ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS

In this work, the possibility of electrochemical synthesis of tantalum silicides, in particular Ta2Si, using chloride-fluoride melts NaCl–KCl–K2TaF7–K2SiF6 as an electrolytic medium was investigated. The influence of key process parameters, such as temperature, melt composition and potential, on the...

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Datum:2025
Hauptverfasser: Kuleshov, Serhii, Devyatkin, Sergei, Yang, Peixia, Meng, Fan
Format: Artikel
Sprache:English
Veröffentlicht: V.I.Vernadsky Institute of General and Inorganic Chemistry 2025
Online Zugang:https://ucj.org.ua/index.php/journal/article/view/729
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Назва журналу:Ukrainian Chemistry Journal

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Ukrainian Chemistry Journal
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spelling oai:ojs2.1444248.nisspano.web.hosting-test.net:article-7292025-09-25T13:39:01Z ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS Kuleshov, Serhii Devyatkin, Sergei Yang, Peixia Meng, Fan tantalum silicides, electrochemical synthesis, halide molten salts. In this work, the possibility of electrochemical synthesis of tantalum silicides, in particular Ta2Si, using chloride-fluoride melts NaCl–KCl–K2TaF7–K2SiF6 as an electrolytic medium was investigated. The influence of key process parameters, such as temperature, melt composition and potential, on the phase composition and morphology of the final products was studied. Based on thermodynamic calculations that take into account the Gibbs energy of formation of the corresponding compounds, as well as a complex of voltammetric studies, including cyclic voltammetry, the mechanism of electrochemical reduction of tantalum and silicon ions to Ta2Si was established. This confirms the effectiveness of using chloride-fluoride melts for the direct synthesis of tantalum silicides. It was experimentally shown that the ratio of the volumetric concentrations of tantalum and silicon in the melt does not affect the stoichiometry of the cathodic reduction products. Regardless of the initial ratio, the main product of electrolysis is Ta2Si, which indicates the thermodynamic advantage of the formation of this particular phase under the studied conditions. Electrolysis on nickel cathodes produced Ta2Si powders and coatings that differ in morphology and particle size. The phase composition and morphology of the synthesized products were confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The effect of current density on the deposition rate and quality of the obtained materials was studied. In particular, in a NaCl–KCl melt containing 2 wt.% K2SiF6 and 5 wt.% K2TaF7, at a current density in the range of 0.1–0.2 A/cm² and a temperature of 700 °C, powders with a porous structure consisting of agglomerates of small dendritic particles were obtained. The optimal current density range of 0.03–0.08 A/cm² for the deposition of homogeneous and dense Ta2Si coatings with characteristic globular elements has been determined. The results obtained demonstrate the significant potential of electrochemical synthesis from chloride-fluoride melts for obtaining tantalum silicides with controlled phase composition and morphological characteristics, which opens up prospects for their application in various high-tech industries, including microelectronics, wear-resistant and corrosion-resistant coatings, and high-temperature materials. V.I.Vernadsky Institute of General and Inorganic Chemistry 2025-05-25 Article Article Physical chemistry Физическая xимия Фізична xімія application/pdf https://ucj.org.ua/index.php/journal/article/view/729 10.33609/2708-129X.91.4.2025.88-98 Ukrainian Chemistry Journal; Vol. 91 No. 4 (2025): Ukrainian Chemistry Journal; 88-98 Украинский химический журнал; Том 91 № 4 (2025): Ukrainian Chemistry Journal; 88-98 Український хімічний журнал; Том 91 № 4 (2025): Ukrainian Chemistry Journal; 88-98 2708-129X 2708-1281 en https://ucj.org.ua/index.php/journal/article/view/729/369
institution Ukrainian Chemistry Journal
baseUrl_str
datestamp_date 2025-09-25T13:39:01Z
collection OJS
language English
topic_facet tantalum silicides
electrochemical synthesis
halide molten salts.
format Article
author Kuleshov, Serhii
Devyatkin, Sergei
Yang, Peixia
Meng, Fan
spellingShingle Kuleshov, Serhii
Devyatkin, Sergei
Yang, Peixia
Meng, Fan
ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
author_facet Kuleshov, Serhii
Devyatkin, Sergei
Yang, Peixia
Meng, Fan
author_sort Kuleshov, Serhii
title ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
title_short ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
title_full ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
title_fullStr ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
title_full_unstemmed ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF Tа2Si OBTAINED FROM CHLORIDE-FLUORIDE MELTS
title_sort electrochemical synthesis and characterization of tа2si obtained from chloride-fluoride melts
description In this work, the possibility of electrochemical synthesis of tantalum silicides, in particular Ta2Si, using chloride-fluoride melts NaCl–KCl–K2TaF7–K2SiF6 as an electrolytic medium was investigated. The influence of key process parameters, such as temperature, melt composition and potential, on the phase composition and morphology of the final products was studied. Based on thermodynamic calculations that take into account the Gibbs energy of formation of the corresponding compounds, as well as a complex of voltammetric studies, including cyclic voltammetry, the mechanism of electrochemical reduction of tantalum and silicon ions to Ta2Si was established. This confirms the effectiveness of using chloride-fluoride melts for the direct synthesis of tantalum silicides. It was experimentally shown that the ratio of the volumetric concentrations of tantalum and silicon in the melt does not affect the stoichiometry of the cathodic reduction products. Regardless of the initial ratio, the main product of electrolysis is Ta2Si, which indicates the thermodynamic advantage of the formation of this particular phase under the studied conditions. Electrolysis on nickel cathodes produced Ta2Si powders and coatings that differ in morphology and particle size. The phase composition and morphology of the synthesized products were confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The effect of current density on the deposition rate and quality of the obtained materials was studied. In particular, in a NaCl–KCl melt containing 2 wt.% K2SiF6 and 5 wt.% K2TaF7, at a current density in the range of 0.1–0.2 A/cm² and a temperature of 700 °C, powders with a porous structure consisting of agglomerates of small dendritic particles were obtained. The optimal current density range of 0.03–0.08 A/cm² for the deposition of homogeneous and dense Ta2Si coatings with characteristic globular elements has been determined. The results obtained demonstrate the significant potential of electrochemical synthesis from chloride-fluoride melts for obtaining tantalum silicides with controlled phase composition and morphological characteristics, which opens up prospects for their application in various high-tech industries, including microelectronics, wear-resistant and corrosion-resistant coatings, and high-temperature materials.
publisher V.I.Vernadsky Institute of General and Inorganic Chemistry
publishDate 2025
url https://ucj.org.ua/index.php/journal/article/view/729
work_keys_str_mv AT kuleshovserhii electrochemicalsynthesisandcharacterizationofta2siobtainedfromchloridefluoridemelts
AT devyatkinsergei electrochemicalsynthesisandcharacterizationofta2siobtainedfromchloridefluoridemelts
AT yangpeixia electrochemicalsynthesisandcharacterizationofta2siobtainedfromchloridefluoridemelts
AT mengfan electrochemicalsynthesisandcharacterizationofta2siobtainedfromchloridefluoridemelts
first_indexed 2025-09-26T01:42:09Z
last_indexed 2025-09-26T01:42:09Z
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