Synthesis of Ferrofluid

Valentin Uzunov (author), Tom Ronay and Hans Harshfield

PSU ID#: 964100377
CHM 229H, Lab 269


ABSTRACT
The current report details a simple method for the synthesis of aqueous based ferrofluid. The
synthesis method is based on the reaction between aqueous iron(II) and Iron(III) ions with
aqueous ammonia solution, to form magnetite, Fe
3
O
4
precipitate. The nanoparticles of magnetite
produced were then mixed with a surfactant, tetramethylammonium hydroxide (CH
3
)
4
NOH,
forming a colloidal suspension of the magnetite crystals. When a magnet was applied to the
colloid suspension, spikes formed along the surface of the fluid, and varied in size and numbers
depending on the strength of the magnetic field.

EXPERIMENTAL
Magnetite nanoparticles were synthesized by reacting 1.0 mL of 2.0 M FeCl
2
, 4.0 ml of 1.0 M
F
3
Cl
3
and 50 mL of 0.7 M aqueous ammonia solution:
2 FeCl
3
(aq) + FeCl
2
(aq) + 8 NH
3
(aq) + 4 H
2
0 Fe
3
O
4
(s) + 8 NH
4
Cl (aq)
[Rxn 1]
Ammonia was added drop wise at a rate of 5-7 drops per second using a 50 mL buret, while the
solution was constantly stirred. The precipitate formed was allowed to settle before excess liquid
was decanted. Remaining solution was further separated, using a centrifuge for 1 min at 1000
rpm. Any remaining supernatant was then decanted and the remaining magnetite precipitate was
mixed thoroughly with 8 mL 25% aqueous tetramethylammonium hydroxide (CH
3
)
4
NOH
solution. It is important that final product be not to moist or dry.

RESULTS
The final product of the synthesis was a dark black liquid, wish a viscosity somewhat similar to
that of the solvent. When a magnetic field from a strong magnet (Neodymium magnet) was
placed near the liquid, it responded by forming spikes on its surface (Figure 1).
Figure 1 shows the synthetizes product. The magnetic field from the
magnetic field passing through the fluid is causing the spike
formation










It was observed that the size of the spikes
depended on the viscosity if the liquid.
When the fluid was to wet (saturated with
water), the spikes created with the magnet were smaller and less well defined. When excess
water was removed, the spikes were bigger in size and formed well defined sharp points.
It was also observed that the distance of the magnet from the fluid had an influence on the spike
length. When the magnet was touching the weight boat the spikes were small and tightly packed.
When the magnet was withdrawn, the spiked grew in size and were less tightly packed.

DISCUSSION
The objective of the current experiment was to replicate the ferrofluid synthesis process
described by Berger et al. (1999) in the Journal of Chemical Education.
In the current experiment, the removal of ammonia, though vacuum aspiration was omitted from
the procedure. It would expected that by removing any excess ammonia from the precipitate the
ferrofluid formed would be of higher quality and and likely form large spikes [1]. Despite so, the
product synthesized, without this step was of sufficient quality to display the desired magnetic
behavior common to ferrofluids.
The magnetic properties of the synthesized fluid are due to the magnetic properties of magnetite
particles in the colloidal suspension. Ferrofluids display an interesting physical property, which
is the formation of spikes at their surface in the presence of a sufficiently strong magnetic field
(ie. from a neodymium magnet). The spike formation can be attributed to the surface instability
of the suspended particles in the fluid, causing constant small waves on the surface. When a
vertical magnetic field, strong enough to overcome the surface tension of the fluid is applied, the
amplitude of these surface waves increases along the magnetic field lines. Depending on the
strength of the interactions between the magnetite particles and the magnetic field, it will
determine the maximal size the spikes can reach [1].
Along with the quality of the fluid, an inverse relationship was observed between the number and
size of spikes and the distance of the magnet from the fluid. This observation can be explained
by the dissipating strength of the magnetic field with distance from the source.
The success of the experiment demonstrates the effectiveness of the synthesis procedure used.
The quality of the final product can be adjusted in further trials to improve the quality of the
product. One way to do so, would be to adjust the initial concentrations of the reactants, as the
product of the magnetite is sensitive to the stoichiometry between Fe2+ ions and Fe3+ ions. The
ratio and positioning between Fe2+ and Fe3+ in the magnetite crystals is important, as it
determines the net magnetization of the crystals, and in turn how well the fluid will respond to
the external magnetic field [1].
It would also be of interest to compare the difference in quality of fluid synthesized when excess
ammonia was remove from the precipitate before mixing with surfactant, as recommended by
Berger et al., compared to current results

CITATIONS
[1] Berger, Patricia; Adelman, Nicholas B; Beckman, Katie J; Campbell, Dean J; Ellis, Arthur B;
and Lisensky, George C. Preparation and Properties of an Aqueous Ferrofluid", Journal of
Chemical Education, 1999, 76(7), 943.