exhibits 7 mW laser power output; the fibre has a Ce3+-doped core (8.5 μm diameter), concentrically surrounded by an inner- and outer-cladding, where both cladding-glasses are nominally the same composition. High resolution transmission electron microscopy and electron diffraction show that the core, inner-cladding and outer-cladding of the lasing fibre are internally nano-crystallite-free and amorphous. However, the external outer surface of the last 10 m of fibre drawn, of the total 100 m, contains monoclinic GeSe2 crystallites adjacent to discrete, small (<0.5 mm) wrinkled defects. The final length of fibre is drawn from the final part of the glass fibreoptic preform. The glass preform has as its outermost component an extruded chalcogenide glass tube. It is the last part of the tube which spends the longest time at high temperature inside the extruder during tube manufacture, encouraging heterogeneous nucleation at the tube outer-surface in contact with the extruder. These heterogeneous nuclei subsequently nucleate crystal growth during fibre-drawing in the outermost fibre surface. KW - Optical glass KW - Photonics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653371 DO - https://doi.org/10.1016/j.optmat.2025.117219 SN - 0925-3467 VL - 166 SP - 1 EP - 14 PB - Elsevier CY - Amsterdam AN - OPUS4-65337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -