Thermolysis of Hydrated Antimony Pentoxide

Kovalenko, Liliya Yu.; Yaroshenko, F. A.; Burmistrov, V. A.; Isaeva, T. N.; Галимов, Д. М.

doi:10.1134/s0020168519060086

Cited by 11 publications

(9 citation statements)

References 27 publications

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“…As can be seen from the comparison of STA and TG data, the mass losses of pure PAA in the region of 20-350 • C can be attributed to water losses. This assumption is in accordance with data in the literature on PAA thermolysis [39]. Based on mass losses of up to 350 • C, the composition of PAA after synthesis was calculated to be Sb 2 O 5 •2.92H 2 O.…”

Section: Effect Of the Binder Concentration On The Thermal Evolution ...supporting

confidence: 89%

“…Roughly three water molecules are attributed per each Sb 2 O 5 in the PAA structure. Based on experimental STA data and data from [39], the decomposition of hydrated antimony oxide takes place accordingly to a two-step schematic reaction sequence, described by Equations ( 4) and ( 5):…”

Section: Effect Of the Binder Concentration On The Thermal Evolution ...mentioning

confidence: 99%

“…The differences observed may be due to changes in polymer density during compaction upon the membrane compaction. Literature data on fluoroplastic powder density varied significantly, from 1.6-2.2 g/cm 3 [39][40][41]; the fluoroplastic could also contain some co-polymer, such as polystyrole or polyethylene, in the different ratios. Therefore, it can be stated that within the determined experimental relative density error, the chosen compaction conditions are suitable for obtaining fully dense membranes.…”

Section: Effect Of the Binder Concentration On The Thermal Evolution ...mentioning

confidence: 99%

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Electrochemical Characterization of Novel Polyantimonic-Acid-Based Proton Conductors for Low- and Intermediate-Temperature Fuel Cells

et al. 2021

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The development of novel proton-conducting membrane materials for electrochemical power units, i.e., low temperature fuel cells (FCs), efficiently working up to 300 °C, is a critical problem related to the rapid shift to hydrogen energy. Polyantimonic acid (PAA) is characterized by high conductivity, sufficient thermal stability and can be regarded as a prospective proton-conducting material. However, the fabrication of bulk PAA-based membranes with high proton conductivity remains a challenging task. In the present work, for the first time, the authors report the investigation on proton conductivity of bulk PAA-based membranes in the temperature range 25–250 °C, both in dry air and in moisturized air. Using PAA powder and fluoroplastic as a binder, fully dense cylindrical membranes were formed by cold uniaxial pressing. The structures of the PAA-based membranes were investigated by SEM, EDX, XRD and Raman techniques. STA coupled with in situ thermo-XRD analysis revealed that the obtained membranes corresponded with Sb2O5·3H2O with pyrochlore structure, and that no phase transitions took place up to 330 °C. PAA-based membranes possess a high-grain component of conductivity, 5 × 10−2 S/cm. Grain boundary conductivities of 90PAA and 80PAA membranes increase with relative humidity content and their values change non-linearly in the range 25–250 °C.

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Section: Effect Of the Binder Concentration On The Thermal Evolution ...supporting

confidence: 89%

Section: Effect Of the Binder Concentration On The Thermal Evolution ...mentioning

confidence: 99%

Section: Effect Of the Binder Concentration On The Thermal Evolution ...mentioning

confidence: 99%

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Electrochemical Characterization of Novel Polyantimonic-Acid-Based Proton Conductors for Low- and Intermediate-Temperature Fuel Cells

et al. 2021

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“…For instance, Yu et al [23,24] obtained super soluble amorphous antimonic acid via controlled hydrolysis of SbCl 3 that was previously oxidized to SbCl 5 ; then, using 30% of hydrogen peroxide, they performed an efficient removal of Bi(III) from the solution. Hydrated antimony pentoxide was obtained also by the research group of Klestchov et al [25,26], using the same hydrolysis technique approach. The obtained precipitate was aged at 27 and then at 62 °C; after ageing, its thermolysis process was scrutinized in detail.…”

Section: Introductionmentioning

confidence: 99%

Polyantimonic acid-based materials evaluated as moisture sensors at ambient temperature

Mendes

Kurapova

Faia

et al. 2022

J Solid State Electrochem

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Humidity sensors are in high demand for many applications, such as environmental monitoring and air and food quality control. Despite many inorganic and organic materials exhibit moisture sensing properties, the electrical response of many existing sensors is not stable along the time. Polyantimonic acid (PAA) is characterized by elevated proton conductivity and by high thermal stability: consequently, it is seen as promising proton conductor for usage in humidity sensing devices. In this work, for the first time, PAA-based bulk solid membranes were produced and tested as potential materials for relative humidity (RH) detection and their moisture sensitivity was evaluated. Two different amounts of binder were used for moulding the solid sensors: the ones with 10% of binder were designated as 90PAA, while the ones with 20% were named 80PAA. The structures of the solid samples were investigated by X-ray diffraction (XRD) technique, adsorption–desorption curves via Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) techniques. The electrical behaviour was examined at ambient temperature by electrical impedance spectroscopy in the entire relative humidity (RH) interval (0–100%) and in the frequency range of 40 Hz up to 60 MHz. Electrical response of the materials was correlated with the structural features of the membranes. Both 90PAA and 80PAA sensors showed total resistance 3 × 105 and 3.5 × 105 Ω at 10% RH, respectively. A linear decrease of the resistance on RH was observed in the range 30–90% RH for both sensors. The electrical response of the evaluated PAA-based sensors displays good repeatability and reproducibility: the ones with lower binder content showed higher moisture sensitivity as well as very good time stability over 1 year.

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“…These structures were inferred from the total weight loss of the AA sample, and later confirmed by carefully matching up these curves with the TGA and DTA curves of the Kovalenko et al . thermolysis analysis reported for a hydrated antimony pentoxide sample 38 . ( c , d ) low magnification SEM images of the AA sample obtained by soft-chemistry oxidative hydrolysis reaction.…”

Section: Resultsmentioning

confidence: 99%

Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid

Mayer

Rodrigues

Sobrados

et al. 2021

Sci Rep

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The elusive crystal structure of the so-called ‘antimonic acid’ has been investigated by means of robust and state-of-the-art techniques. The synergic results of solid-state magic-angle spinning nuclear magnetic resonance spectroscopy and a combined Rietveld refinement from synchrotron X-ray and neutron powder diffraction data reveal that this compound contains two types of protons, in a pyrochlore-type structure of stoichiometric formula (H3O)1.20(7)H0.77(9)Sb2O6. Some protons belong to heavily delocalized H3O+ subunits, while some H+ are directly bonded to the oxygen atoms of the covalent framework of the pyrochlore structure, with O–H distances close to 1 Å. A proton diffusion mechanism is proposed relying on percolation pathways determined by bond-valence energy landscape analysis. X-ray absorption spectroscopy results corroborate the structural data around Sb5+ ions at short-range order. Thermogravimetric analysis and differential scanning calorimetry endorsed the conclusions on the water content within antimonic acid. Additional 0.7 water molecules per formula were assessed as moisture water by thermal analysis.

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Thermolysis of Hydrated Antimony Pentoxide

Cited by 11 publications

References 27 publications

Electrochemical Characterization of Novel Polyantimonic-Acid-Based Proton Conductors for Low- and Intermediate-Temperature Fuel Cells

Electrochemical Characterization of Novel Polyantimonic-Acid-Based Proton Conductors for Low- and Intermediate-Temperature Fuel Cells

Polyantimonic acid-based materials evaluated as moisture sensors at ambient temperature

Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid

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