High Temperature Study of Oxide Systems: Thermal Analysis and Knudsen Effusion Mass Spectrometry
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VI INTERNATIONAL CONFERENCE ON THERMAL ANALYSIS AND CALORIMETRY IN RUSSIA
High Temperature Study of Oxide Systems: Thermal Analysis and Knudsen Effusion Mass Spectrometry V. L. Stolyarovaa,b,* and V. A. Vorozhtcova,b a Saint
b Grebenshchikov
Petersburg State University, St. Petersburg, 199034 Russia Institute of Silicate Chemistry, Russian Academy of Sciences, St. Petersburg, 199034 Russia * e-mail: [email protected] Received April 15, 2020; revised April 22, 2020; accepted April 24, 2020
Abstract—Advantages and comparison of thermal analysis (TA) and Knudsen effusion mass spectrometry (KEMS) were discussed for the investigation of high temperature behavior of oxide systems such as ceramics and glass-forming melts. This brief overview proposes filling the gap by considering various approaches of interaction between the TA and KEMS data. The reliability of experimental data found using both methods is critically analyzed for thermodynamic values of the lanthanoid hafnates obtained by DSC and KEMS and mass losses of the samples in the Bi2O3–P2O5–SiO2 system found by thermogravimetry and KEMS. Recent achievements in experimental installations for these methods were also noted. Keywords: thermal analysis, DSC, Knudsen effusion mass spectrometry, thermodynamics, oxide ceramics, glass-forming melts DOI: 10.1134/S0036024420130257
INTRODUCTION Nowadays, the knowledge of the reliable information on thermodynamic properties and vaporization processes of oxide systems at high temperatures is urgently required for development of advanced approaches for preparation of new materials with the special properties and for modern technologies dealing with space, nuclear, metallurgical, electronics, and some others important applications. Thermal analysis (TA) and Knudsen effusion mass spectrometry (KEMS) are the most contemporary methods used for these purposes. TA has gradually increased the area of its application: from a simple method for evaluation of the phase transition temperatures of clay minerals as was demonstrated by Le Chatelier [1, 2] to a complex range of techniques for determination of various thermodynamic properties [3–5]. At present, capacities of thermal analysis continue evolving, particularly, towards increase in experimental temperatures of measurements of thermodynamic characteristics [6] and towards expansion of the range of the studied substances and materials [5] including hydrides [7], complex oxides [8], amorphous metal alloys [9], coordination complexes [10], polymers [11], and biomaterials [6], as well as ionic liquids [12]. A comprehensive review on various methods used to obtain thermodynamic properties of ceramics at temperatures above 1773 K was presented by Ushakov and Navrotsky [13]. While a wide spectrum of experimental methods was
considered including a range of calorimetric approaches and high temperature mass spectrometry [13], less attention was paid to potential combination of these techniques with the aim to increase their capacities or check mutual consistency of the data obtained. I
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