Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors

In this study, the potential to modify the phase structure and morphology of manganese dioxide synthesized via the hydrothermal route was explored. A series of samples were prepared at different synthesis temperatures (100, 120, 140, and 160 °C) using KMnO<sub>4</sub> and MnSO<sub>...

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Main Authors: Vania Ilcheva, Victor Boev, Mariela Dimitrova, Borislava Mladenova, Daniela Karashanova, Elefteria Lefterova, Natalia Rey-Raap, Ana Arenillas, Antonia Stoyanova
Format: Article
Language:English
Published: MDPI AG 2025-01-01
Series:Gels
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Online Access:https://www.mdpi.com/2310-2861/11/1/68
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author Vania Ilcheva
Victor Boev
Mariela Dimitrova
Borislava Mladenova
Daniela Karashanova
Elefteria Lefterova
Natalia Rey-Raap
Ana Arenillas
Antonia Stoyanova
author_facet Vania Ilcheva
Victor Boev
Mariela Dimitrova
Borislava Mladenova
Daniela Karashanova
Elefteria Lefterova
Natalia Rey-Raap
Ana Arenillas
Antonia Stoyanova
author_sort Vania Ilcheva
collection DOAJ
description In this study, the potential to modify the phase structure and morphology of manganese dioxide synthesized via the hydrothermal route was explored. A series of samples were prepared at different synthesis temperatures (100, 120, 140, and 160 °C) using KMnO<sub>4</sub> and MnSO<sub>4</sub>·H<sub>2</sub>O as precursors. The phase composition and morphology of the materials were analyzed using various physicochemical methods. The results showed that, at the lowest synthesis temperature (100 °C), an intercalation compound with composition K<sub>1.39</sub>Mn<sub>3</sub>O<sub>6</sub> and a very small amount of α-MnO<sub>2</sub> was formed. At higher temperatures (120–160 °C), the amount of α-MnO<sub>2</sub> increased, indicating the formation of two clearly distinguished crystal structures. The sample obtained at 160 °C exhibited the highest specific surface area (approximately 157 m<sup>2</sup>/g). These two-phase (α-MnO<sub>2</sub>/K<sub>1.39</sub>Mn<sub>3</sub>O<sub>6</sub>) materials, synthesized at the lowest and highest temperatures, respectively, and containing an appropriate amount of carbon xerogel, were tested as active mass for positive electrodes in a solid-state supercapacitor, using a Na<sub>+</sub>-form Aquivion<sup>®</sup> membrane as the polymer electrolyte. The electrochemical evaluation showed that the composite with the higher specific surface area, containing 75% manganese dioxide, demonstrated improved characteristics, including 96% capacitance retention after 5000 charge/discharge cycles and high energy efficiency (approximately 99%). These properties highlight its potential for application in solid-state supercapacitors.
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spelling doaj-art-b928686135fa4a47ae6e1f31fdff01e02025-01-24T13:34:00ZengMDPI AGGels2310-28612025-01-011116810.3390/gels11010068Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State SupercapacitorsVania Ilcheva0Victor Boev1Mariela Dimitrova2Borislava Mladenova3Daniela Karashanova4Elefteria Lefterova5Natalia Rey-Raap6Ana Arenillas7Antonia Stoyanova8Institute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaInstitute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaInstitute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaInstitute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaInstitute of Optical Materials and Technologies, Bulgarian Academy of Sciences, Acad. G. Bonchev Str. bl.109, 1113 Sofia, BulgariaInstitute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaInstituto de Ciencia y Tecnología del Carbono, INCAR-CSIC, Francisco Pintado Fe 26, 33011 Oviedo, SpainInstituto de Ciencia y Tecnología del Carbono, INCAR-CSIC, Francisco Pintado Fe 26, 33011 Oviedo, SpainInstitute of Electrochemistry and Energy Systems, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 10, 1113 Sofia, BulgariaIn this study, the potential to modify the phase structure and morphology of manganese dioxide synthesized via the hydrothermal route was explored. A series of samples were prepared at different synthesis temperatures (100, 120, 140, and 160 °C) using KMnO<sub>4</sub> and MnSO<sub>4</sub>·H<sub>2</sub>O as precursors. The phase composition and morphology of the materials were analyzed using various physicochemical methods. The results showed that, at the lowest synthesis temperature (100 °C), an intercalation compound with composition K<sub>1.39</sub>Mn<sub>3</sub>O<sub>6</sub> and a very small amount of α-MnO<sub>2</sub> was formed. At higher temperatures (120–160 °C), the amount of α-MnO<sub>2</sub> increased, indicating the formation of two clearly distinguished crystal structures. The sample obtained at 160 °C exhibited the highest specific surface area (approximately 157 m<sup>2</sup>/g). These two-phase (α-MnO<sub>2</sub>/K<sub>1.39</sub>Mn<sub>3</sub>O<sub>6</sub>) materials, synthesized at the lowest and highest temperatures, respectively, and containing an appropriate amount of carbon xerogel, were tested as active mass for positive electrodes in a solid-state supercapacitor, using a Na<sub>+</sub>-form Aquivion<sup>®</sup> membrane as the polymer electrolyte. The electrochemical evaluation showed that the composite with the higher specific surface area, containing 75% manganese dioxide, demonstrated improved characteristics, including 96% capacitance retention after 5000 charge/discharge cycles and high energy efficiency (approximately 99%). These properties highlight its potential for application in solid-state supercapacitors.https://www.mdpi.com/2310-2861/11/1/68MnO<sub>2</sub>carbon xerogelhydrothermal synthesissolid-state supercapacitors
spellingShingle Vania Ilcheva
Victor Boev
Mariela Dimitrova
Borislava Mladenova
Daniela Karashanova
Elefteria Lefterova
Natalia Rey-Raap
Ana Arenillas
Antonia Stoyanova
Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
Gels
MnO<sub>2</sub>
carbon xerogel
hydrothermal synthesis
solid-state supercapacitors
title Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
title_full Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
title_fullStr Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
title_full_unstemmed Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
title_short Influence of Synthesis Conditions on the Capacitance Performance of Hydrothermally Prepared MnO<sub>2</sub> for Carbon Xerogel-Based Solid-State Supercapacitors
title_sort influence of synthesis conditions on the capacitance performance of hydrothermally prepared mno sub 2 sub for carbon xerogel based solid state supercapacitors
topic MnO<sub>2</sub>
carbon xerogel
hydrothermal synthesis
solid-state supercapacitors
url https://www.mdpi.com/2310-2861/11/1/68
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