Preparation of Precursor Solution:
Dissolve 1.09 g of FeCl₃·6H₂O and 0.609 g of SC(NH₂)₂ in a beaker containing 80 mL of ethylene glycol (for pure Fe₃S₄ phase, Greigite).
(If a mixed phase of Fe₃S₄ and FeS₂ is desired, use 60 mL ethylene glycol and 20 mL distilled water instead.)
Place the beaker on a magnetic stirrer and stir the solution until complete dissolution is achieved (Yellowish hazel color).
Hydrothermal Reaction:
Transfer the well-mixed solution into a Teflon-lined stainless-steel autoclave.
Seal the autoclave and place it inside an electric oven preheated to 180°C.
Maintain the reaction for 12 hours until a black powder forms, indicating Fe₃S₄ formation.
Cooling and Washing Process:
Allow the autoclave to cool naturally to room temperature before opening.
Collect the black precipitate and wash it twice with distilled water and once with ethanol.
Use centrifuge tubes to hold the sample and place them in a centrifuge set at 8000 rpm for 8 minutes (optional; for low rpm use more time) to separate impurities.
Transfer the residue into a beaker and use a mixer to evenly mix the fluids and sample.
Drying the Fe₃S₄ NPs:
Place the washed precipitate inside a vacuum oven and dry it overnight to obtain pure undoped Fe₃S₄ nanoparticles.