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Synthesis of Aqueous Ferrofluid: Laboratory Exercise 3
Synthesis of Aqueous Ferrofluid: Laboratory Exercise 3
Synthesis of Aqueous Ferrofluid: Laboratory Exercise 3
Laboratory Exercise 3
Morley, Jacob
CHEM 314 TA: Gulsah Uygur
11 February 2014
Morley 1
Background and Introduction
Magnetic nanoparticles in colloidal suspensions are deemed ferrofluids. A colloidal
solution is a suspension in which particles are sufficiently small to remain in solution and not
gravitationally settle rapidly. Ferrofluids are capable of aligning themselves with magnetic fields.
This laboratory exercise aimed to prepare ferrofluid with Fe
3
O
4
(magnetite) nanoparticles, via a
mixture of Fe (II) and Fe (III) salts in a basic solution. A surfactant was added to prevent the
nanoparticles from folliculating. Fe (II) and Fe(III) are both paramagnetic materials that contain
unpaired d-block electrons. Specifically, the unpaired electrons cause the paramagnetic field, as
paramagnetic molecules results from partially unfilled orbitals and can respond to magnetic
fields. The unpaired electrons with the parallel spins create the magnetic field. The ferrofluids
exhibit spikes when acted upon by a strong magnet.
For synthesis, the relevant reaction is as follows:
2FeCl
3
+ FeCl
2
+ 8NH
3
+ 4H
2
O Fe
3
O
4
+ 8NH
4
Cl
The resulting magnetite is then mixed with aqueous tetramethylammonium hydroxide to
complex the magnetite with tetramethylammonium cations and hydroxide anions and to induce
repulsion between the magnetite (Fig 1.1).
Fig. 1.1. Role of tetramethylammonium hydroxide from [2].
Beyond the Curie temperature, a temperature at which solids begin to lose their magnetic
properties as heat prevents their electrons from aligning in magnetic domains, magnets are
suboptimal [3]. Accordingly, ferrofluids can serve to augment traditional magnet application in
environments in which traditional magnets are suboptimal [4].
Morley 2
Experimental Procedure
Four mL of 1M FeCl
3
and 5mL of 2M FeCl
2
were added to a clean 100mL beaker. A
glass stirring rod was used to stir the solution while a pipette was used to add 50mL of 1M
aqueous NH
3
dropwise from a 100mL beaker at a rate of approximately 10mL/minute. The
magnetite was allowed to settle, during which a strong magnet was placed beneath the solution
for settlement acceleration. With the magnet still beneath the solution, the solution was decanted
and the clear fluid was discarded. The solid magnetite was transferred into a weigh boat with the
magnet beneath to ensure efficient transfer. A wash bottle was used to remove additional
magnetite. This process was repeated to remove any additional liquid. Two mL of 25%
tetramethylammonium hydroxide were added to prevent aggregation (i.e. as a surfactant). After 1
minute of stirring, with a magnet beneath the weigh boat, the dark liquid was decanted and
discarded, with the solid preserved. The magnet was moved below the weigh boat to explore the
properties of the ferrofluid. Spiking was recorded.
Morley 3
Data and Observations
Procedural Step Observation
Associated Reaction/
Molecular Interaction
Mixing of FeCl
3
and
FeCl
2
Orange FeCl
3
and light green FeCl
2
mixture forms clear-orange mixture
2FeCl
3
+ FeCl
2
+ 8NH
3
+
4H
2
O Fe
3
O
4
+ 8NH
4
Cl Addition of aqueous
NH
3
Mixture turns a deeper orange.
Reaction mixture turns from orange
to brown-red to dark brown to black.
Solid black particles settle
gravitationally.
Decanting of solution
Extremely viscous liquid/nearly solid
black remains. Removed liquid is
clear (i.e. no black magnetite visible).
--
Addition of
N(CH
3
)
4
+
OH
,
decanting
Solution remains black, increases in
viscosity.
N(CH
3
)
4
+
OH