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- ItemUV-VIS spectroscopic investigations of amber glass at high temperatures(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1999) Müller, Matthias; Rüssel, Christian; Claußen, OlafThe absorption spectra of iron-containing glasses and an amber glass were recorded in the temperature ränge of 25 to 700 °C. Α shift of the UV absorption edge towards lower wave numbers with increasing temperature was found. The amount of the shift depends on the Fe³⁺ concentration. Here, the UV absorption edge may superimpose or even cover up the absorption bands of colouring ions with increasing temperatures. For an amber glass sample, with increasing temperature, the intensity of the absorption bands of the amber chromophore decreases slightly. However, above 550 °C the decomposition of the chromophore is observed. All changes are reversible when temperature is decreased again. The decomposition of the chromophore and the attributed temperature ränge are in agreement with thermodynamic calculations.
- ItemRedox equilibria of polyvalent elements in binary Na2O · xSiO2 melts(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2000) Gönna, Gordon von der; Rüssel, ChristianGlass melts with the basic compositions (in mol%) of 15 Na2O ∙ 85 SiO2 and Na2O ∙ 2 SiO2 were doped with oxides of various polyvalent elements. At temperatures in the range of 800 to 1550°C, square-wave voltammograms were recorded, which exhibit distinct maxima attributed to respective reduction processes. The following redox steps were observed: Sb5+/Sb3+, Sb3+/Sb0, As5+/As3+, As3+/As0, Cu+/Cu0, V5+/V4+, V4+/V3+, Cr6+/Cr3+, Cr3+/Cr2+, Fe3+/Fe2+ and Ti4+/Ti3+. Peak potentials measured in the Na2O ∙ 2 SiO2 glass depended linearly on temperature, while those of the 15 Na2O ∙ 85 SiO2 melt were affected by the crystallization of cristobalit at temperatures < 1300°C. Redox equilibria in the alkali-rich Na2O ∙ 2 SiO2 melt were generally shifted to the oxidized state by comparison to those measured in the 15 Na2O ∙ 85 SiO2 melt.
- ItemInfluence of nucleating agents on the crystallization of Mg-Ca-Si-Al-O-N oxynitride glasses(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1998) Deckwerth, Martin; Rüssel, ChristianOxynitride glasses in the system M g - C a - S i - A l - O - N were prepared with the aid of a polymeric preceramic aluminum nitride precursor as nitrogen source and transformed into glass-ceramics at temperatures in the ränge of 950 to 1350°C To support the devitrification process, TiO₂ , Cr₂O₃, MgF₂ and ZrO₂ were added to the batches as potentially nucleating agents. Under the reducing meldng conditions applied. TiO₂ led to undesired reactions in the glass melt and was rejected as nucleadng agent. Cr₂O₃ could only be dissolved in the glasses to a maximum content of 1 wt% and did not lead to obvious effects concerning nucleation and crystal growth. The addition of fluorine results in the formation of a fine-grained microstructure but by analogy to Cr₂O₃, did not lead to phase Separation. Adding ZrO₂, provoked phase Separation in the oxynitride glasses, which was even promoted by the presence of nitrogen. These glass-ceramics possessed an extremely fine-grained microstructure containing nonstabilized tetragonal ZrO₂, which results in an additional nitrogen content independent improvement of the mechanical properties. By comparison to Ti02, Cr203 and MgF2, zirconia has a twofold effect: it is not only an efficient nucleating agent in the case of oxynitride glasses but also an efficient toughening agent for the resulting glass-ceramics.
- ItemGlass-ceramic with preferred orientation of Li2Si205 crystals produced by extrusion below crystallization temperature and subsequent heat treatment(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1994) Durschang, Bernward R.; Carl, Gunter; Rüssel, Christian; Marchetti, Kurt; Roeder, ErwinGlass-ceramics with oriented crystals have been produced from a lithium disilicate glass system by extruding the nucleated glass below the crystallization temperature, and subsequent heat treatment to achieve high-crystalline glass-ceramics. The extruded glass was found to possess a small amount of ahgned, elongated lithium disilicate crystallites and anisotropic stresses. The resulting glassceramic shows a high orientation of the needle-shaped Li₂Si₂O₅ crystals with their c-axis parallel to the extrusion direction. The degree of crystallographic orientation was found to be decreased for samples with an additional heat treatment slightly above Tg, placed between the extrusion process and the crystallization. The crystal alignment of specimens extruded below crystallization temperature is significantly higher than the alignment o f extruded glass-ceramic.
- ItemRheological properties of calcium metaphosphate melts during extrusion(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1999) Yue, Yuanzheng; Carl, Gunter; Rüssel, ChristianAn extrusion method to determine viscosities is described. Here, different stages of the response on the load applied are observed and the viscous heating efFect caused by the mechanical deformation work is taken into account. The method enables the determination of viscosities in the ränge of 10⁶ to 10^(8.5) dPa s. The values obtained are in good agreement with interpolated ones determined by beam bending and cylinder rotation. During extruding of calcium metaphosphate melts, the viscositiy decreases with increasing shear rate. This shear-thinning efFect (or non-Newtonian behaviour) is attributed to the orientation of flow units of the dynamic melt network. It is found that both Newtonian and non-Newtonian flow behaviour of calcium metaphosphate melts was largely influenced by adding a small amount of SiO₂. However, the introduction of a small amount of SiO₂ into calcium metaphosphate melts is beneficial to study the flow behaviour, since by that the crystallization of melts is avoided, which hinders the continuation of extruding processes.
- ItemHigh-temperature UV-VIS-NIR spectroscopy of chromium-doped glasses(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2001) Gödeke, Dieter; Müller, Matthias; Rüssel, ChristianChromium-doped glasses with the basic composition (in mol%) 16 Na2O · 10 CaO · 74 SiO2 were melted under different redox conditions. From these glasses, UV-VIS-NIR absorption spectra were recorded at temperatures up to 1200 °C. While the intensity of the peak attributed to Cr6+ decreases, some of the peaks caused by Cr3+ increase in intensity at higher temperature. All peaks are slightly shifted to larger wavelengths and get broader with increasing temperature. Glasses melted under oxidizing conditions were slowly cooled as well as quenched. Using EPR spectroscopy, in the quenched sample, Cr5+ was detected in a larger concentration than in the slowly cooled sample. Otherwise, the Cr6+ concentration was larger in the slowly cooled sample. This is explained by a redox reaction, i.e. a disproportionation of Cr5+ to Cr6+ and Cr3+ during cooling. As shown by high-temperature spectroscopy of the quenched sample, this redox reaction is frozen in below 550 °C.
- ItemHigh-temperature spectroscopic study of redox reactions in iron-and arsenic-doped melts(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2003) Schirmer, Henning; Müller, Matthias; Rüssel, ChristianGlasses with the basic composition 16Na2O - 10CaO - 74SiO2 doped with iron or with both iron and arsenic were studied by means of high-temperature UV-VIS-NIR spectroscopy. Increasing temperatures led to a shift of the UV absorption edge caused by Fe3+ -charge transfer bands to larger wavelengths. All other bands, especially the Fe2+ absorption band at around 1100 nm, decreased in intensity at higher temperatures. For glasses, solely doped with iron, the temperature dependency of the extinction coefficient was quantitatively determined. Glasses doped with both arsenic and iron showed a different behaviour: the intensity of the bands decreased up to a temperature of 600 to 650 °C and then increased again. This can be explained by the temperature-dependent redox reaction 2Fe3+ + As3+ ⇌ 2Fe2+ + As5+. Increasing temperatures lead to a shift of the reaction to the right. This reaction is in equilibrium at temperatures > 650 °C and gets frozen in at smaller temperatures, depending on the respective iron and arsenic concentrations. The latter is explained by a numerical simulation assuming the redox reactions to be controlled by diffusion.
- ItemKinetics of phase separation in a 6.5 Na2O ∙ 33.5 B2O3 ∙ 60 SiO2 glass(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2000) Flügel, Alexander; Rüssel, ChristianIndustrially melted glasses with the composition (in mol%) 6.5 Na2O ∙ 33.5 B2O3 ∙ 60 SiO2 were thermally treated at temperatures in the range of 660 to 750 °C. This resulted in phase separation, i.e. in the formation of a silica- and a sodium borate-rich phase with an interconnected microstructure. Both, the volume content of the borate-rich phase and the mean structure thickness (the correlation length) increased with time as well as with temperature. The volume content approached to a limiting value at constant temperature. The correlation length increased with time according to a power law (~ t^1/n). By contrast to previous studies, n was in the range of 1 to 1.2 within the temperature range and time scale studied. The correlation lengths were much larger (up to 12 µm) and the viscosities much lower than in most previous studies. The kinetic law was explained as controlled by visous flow.
- ItemHigh-temperature UV-VIS-NIR absorption and emission spectroscopy of soda-lime-silica glasses doped with Nd2O3(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2003) Gödeke, Dieter; Müller, Matthias; Rüssel, ChristianAbsorption spectra were recorded from a glass with the basic composition 16Na2O ∙ 10CaO ∙ 74SiO2 doped with 4 wt% Nd2O3 at temperatures in the range from 25 to 1400°C. The effective width of the observed absorption peaks increased with increasing temperature, while the peak positions remained nearly constant. Some absorption coefficients decreased with temperature while that at a wavelength of 657 nm increased notably. Emission spectra were recorded from glass melts exhibiting a temperature gradient at the surface (cold surface). The spectra showed distinguished minima at those wavelengths where the absorption maxima occurred. Numerical simulation of the emission spectra assuming a constant temperature gradient at the surface is in agreement with the experimental spectra.
- ItemCrystallization and vicosity of phosphate melts in the system Na2O-CaO-MgO-P2O5-Al2O3-TiO2(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2004) Wange, Peter; Vogel, Jürgen; Knoche, Silke; Rüssel, ChristianGlasses in the system Na2O-CaO-MgO-P2O5-Al2O3-TiO2 were studied with respeet to their crystallization and viscosity. Glasses in the metaphosphate range are composed of phosphate chains, and possess a comparably small tendeney to crystallization. Here, AlPO4 in a cristobalite-like modification and Ca2P2O7 are formed. Glasses in the intermediate range between metaphosphate and invert glass structures are composed of smaller phosphate units and show higher erystal growth velocities as well as higher viscosities. Additions of MgO, AI2O3 and TiO2 result in a strengthening of the glass network, and hence, inereasing viscosities and a notably smaller tendeney to crystallization.