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Crystallization of glasses in the system SiO2-Li2O-TiO2-Al2O3, investigated in situ at high temperature by XRD and DTA methods

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Abstract

The processes of crystallization of fibres (diameter 10–15μm) and coarse powders (grain size 500–1000μm) with four compositions in the system SiO2-Li2O-TiO2-Al2O3 were studied by conventional and in situ high-temperature XRD, DTA, SEM and optical microscopy. Activation energies of crystallization and morphological indices were deduced from the kinetic curves obtained by recording the high-temperature XRD peak intensity as a function of time. The glass-ceramic fibres drawn from compositions which exhibit glass-inglass phase separation show prevailing not-oriented bulk crystallization, whereas prevailing surface crystallization was found for single-phase glass fibres. Homogeneously-dispersed crystallization was obtained on heating fibres of these compositions. The partially cocrystallized glass fibres of eutectic composition between Li-metasilicate andβ-spodumene gave rise to a very fine and homogeneously-dispersed sub-microstructure.

Zusammenfassung

Die Prozesse der Kristallisation von Fasern (Durchmesser 10–15μm) und groben Pulvern (Korngröße 500–1000μm) von SiO2-LiO2-TiO2-Al2O3 in vier verschiedenen Zusammensetzungen wurden mittels herkömmlicher und in situ XRD, DTA, SEM und optischer Mikroskopie untersucht. Aktivierungsenergien der Kristallisation und morphologische Indices wurden aus den durch Registrierung der Intensität der Hochtemperatur-XRT-Peaks in Abhängigkeit von der Zeit erhaltenen kinetischen Kurven ermittelt. Die aus Gemischen einer die Glas-in-Glas-Phasentrennung bedingenden Zusammensetzung gezogenen Glas-Keramik-Fasern zeigen vorwiegend eine nicht-orientierte Bulk-Kristallisation, während vorherrschend Oberflächenkristallisation bei Einphasen-Glasfasern festgestellt wurde. Eine homogen verteilte Kristallisation wurde beim Erhitzen der Fasern dieser Zusammensetzungen erhalten. Bei partiell ko-kristallisierten Glasfasern einer eutektischen Mischung von Li-Metasilikat und (β-Spodumen liegt eine sehr feine und homogen-disperse Submikrostruktur vor.

Резюме

Процессы кристаллиз ации волокон (диаметр 10–15 мкм) и крупнозернистых порошков (размер зере н 500–1000 мкм) четырех соста вов в системе SiO2-Li2O-ТiO2AL2O3 были изучены при обыч ной и высокой темпера турах методами диффракции рентгеновских лучей, ДТА, электронно й и оптической микрос копии. Энергии активации пр оцесса кристаллизации и мор фологические индекс ы были определены из кинети ческих кривых, полученных из мерением высокотемп ературных рентгено-дифракцион ных пиков интенсивности в зави симости от времени. Стеклокерамические волокна, вытянутые из составов с фазовым ра зделением типе стекл о-в-стекле, показали преимущест венно неориентирова нную кристаллизацию во вс ем объëме, тогда как дл я однофазных стеклово локон-превалирующей была кристаллизация на поверхности. При на гревании стекловолокон такого состава проис ходила их гомогенно-диспергиз ованная кристаллиза ция.В случае стекловолоко н эвтектического сос тава метасиликат лития — β-сподумен частично происходила их совме стная кристаллизаци я с образованием очень м елкой и гомогенно-дис пергированной гомогенно-диспергир ованной субструктуры.

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Authors and Affiliations

  1. Dipartimento di Spettroscopia, Elettrochimica E Chimica Fisica, Università di Venezia, Calle Larga S. Marta D. D. 2137, 30123, Venezia

    A. Benedetti, G. Fagherazzi, S. Meriani & G. Sorarù

  2. Istituto di Chimica Applicata dell'Università di Trieste, Via Valerio 2, 34127, Trieste

    S. Meriani

  3. Istituto di Chimica Industriale dell'Università di Padova, Via Marzolo 9, 35200, Padova, Italy

    G. Sorarù

Authors
  1. A. Benedetti
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  2. G. Fagherazzi
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  3. S. Meriani
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  4. G. Sorarù
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Additional information

This work was supported by the Italian C. N. R., “Progetto Finalizzato Chimica Fine e Secondaria — Sottoprogetto Metodologie”.

We are indebted to Dr. B. Locardi of Stazione Sperimentale del Vetro, Murano (Venice) for furnishing the initial glasses and fibres.

We are also indebted to the “G. Giacomello” Institute (C. N. R., Rome) for furnishing the computer programme for the unit cell parameter refinement. Assistance by M. Pistolato and F. Venuda in the experimental work is gratefully acknowledged.

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Benedetti, A., Fagherazzi, G., Meriani, S. et al. Crystallization of glasses in the system SiO2-Li2O-TiO2-Al2O3, investigated in situ at high temperature by XRD and DTA methods. Journal of Thermal Analysis 29, 733–743 (1984). https://doi.org/10.1007/BF01913532

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