Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor

Metal–organic frameworks (MOFs) are hybrid materials that are being explored as active electrode materials in energy storage devices, such as rechargeable batteries and supercapacitors (SCs), due to their high surface area, controllable chemical composition, and periodic ordering. However, the facil...

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Main Authors: Carolina Manquian, Alberto Navarrete, Leonardo Vivas, Loreto Troncoso, Dinesh Pratap Singh
Format: Article
Language:English
Published: MDPI AG 2024-02-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/14/4/353
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author Carolina Manquian
Alberto Navarrete
Leonardo Vivas
Loreto Troncoso
Dinesh Pratap Singh
author_facet Carolina Manquian
Alberto Navarrete
Leonardo Vivas
Loreto Troncoso
Dinesh Pratap Singh
author_sort Carolina Manquian
collection DOAJ
description Metal–organic frameworks (MOFs) are hybrid materials that are being explored as active electrode materials in energy storage devices, such as rechargeable batteries and supercapacitors (SCs), due to their high surface area, controllable chemical composition, and periodic ordering. However, the facile and controlled synthesis of a pure MOF phase without impurities or without going through a complicated purification process (that also reduces the yield) are challenges that must be resolved for their potential industrial applications. Moreover, various oxide formations of the Ni during Ni-MOF synthesis also represent an issue that affects the purity and performance. To resolve these issues, we report the controlled synthesis of nickel-based metal–organic frameworks (NiMOFs) by optimizing different growth parameters during hydrothermal synthesis and by utilizing nickel chloride as metal salt and H<sub>2</sub>bdt as the organic ligand, in a ratio of 1:1 at 150 °C. Furthermore, the synthesis was optimized by introducing a magnetic stirring stage, and the reaction temperature varied across 100, 150, and 200 °C to achieve the optimized growth of the NiMOFs crystal. The rarely used H<sub>2</sub>bdt ligand for Ni-MOF synthesis and the introduction of the ultrasonication stage before putting it in the furnace led to the formation of a pure phase without impurities and oxide formation. The synthesized materials were further characterized by powder X-ray diffraction (XRD) technique, scanning electron microscopy (SEM), and UV–vis spectroscopy. The SEM images exhibited the formation of nano NiMOFs having a rectangular prism shape. The average size was 126.25 nm, 176.0 nm, and 268.4 nm for the samples (1:1)s synthesized at 100 °C, 150 °C, and 200 °C, respectively. The electrochemical performances were examined in a three-electrode configuration, in a wide potential window from −0.4 V to 0.55 V, and an electrolyte concentration of 2M KOH was maintained for each measurement. The charge–discharge galvanostatic measurement results in specific capacitances of 606.62 F/g, 307.33 F/g, and 287.42 F/g at a current density of 1 A/g for the synthesized materials at 100 °C, 150 °C, and 200 °C, respectively.
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spelling doaj.art-2374545b31ed44bcbb5185db14df56012024-02-23T15:29:25ZengMDPI AGNanomaterials2079-49912024-02-0114435310.3390/nano14040353Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for SupercapacitorCarolina Manquian0Alberto Navarrete1Leonardo Vivas2Loreto Troncoso3Dinesh Pratap Singh4Department of Metallurgical Engineering, Faculty of Engineering, University of Santiago of Chile (USACH), Av. Lib. Bernardo O’Higgins 3363, Estación Central, Santiago 9170022, ChileDepartment of Metallurgical Engineering, Faculty of Engineering, University of Santiago of Chile (USACH), Av. Lib. Bernardo O’Higgins 3363, Estación Central, Santiago 9170022, ChilePhysics Department, Millennium Institute for Research in Optics (MIRO), Faculty of Science, University of Santiago of Chile (USACH), Avenida Victor Jara 3493, Estación Central, Santiago 9170124, ChileInstitute of Mechanical Engineering, MIGA Millennium Institute, University Austral of Chile, Valdivia 5090000, ChileDepartment of Metallurgical Engineering, Faculty of Engineering, University of Santiago of Chile (USACH), Av. Lib. Bernardo O’Higgins 3363, Estación Central, Santiago 9170022, ChileMetal–organic frameworks (MOFs) are hybrid materials that are being explored as active electrode materials in energy storage devices, such as rechargeable batteries and supercapacitors (SCs), due to their high surface area, controllable chemical composition, and periodic ordering. However, the facile and controlled synthesis of a pure MOF phase without impurities or without going through a complicated purification process (that also reduces the yield) are challenges that must be resolved for their potential industrial applications. Moreover, various oxide formations of the Ni during Ni-MOF synthesis also represent an issue that affects the purity and performance. To resolve these issues, we report the controlled synthesis of nickel-based metal–organic frameworks (NiMOFs) by optimizing different growth parameters during hydrothermal synthesis and by utilizing nickel chloride as metal salt and H<sub>2</sub>bdt as the organic ligand, in a ratio of 1:1 at 150 °C. Furthermore, the synthesis was optimized by introducing a magnetic stirring stage, and the reaction temperature varied across 100, 150, and 200 °C to achieve the optimized growth of the NiMOFs crystal. The rarely used H<sub>2</sub>bdt ligand for Ni-MOF synthesis and the introduction of the ultrasonication stage before putting it in the furnace led to the formation of a pure phase without impurities and oxide formation. The synthesized materials were further characterized by powder X-ray diffraction (XRD) technique, scanning electron microscopy (SEM), and UV–vis spectroscopy. The SEM images exhibited the formation of nano NiMOFs having a rectangular prism shape. The average size was 126.25 nm, 176.0 nm, and 268.4 nm for the samples (1:1)s synthesized at 100 °C, 150 °C, and 200 °C, respectively. The electrochemical performances were examined in a three-electrode configuration, in a wide potential window from −0.4 V to 0.55 V, and an electrolyte concentration of 2M KOH was maintained for each measurement. The charge–discharge galvanostatic measurement results in specific capacitances of 606.62 F/g, 307.33 F/g, and 287.42 F/g at a current density of 1 A/g for the synthesized materials at 100 °C, 150 °C, and 200 °C, respectively.https://www.mdpi.com/2079-4991/14/4/353nanomaterialsNi-basedmetal–organic frameworksH<sub>2</sub>bdtelectrochemical characterizationsupercapacitors
spellingShingle Carolina Manquian
Alberto Navarrete
Leonardo Vivas
Loreto Troncoso
Dinesh Pratap Singh
Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
Nanomaterials
nanomaterials
Ni-based
metal–organic frameworks
H<sub>2</sub>bdt
electrochemical characterization
supercapacitors
title Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
title_full Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
title_fullStr Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
title_full_unstemmed Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
title_short Synthesis and Optimization of Ni-Based Nano Metal–Organic Frameworks as a Superior Electrode Material for Supercapacitor
title_sort synthesis and optimization of ni based nano metal organic frameworks as a superior electrode material for supercapacitor
topic nanomaterials
Ni-based
metal–organic frameworks
H<sub>2</sub>bdt
electrochemical characterization
supercapacitors
url https://www.mdpi.com/2079-4991/14/4/353
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