Alternative route for LiFePO4 synthesis: Carbothermal reduction combined with microwave-assisted solid-state reaction. (February 2017)

• Record Type: Journal Article
• Authors: Smecellato, Pamela C.; Davoglio, Rogério A.; Biaggio, Sonia R.; Bocchi, Nerilso; Rocha-Filho, Romeu C.
• Is Part Of: Materials research bulletin. Volume 86(2017)
• Page Start: 209
• Page End: 214
• Publication Date: 2017-02
• Subjects: A. Inorganic compounds -- B. Chemical synthesis -- C. Electron microscopy -- C. Thermogravimetric analysis -- D. Electrochemical properties; Materials -- Periodicals; Crystal growth -- Periodicals; Matériaux -- Périodiques; Cristaux -- Croissance -- Périodiques; Crystal growth; Materials; Periodicals; 620.11
• DOI: 10.1016/j.materresbull.2016.11.003
• Languages: English
• ISSNs: 0025-5408

Abstract

Graphical abstract: Highlights: Short-time LiFePO4 synthesis in a practical setup using domestic microwave oven. LiFePO4 can be prepared combining carbothermal and microwave heating steps. LiFePO4 nanoparticles are obtained in only 3 min of microwave calcination. Fast and easy method proposed to prepare a material for lithium ion intercalation. Abstract: LiFePO4 was synthesized via a microwave-assisted solid-state reaction. The precursors LiOH·H2 O, FePO4 ·4H2 O, glucose, and graphite were first subjected to carbothermal reduction at 200 °C during 3 h and subsequently calcined under microwave irradiation at 800 W for very short times varying from 1 to 5 min. The products obtained at different microwave calcination times were systematically investigated through thermal (TGA-DTG and DSC), structural (XRD), morphological (SEM), and electrochemical (cyclic voltammetry) analyses. The best results were attained for the product obtained at the microwave calcination time of 3 min: smallest particle size (majority in the range of 100–150 nm), crystallographic pattern of LiFePO4 and some by-products, and voltammetric profile characteristic of LiFePO4 . Thus, the here-presented synthesis methodology implies a significant reduction in processing time while yielding LiFePO4 nanoparticles with good electrochemical activity for the Li ion intercalation process.