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2.

Materials and methods


For the synthesis, Iron (III) chloride hexahydrate (Min. 98%,
VWR BDH Prolabo), Cobalt (II) chloride hexahydrate (Min. 98%,
VWR BDH Prolabo), Magnesium chloride hexahydrate (ACS
reagent, 99% Sigma-Aldrich ), Manganese (II) chloride
tetrahydrate (Reagent Plus >99% Sigma-Aldrich), Nickel (II)
chloride (Anhydrous, powder, 99% Sigma-Aldrich), Linseed Oil
(LO) and Sodium hydroxide were used. Distilled water is used to
prepare all the solution and all the chemicals were used as
received without any purification.
2.1. Preparation of nanocrystalline MFe2O4
Nanoparticles of MFe2O4 (M=Co, Mg, Mn, Ni) were prepared
by coprecipitation method in presence of Linseed Oil such as
surfactant. Requisite quantity of aqueous solution of 0.2M
MCl2xH2O was mixed with 0.4M FeCl36H2O under constant
magnetic stirring. After a digestion time of 30 min, 10mL of
linseed oil solution was added into above solution to restrict de
particle growth and as capping agent, followed by the addition
in dropwise of an aqueous solution of 3M NaOH. At this step the
emulsion becomes black in color and precipitate appears. The
pH of the mixture was continuously monitored and maintained
in the range of 11-12 with excess NaOH solution. Nanoparticles
were formed by conversion of metal salts into hydroxides, which
take place immediately. The solution was heated and
maintained at 80C and constantly stirred for 1 hour. This
duration was sufficient for the transformation of hydroxides into
MFe2O4 spinel ferrite. The reaction vessel was then cooled to
room temperature and magnetically decanted. A blackish
precipitate was separated and several time washed with water
and ethanol. All samples were heated in the furnace at 500 C
for 6 hours.
2.2. Structural characterization
The structural analysis of the annealed samples was
performed by powder X-ray Diffraction (XRD) using a X-ray

diffractometer (Bruker D8 ADVANCE) with CuK1 radiation ( =


0.15406 nm), data being handled by FullProf 2000 program. The
theromgravimetric experiments were conducted on a TG-DTA
92-1600 SETARAM thermoanalyzer under air atmosphere with a
heating rate of 10 C/min from room temperature to 700 C.
Infrared spectra of all samples were measured on a PerkinElmer Spectrum Two spectrometer between 4000 to 400 cm -1,
equipped with a diamond attenuated total reflectance (ATR)
accessory.

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