Thermal annealing dynamics of carbon-coated LiFePO{sub 4} nanoparticles studied by in-situ analysis
- Department of Chemistry and Applied Biosciences, ETH Zurich, Vladimir-Prelog-Weg 1, 8093 Zurich (Switzerland)
- Department of Mechanical and Process Engineering, ETH Zurich, Sonneggstrasse 3, 8092 Zurich (Switzerland)
The thermal behavior of core-shell carbon-coated lithium iron phosphate (LiFePO{sub 4}-C) nanoparticles made by flame spray pyrolysis (FSP) during annealing was investigated by in-situ transmission electron microscopy (TEM), in-situ X-ray powder diffraction (XRD) as well as ex-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Crystallization of the initially glassy LiFePO{sub 4}-C nanoparticles starts at quite low temperatures (T=400 °C), forming single crystals inside the confinement of the carbon shell. Upon increasing the temperature to T≥700 °C, LiFePO{sub 4} starts to diffuse through the carbon shell resulting in cavities inside the mostly intact carbon shell. By increasing the temperature further to T≥800 °C, the initial core-shell morphology converts into open carbon shells (flakes and cenospheres) and bulky LiFePO{sub 4} particles (diameter in the range 300–400 nm), in agreement with ex-situ experiments. - Graphical abstract: TEM images of a typical sample area recorded at room temperature and after heating in-situ heating reveal the growth of particles and the formation of empty carbon cages. - Highlights: • LiFePO{sub 4} coated by a carbon shell is produced by flame spray pyrolysis. • The amorphous LiFePO{sub 4} starts to crystallize at 400 °C as revealed by in-situ XRD. • Crystal growth was visualized by TEM heating experiments. • The formation of empty carbon cages starts at 700 °C.
- OSTI ID:
- 22658033
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: Part 1 Vol. 242; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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