Abstract
Thermogravimetry (TG) and differential scanning calorimetry (DSC) have been used to examine the thermal behaviour, in N2 and in air, of the Si/Sb2O3, Si/KNO3, Si/Fe2O3 and Si/SnO2 pyrotechnic systems, in relation to the behaviour of the individual constituents.
TG curves for Si powder, heated alone in air, showed that limited oxidation of Si occurred above 700°. In N2, Sb2O3 sublimed completely between 500 and 900° and, in air, sublimation was accompanied by oxidation to Sb2O4. The Sb2O4 decomposed at higher temperatures. DSC curves for KNO3 heated in N2 showed the usual crystalline transition and melting endotherms followed by endothermic decomposition between 400 and 950°. DSC and TG curves of SnO2and Fe2O3 revealed no thermal events when samples were heated to 1000° in either N2 or air.
For the Si/Sb2O3 system, the oxidation of Si by Sb2O3 between 590 and 700°, was complicated by sublimation of Sb2O3 in N2 and also by the oxidation of Sb2O3 in air. No thermal events were observed for the Si/SnO2and Si/Fe2O3 systems when heated under a variety of conditions in either N2 or in air, although these systems do sustain combustion on suitable ignition. In the Si/KNO3 system, oxidation of Si occurs in a KNO3 melt at temperatures above 560° in nitrogen and in air.
Zusammenfassung
Mittels TG und DSC wurde das thermische Verhalten der pyrotechnischen Systeme Si/Sb2O3, Si/KNO3, Si/Fe2O3 und Si/SnO2in N2 und in Luft im Vergleich zum Verhalten der einzelnen Komponenten untersucht.
TG-Aufnahmen über das Erhitzen von Si-Pulver in Luft zeigten eine begrenzte Oxidation von Silizium oberhalb 700°C. Sb2O3 sublimiert in Stickstoff vollständig zwischen 500 und 900°C, in Luft wird die Sublimation durch Oxidation zu Sb2O4 begleitet. Sb2O4 zersetzt sich bei höheren Temperaturen. DSC-Aufnahmen für KNO3 in N2 zeigen die gewohnten Umwandlungs- und Schmelzendothermen, gefolgt von einer endothermen Zersetzung zwischen 400 und 950°C. Die DSC- und TG-Kurven für SnO2und Fe2O3 zeigen bei Erhitzen bis 1000°C weder in N2 noch in Luft den Verlauf thermische Prozesse an.
Bei dem System Si/Sb2O3 spielt sich neben der Oxidation von Si durch Sb2O3 zwischen 590 und 700°C auch eine Sublimation von Sb2O3 in N2 sowie eine Oxidation von Sb2O3 in Luft ab. Für die Systeme Si/SnO2und Si/Fe2O3 konnten durch Erhitzen unter einer Reihe von Bedingungen weder in Luft noch in N2 Thermoprozesse nachgewiesen werden, obwohl diese Systeme nach geeigneter Zündung den Brennvorgang aufrechterhalten. Im System Si/KNO3 erfolgt sowohl in N2 als auch in Luft oberhalb 560°C die Oxidation von Si in der KNO3-Schmelze.
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Dedicated to Professor Dr. H. J. Seifert on the occasion of his 60th birthday
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Rugunanan, R.A., Brown, M.E. Reactions of powdered silicon with some pyrotechnic oxidants. Journal of Thermal Analysis 37, 1193–1211 (1991). https://doi.org/10.1007/BF01913854
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DOI: https://doi.org/10.1007/BF01913854