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This work reports an electrochemical synthesis method for ferrous fluorosilicate (FFS) hexahydrate (FeSiF6 ·6H2O) nanopowders that exhibit strong luminescence and stability. It is thought that the intense photoluminescence in the red-yellow part of the spectrum in the created nanopowders is due to electronic defect states associated with silicon that are located deep within the FFS band gap.
Synthesis procedure of FFS nanopowders
· The synthesis of highly luminescent FFS nano-powder was achieved through the electrochemical process using bulk metallurgical substrates containing crystalline phases of iron disilicide (FeSi2) and silicon (Si).
· The electrochemical etching of the FeSi2/Si substrates was conducted for 180 minutes at a low temperature of 20°C in a PTFE anodization cell filled with a 1:1 mixture (by volume) of hydrofluoric acid (HF) and ethanol (C2H5OH) under a constant current mode of 100 mA cm2.
· A copper plate was used as the rear contact for the FeSi2/Si substrates, while a platinum wire served as the cathode. To prevent overheating of the etching solution, a one-second stop-etching pulse was applied after each one-second period of current on-pulse.
· After the anodization process, the sample was washed with ethanol, dried, and then scraped from the substrate. The yield of the product ranged from 3.5 to 5.0%, depending on the specific anodization conditions employed.