A new strategy to quickly synthetize true nanoparticles of the spinel LiMn2O4 by using a microwave-assisted hydrothermal route

Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel LiMn2O4 (LMO) at a low temperature (140 °C) and short reaction time (5 min), using exclusively water-soluble reagents. The obtention of this mate...

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Published in:	Journal of alloys and compounds Vol. 911; p. 164856
Main Authors:	Silva, Daiane Piva B., Falqueto, Juliana Bruneli, Bocchi, Nerilso, Biaggio, Sonia R., Rocha-Filho, Romeu C.
Format:	Journal Article
Language:	English
Published:	Lausanne Elsevier B.V 05-08-2022 Elsevier BV
Subjects:	Crystal structure Discharge Electrochemical analysis Electrodes Emission analysis Energy storage material Energy-saving microwave-assisted hydrothermal route Genuinely nanostructured spinel LiMn2O4 High resolution electron microscopy Hydrothermal reactions Inductively coupled plasma Li-ion battery Lithium manganese oxides Low temperature Nanoparticles Reaction time Reagents Spinel Energy storage material Li-ion battery Genuinely nanostructured spinel LiMn2O4 Energy-saving microwave-assisted hydrothermal route
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Abstract	Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel LiMn2O4 (LMO) at a low temperature (140 °C) and short reaction time (5 min), using exclusively water-soluble reagents. The obtention of this material was confirmed by using different techniques such as X-ray diffractometry, Rietveld crystal structure refinement, inductively coupled plasma-atomic emission spectroscopy and high-resolution transmission electron microscopy. Electrochemical evaluations were performed by using cyclic voltammetry and galvanostatic charge and discharge tests. Only electrodes prepared from spinel LMO nanoparticles with an average size of ~15 nm showed electrochemical activity. From charge and discharge tests at a constant rate of C/5, the electrodes prepared from this active material exhibited an initial specific capacity of 128 mA h g–1 with a capacity retention of 95% after the 27th cycle. The hallmark of the synthesis route here described is the saving of energy while preparing truly nanoparticulate LMO with excellent chemical, structural and promising electrochemical properties. [Display omitted] •Highly pure nanoparticles (≤15 nm) of LiMn2O4 (LMO) are prepared by a new route.•The LMO preparation is based on a microwave-assisted hydrothermal reaction (MWH).•Low temperature, short time and water-soluble reagents are used in the MWH reaction.•LMO nanoparticles show excellent chemical, structural and electrochemical properties.
AbstractList	Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel LiMn2O4 (LMO) at a low temperature (140 °C) and short reaction time (5 min), using exclusively water-soluble reagents. The obtention of this material was confirmed by using different techniques such as X-ray diffractometry, Rietveld crystal structure refinement, inductively coupled plasma-atomic emission spectroscopy and high-resolution transmission electron microscopy. Electrochemical evaluations were performed by using cyclic voltammetry and galvanostatic charge and discharge tests. Only electrodes prepared from spinel LMO nanoparticles with an average size of ~15 nm showed electrochemical activity. From charge and discharge tests at a constant rate of C/5, the electrodes prepared from this active material exhibited an initial specific capacity of 128 mA h g–1 with a capacity retention of 95% after the 27th cycle. The hallmark of the synthesis route here described is the saving of energy while preparing truly nanoparticulate LMO with excellent chemical, structural and promising electrochemical properties. Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel LiMn2O4 (LMO) at a low temperature (140 °C) and short reaction time (5 min), using exclusively water-soluble reagents. The obtention of this material was confirmed by using different techniques such as X-ray diffractometry, Rietveld crystal structure refinement, inductively coupled plasma-atomic emission spectroscopy and high-resolution transmission electron microscopy. Electrochemical evaluations were performed by using cyclic voltammetry and galvanostatic charge and discharge tests. Only electrodes prepared from spinel LMO nanoparticles with an average size of ~15 nm showed electrochemical activity. From charge and discharge tests at a constant rate of C/5, the electrodes prepared from this active material exhibited an initial specific capacity of 128 mA h g–1 with a capacity retention of 95% after the 27th cycle. The hallmark of the synthesis route here described is the saving of energy while preparing truly nanoparticulate LMO with excellent chemical, structural and promising electrochemical properties. [Display omitted] •Highly pure nanoparticles (≤15 nm) of LiMn2O4 (LMO) are prepared by a new route.•The LMO preparation is based on a microwave-assisted hydrothermal reaction (MWH).•Low temperature, short time and water-soluble reagents are used in the MWH reaction.•LMO nanoparticles show excellent chemical, structural and electrochemical properties.
ArticleNumber	164856
Author	Falqueto, Juliana Bruneli Bocchi, Nerilso Rocha-Filho, Romeu C. Biaggio, Sonia R. Silva, Daiane Piva B.
Author_xml	– sequence: 1 givenname: Daiane Piva B. surname: Silva fullname: Silva, Daiane Piva B. – sequence: 2 givenname: Juliana Bruneli surname: Falqueto fullname: Falqueto, Juliana Bruneli – sequence: 3 givenname: Nerilso surname: Bocchi fullname: Bocchi, Nerilso email: bocchi@ufscar.br – sequence: 4 givenname: Sonia R. surname: Biaggio fullname: Biaggio, Sonia R. – sequence: 5 givenname: Romeu C. surname: Rocha-Filho fullname: Rocha-Filho, Romeu C.
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CitedBy_id	crossref_primary_10_1016_j_matchemphys_2023_127699 crossref_primary_10_1016_j_ces_2023_118600 crossref_primary_10_1016_j_jallcom_2023_168704 crossref_primary_10_1016_j_jallcom_2022_166537 crossref_primary_10_1007_s11581_023_05132_6 crossref_primary_10_1016_j_jpowsour_2022_232307 crossref_primary_10_1002_smtd_202201152 crossref_primary_10_1149_1945_7111_acf8fd crossref_primary_10_2139_ssrn_4198028 crossref_primary_10_1016_j_matlet_2023_134838
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Keywords	Energy storage material Li-ion battery Genuinely nanostructured spinel LiMn2O4 Energy-saving microwave-assisted hydrothermal route
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Snippet	Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel... Based on a microwave-assisted hydrothermal reaction, a new route is proposed to prepare highly pure true nanoparticles (≤15 nm) of the single-phase spinel...
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SubjectTerms	Crystal structure Discharge Electrochemical analysis Electrodes Emission analysis Energy storage material Energy-saving microwave-assisted hydrothermal route Genuinely nanostructured spinel LiMn2O4 High resolution electron microscopy Hydrothermal reactions Inductively coupled plasma Li-ion battery Lithium manganese oxides Low temperature Nanoparticles Reaction time Reagents Spinel
Title	A new strategy to quickly synthetize true nanoparticles of the spinel LiMn2O4 by using a microwave-assisted hydrothermal route
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