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Hydrothermal treatment of Zr, Ti, Sn and Ge hydrogenphosphates

Characterization of the derived compounds by thermal methods

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Abstract

The Zr, Ti, Sn and Ge hydrogenphosphates, generally prepared in a crystalline form by the refluxing method, have been submitted to hydrothermal treatment at 180° and 300°C in order to observe if the preparation time can be shortened maintaining their chemical composition and their α-structure. Simultaneous TG and DTA together with XRD revealed to be very suitable techniques for the characterization of the obtained products.

Zr phosphate is the most stable and gives in all conditions the α-monohydrated hydrogenphosphate phase. Similar behaviour for the Ti phosphate at 180°C, while at 300°C the compound transforms into γ-Ti(HPO4)2·2H2O. Sn phosphate, even on maintaining its α-structure, gives rise to more and more dehydrated phases on the increasing of the temperature of the HT and the concentration of the used phosphoric acid.

Ge hydrogenphosphate resulted the least stable under hydrothermal conditions, since even at 180°C it gives rise to GeOHPO4. Because of the easy hydrolyzability of Ge, the hydrothermal method is not a way to prepare the crystalline α-germanium hydrogenphosphate.

Zusammenfassung

Die Hydrogenphosphate von Zr, Ti, Sn und Ge wurden mittels der Refluxmethode in kristalliner Form hergestellt und bei 180° und 300°C einer hydrothermischen Behandlung unterzogen, um festzustellen, ob die Herstellungszeit bei gleichbleibender chemischer Zusammensetzung und ihrer α-Struktur verkürzt werden kann. Simultane TG und DTA zusammen mit Röntgendiffraction scheinen eine sehr gute Technik darzustellen, um die erhaltenen Produkte zu charakterisieren.

Zr-Phosphate ist am stabilsten und ergibt unter allen Bedingungen eine α-monohydrierte Hydrogenphosphate-Phase. Ein ähnliches Verhalten zeigt das Titanphosphat bei 180°C, während die Verbindung sich bei 300°C in γ-Ti(HPO4)2·2H2O umwandelt. Sn-Phosphat gibt — gerade um seine α-Sruktur zu behalten — durch die steigende Temperatur und steigende Konzentration an Phosphorsäure Anlaß für mehr und mehr dehydratierte Phasen.

Ge-Hydrogenphosphat erwies sich unter hydrothermischen Bedingungen als am instabilsten bereids bei 180°C liefert as GeOHPO4. Wegen der leichten Hydrolisierbarkeit von Ge ist die hydrothermische Methode kein Weg, um kristallines α-Germaniumhydrogenphosphat herzustellen.

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Authors and Affiliations

  1. Area Ricerca Roma, IMAI-CNR, C. P. 10 Monterotondo Scalo, Roma

    P. Patrono & C. Ferragina

  2. Dipart. Chimica, Universita La Sapienza, Roma, Italy

    A. La Ginestra, M. A. Massucci, A. Frezza & S. Vecchio

Authors
  1. P. Patrono
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  2. A. La Ginestra
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  3. C. Ferragina
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  4. M. A. Massucci
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  5. A. Frezza
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  6. S. Vecchio
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Additional information

Thanks are due to C. N. R. — Progetto Finalizzato ‘Materiali Speciali per Tecnologie Avanzate’ for the financial support.

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Patrono, P., La Ginestra, A., Ferragina, C. et al. Hydrothermal treatment of Zr, Ti, Sn and Ge hydrogenphosphates. Journal of Thermal Analysis 38, 2603–2612 (1992). https://doi.org/10.1007/BF01979736

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  • DOI: https://doi.org/10.1007/BF01979736

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