High Temperature Study of Oxide Systems: Thermal Analysis and Knudsen Effusion Mass Spectrometry

Stolyarova, V. L.; Vorozhtcov, Viktor A.

doi:10.1134/s0036024420130257

Cited by 6 publications

(3 citation statements)

References 41 publications

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“…Semenov, 5 a number of reviews dealing with the vaporization and thermodynamic properties of oxide systems studied using KEMS at high temperatures have been completed. [185][186][187][188][189][190][191][192][193][194][195][196][197][198][199][200][201][202] The general overview in this area was presented in the series of publications from decade to decade. [185][186][187][188][189][190] We can delineate them into three main groups: glassforming oxide systems, [191][192][193][194][195][196] ultrahigh-refractory oxide systems mainly based on 2, [197][198][199] modeling approaches developed using the Knudsen effusion mass spectrometric thermodynamic data on oxide systems for the prediction of their high-temperature behavior, 189,[193][194][195][196]200,201 and comparison to thermodynamic data that may be obtained at high temperatures using KEMS and differential thermal analysis.…”

Section: Following the Publication Of The Monograph By Stolyarova Andmentioning

confidence: 99%

“…Following the publication of the monograph by Stolyarova and Semenov, 5 a number of reviews dealing with the vaporization and thermodynamic properties of oxide systems studied using KEMS at high temperatures have been completed 185–202 . The general overview in this area was presented in the series of publications from decade to decade 185–190 .…”

Section: Measurements Of Partial Pressures and Thermodynamic Properti...mentioning

confidence: 99%

“…[185][186][187][188][189][190] We can delineate them into three main groups: glassforming oxide systems, [191][192][193][194][195][196] ultrahigh-refractory oxide systems mainly based on 2, [197][198][199] modeling approaches developed using the Knudsen effusion mass spectrometric thermodynamic data on oxide systems for the prediction of their high-temperature behavior, 189,[193][194][195][196]200,201 and comparison to thermodynamic data that may be obtained at high temperatures using KEMS and differential thermal analysis. 202 During the period indicated from 1994, systematic studies on the thermodynamic properties of the gaseous oxide salts or associates were successfully continued as the development of a scientific school founded by G. A. Semenov.…”

Section: Following the Publication Of The Monograph By Stolyarova Andmentioning

confidence: 99%

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Knudsen effusion mass spectrometry: Current and future approaches

Jacobson,

Colle,

Stolyarova

et al. 2024

Rapid Comm Mass Spectrometry

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RationaleKnudsen effusion mass spectrometry (KEMS) has been a powerful tool in physical chemistry since 1954. There are many excellent reviews of the basic principles of KEMS in the literature. In this review, we focus on the current status and potential growth areas for this instrumental technique.MethodsWe discuss (1) instrumentation, (2) measurement techniques, and (3) selected novel applications of the technique. Improved heating methods and temperature measurement allow for better control of the Knudsen cell effusive source. Accurate computer models of the effusive beam and its introduction to the ionizer allow optimization of such parameters as sensitivity and removal of background signals. Computer models of the ionizer allow for optimized sensitivity and resolution. Additionally, data acquisition systems specifically tailored to a KEMS system permit improved quantity and quality of data.ResultsKEMS is traditionally utilized for thermodynamic measurements of pure compounds and solutions. These measurements can now be strengthened using first principles and model‐based computational thermochemistry. First principles can be used to calculate accurate Gibbs energy functions (gefs) for improving third law calculations. Calculated enthalpies of formation and dissociation energies from ab initio methods can be compared to those measured using KEMS. For model‐based thermochemistry, solution parameters can be derived from measured thermochemical data on metallic and nonmetallic solutions. Beyond thermodynamic measurements, KEMS has been used for many specific applications. We select examples for discussion: measurements of phase changes, measurement/control of low‐oxygen potential systems, thermochemistry of ultrahigh‐temperature ceramics, geological applications, nuclear applications, applications to organic and organometallic compounds, and thermochemistry of functional room temperature materials, such as lithium ion batteries.ConclusionsWe present an overview of the current status of KEMS and discuss ideas for improving KEMS instrumentation and measurements. We discuss selected KEMS studies to illustrate future directions of KEMS.

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Section: Following the Publication Of The Monograph By Stolyarova Andmentioning

confidence: 99%

Section: Measurements Of Partial Pressures and Thermodynamic Properti...mentioning

confidence: 99%

Section: Following the Publication Of The Monograph By Stolyarova Andmentioning

confidence: 99%

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Knudsen effusion mass spectrometry: Current and future approaches

Jacobson,

Colle,

Stolyarova

et al. 2024

Rapid Comm Mass Spectrometry

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Mass spectrometric study of ceramics in the Sm₂O₃‐ZrO₂‐HfO₂ system at high temperatures

Stolyarova

Vorozhtcov

Лопатин

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale Systems containing zirconia, hafnia, and rare earth oxides are indispensable in various areas of high‐temperature technologies as a basis of ultra‐high refractory ceramics. Exposure of these materials to high temperatures may result in unexpected selective vaporization of components or phase transitions in the condensed phase leading to changes in physicochemical properties. Consequently, reliable application of the ceramics based on systems such as Sm2O3‐ZrO2‐HfO2 is impossible without data on its vaporization processes and thermodynamic properties, which may be used to predict the physicochemical characteristics of the ultra‐high refractory ceramics. Methods Ceramics based on the Sm2O3‐ZrO2‐HfO2 system were obtained by solid‐state synthesis and characterized by X‐ray fluorescence and X‐ray phase analyses. The vaporization and thermodynamics of the system considered were examined by the high‐temperature mass spectrometric method using a MS‐1301 magnetic sector mass spectrometer with a tungsten twin effusion cell. Vapor species effusing from the cell were ionized by electrons with an energy of 25 eV. Results The main vapor species over the Sm2O3‐ZrO2‐HfO2 system were shown to be SmO, Sm, and O at a temperature of 2373 K, indicating selective vaporization of Sm2O3 from the samples. The partial pressures of these vapor species and the Sm2O3 activities were determined in the Sm2O3‐ZrO2‐HfO2 system and allowed the excess Gibbs energies to be evaluated. These excess Gibbs energy values were compared with the results obtained by the semi‐empirical and statistical thermodynamic approaches. Conclusions The data obtained in this study showed negative deviations from the ideal behavior in the Sm2O3‐ZrO2‐HfO2 system at 2373 K. The results calculated according to the semi‐empirical methods and statistical thermodynamic Generalized Lattice Theory of Associated Solutions were in agreement with each other. Thus, this evidenced the desirability of further experimental investigation of the Sm2O3‐ZrO2‐HfO2 system by the high‐temperature mass spectrometric method.

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Unraveling solidification pathways of pure elements by ultra-slow temperature vs. time profile measurements

V．B．,

Srivastav,

Wang

et al. 2024

Thermochimica Acta

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High Temperature Study of Oxide Systems: Thermal Analysis and Knudsen Effusion Mass Spectrometry

Cited by 6 publications

References 41 publications

Knudsen effusion mass spectrometry: Current and future approaches

Knudsen effusion mass spectrometry: Current and future approaches

Mass spectrometric study of ceramics in the Sm₂O₃‐ZrO₂‐HfO₂ system at high temperatures

Unraveling solidification pathways of pure elements by ultra-slow temperature vs. time profile measurements

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High Temperature Study of Oxide Systems: Thermal Analysis and Knudsen Effusion Mass Spectrometry

Cited by 6 publications

References 41 publications

Knudsen effusion mass spectrometry: Current and future approaches

Knudsen effusion mass spectrometry: Current and future approaches

Mass spectrometric study of ceramics in the Sm2O3‐ZrO2‐HfO2 system at high temperatures

Unraveling solidification pathways of pure elements by ultra-slow temperature vs. time profile measurements

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Mass spectrometric study of ceramics in the Sm₂O₃‐ZrO₂‐HfO₂ system at high temperatures