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Synthesis of Li 4 Ti 5 O 12 negative electrode material in a fluidized bed thermogravimetric analyzer
Author(s) -
Tao Ling,
Samih Said,
Sauriol Pierre,
Chaouki Jamal
Publication year - 2021
Publication title -
the canadian journal of chemical engineering
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.404
H-Index - 67
eISSN - 1939-019X
pISSN - 0008-4034
DOI - 10.1002/cjce.24030
Subject(s) - materials science , spinel , fluidization , fluidized bed , lithium (medication) , chemical engineering , thermogravimetric analysis , titanium oxide , titanium , scanning electron microscope , metallurgy , composite material , chemistry , medicine , organic chemistry , engineering , endocrinology
Spinel lithium titanate (Li 4 Ti 5 O 12 ) is the most promising negative electrode material for energy storage which can be applied in lithium‐ion batteries lithium‐sulphur batteries, and supercapacitors. However, the high cost of Li 4 Ti 5 O 12 powder and its high molecular weight limit its application due to the complicated synthesis process. In this work, a facile solid‐state reaction in a fluidized bed reactor was used for the first time to synthesize spinel Li 4 Ti 5 O 12 using lithium carbonate and titanium oxide as solid reactants. We investigated the fluidization behaviour of starting materials and studied different synthesis temperature in fluidized and fixed beds. X‐ray diffraction and scanning electron microscopy were employed to characterize the samples. The results demonstrate that the mixture of Li 2 CO 3 and TiO 2 had a complete fluidization velocity of 0.88 cm/s and showed good fluidization behaviour. Pure spinel Li 4 Ti 5 O 12 was obtained via solid‐state reaction in a fluidized bed reactor at 800°C for 30 minutes, which is much lower than a conventional solid‐state reaction in a fixed bed or muffle furnace. By this novel method, the micro‐sized Li 4 Ti 5 O 12 particles (6‐8 μm) have hollow porous structure composed of nano‐sized particles (<100 nm) synthesized. According to the experimental results, we proposed a different reaction mechanism for the synthesis of Li 4 Ti 5 O 12 in fluidized beds which explains how the Li 2 CO 3 and TiO 2 react to form hollow lithium titanate nano‐structured micro‐particles in fluidized beds. The bulk density, surface area, and bulk conductivity of the synthesized Li 4 Ti 5 O 12 are 3240 kg/m 3 , 4.6 m 2 /g, and 3.90 × 10 −6 S/cm, respectively.