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HOME (HTTPS://EDUCATION.MRSEC.WISC.EDU) / SYNTHESIS OF AQUEOUS FERROFLUID NANOPARTICLES: BURET

SYNTHESIS OF AQUEOUS FERROFLUID

NANOPARTICLES: BURET
Procedure modified by Jonathan
Breitzer and George Lisensky from
“Preparation and Properties of an
Aqueous Ferrofluid
(http://jchemed.chem.wisc.edu/Journal/I
ssues/1999/Jul/abs943.html)” by
Patricia Berger, Nicholas B. Adelman,
Katie J. Beckman, Dean J. Campbell,
Arthur B. Ellis, and George C. Lisensky,
J. Chem. Educ., 76, 943-948 (1999).

A ferrofluid is a liquid made of nanoscale FERROFLUID

ferromagnetic particles dispersed evenly throughout PAGES
a carrier fluid. Ferrofluids become very strongly
magnetized in the presence of a magnetic field. Here,
Fe3O4 magnetite nanoparticles are produced by
mixing Fe(II) and Fe(III) salts together in a basic
BACKGROUND
solution.
FERROFLUIDS

SAFETY:
 Wear eye protection (HTTPS://E
DUCATIO
N.MRSEC.
Chemical gloves recommended
WISC.EDU
/FERROFL
Ferrofluids can be messy. The particular UIDS-
ferrofluid you will prepare will permanently BACKGRO
UND/)
stain almost any fabric.

PROCEDURE:
Step 1. (http://www.youtube.com/watch?
v=srUj4EsOW0M#t=8) Check that the iron solutions
are good since Fe(II) slowly reacts with O2 to become ACTIVITIES
Fe(III). Verify the solution colors!
FERROFLUID
SYNTHESIS
1 M FeCl3 in 2 M HCl AND HIGH
SCHOOL
TEACHING
2 M FeCl2 in 2 M HCl MODULE

Step 2. (http://www.youtube.com/watch? (HTTPS://E

DUCATIO
v=srUj4EsOW0M#t=17) Add 4.0 mL of 1M FeCl3 and N.MRSEC.
1.0 mL of 2M FeCl2 solution to a 100 or 150 mL WISC.EDU
/FERROFL
beaker.
UID-
SYNTHESI
Step 3. (http://www.youtube.com/watch? S-AND-
HIGH-
v=srUj4EsOW0M#t=35) Continue stirring with a glass
SCHOOL-
rod throughout the dropwise addition of 50 mL 1.0 M TEACHING
aqueous NH3 solution over a period of about 5-10 -
MODULE/)
minutes, adding approximately 1 mL every 10
seconds. Avoid addition that is faster than the FERROFLUID
ACTIVITY
solution can be mixed, but also avoid addition that is
so slow that the particles grow large. CAUTION: (HTTPS://E
DUCATIO
Although 1 M NH3 is fairly dilute, NH3 is a strong
N.MRSEC.
base. WISC.EDU
/FERROFL
UID-
Step 4. (http://www.youtube.com/watch?
ACTIVITY/)
v=srUj4EsOW0M#t=35) Let the magnetite settle. You
FERROFLUID
can speed the settling process by putting a magnet
SPIKE
under the container. ACTIVITY

(HTTPS://E
Step 5. (http://www.youtube.com/watch? DUCATIO
N.MRSEC.
v=srUj4EsOW0M#t=70) Decant (pour off) and discard WISC.EDU
the clear liquid without losing a substantial amount /FERROFL
UID-
of solid. This works best if you keep a magnet under
SPIKE-
the container. ACTIVITY/)

FERROFLUID
1. Transfer the solid to a weighing boat with the MAGNETIC
aid of a few squirts from a wash bottle. LIQUID
EXPERIMENT
2. Use a strong magnet to attract the ferrofluid to
(HTTPS://E
the bottom of the weighing boat. DUCATIO
N.MRSEC.
3. Pour off and discard as much clear liquid as WISC.EDU
possible, again keeping the magnet under the /FERROFL
UID-
weighing boat. MAGNETIC
-LIQUID-
4. Rinse with water from a wash bottle and decant EXPERIME
the rinse as before. NT/)

FERROFLUID
5. Remove the magnet. Add 1-2 mL of 25% PENNY
tetramethylammonium hydroxide. Use caution PUSH
EXPERIMENT
as this is a caustic chemical.
(HTTPS://E
6. Gently stir with a glass rod for at least a minute DUCATIO
to suspend the solid in the liquid. Use a strong N.MRSEC.
WISC.EDU
magnet to attract the ferrofluid to the bottom of
/FERROFL
the weighing boat. Pour off and discard the dark UID-
liquid. Move the strong magnet around and PENNY-
PUSH-
again pour off any liquid. If the ferrofluid does EXPERIME
not spike, continue to move the strong magnet NT/)
around, pouring off any liquid.

7. What happens when you move a magnet under

the ferrofluid? If you are using a very strong
magnet you might get more interesting results
by varying the distance of the magnet below the VIDEO
boat. LAB
MANUAL
Option: Obtain the powder x-ray diffraction
SYNTHESIS
spectrum (2θ = 25-65°) of the ferrofluid on a glass OF
slide (the aluminum holder is under the slide as a AQUEOUS
FERROFLUID
template.) Measure the peak width for several peaks NANOPARTICLES:
BURET
as shown at right. Diffraction peaks are a result of (HTTPS://E
constructive interference of X-rays reflected by DUCATIO
N.MRSEC.
crystal planes. The more planes the sharper the peak
WISC.EDU
so the smaller the crystallite size the broader the /SYNTHESI
diffraction peak. Estimate the particle diameter, S-OF-
AQUEOUS-
FERROFLU
where λ is the X-ray wavelength, Δθ is the peak-width ID-
at half-height (FWHM) and 2θ is the peak location. NANOPAR
TICLES-
(For even better results use the peak width of the BURET/)
sample minus the peak width of the same peak in a
SYNTHESIS
bulk sample as the peak width.) OF
AQUEOUS
FERROFLUID
QUESTIONS:
NANOPARTICLES:
1. Were you able to prepare ferrofluid and observe GLASS
ROD
spiking in the presence of a magnet? Pick one
(HTTPS://E
spike in the middle. How many spikes were DUCATIO
immediately around that spike and how were N.MRSEC.
WISC.EDU
they arranged? (You might draw a picture /SYNTHESI
viewed from above. If you did not observe S-OF-
AQUEOUS-
spiking with your sample, you will need to
FERROFLU
inspect a sample that did spike.) ID-
NANOPAR
2. Examine the starting FeCl2 and FeCl3 solids used TICLES-
GLASS-
to prepare magnetite (leave the solids in their
ROD/)
sealed containers.) How do they respond to a
magnet? Which is magnetic?

3. What is the purpose of the surfactant? Explain

chemically how the surfactant works to keep the
nanoparticles suspended.

4. What evidence do you have for the formation of

nanoparticles?

MATERIALS:
Stock solutions for 50 preparations
 2 M HCl (21 mL conc HCl in 250 mL water) for
making iron solutions.

2.0 M FeCl2(H2O)4 in 2 M HCl. (Each student

needs 1 mL. Dissolve 19.9 g in 50 mL 2 M HCl.
Verify color as you weigh out the solid. This
material dissolves readily but the solution reacts
with oxygen and should be freshly prepared.)

1.0 M FeCl3(H2O)6 in 2 M HCl (Each student

needs 4 mL. Dissolve 54.1 g in 200 mL 2 M HCl.
This material often dissolves slowly.)

1.0 M NH3 in water. (Each student needs 50 mL.

Dilute at least 200 mL of concentrated
ammonium hydroxide with water to 3.0 L. It
may be possible to use household ammonia; its
concentration varies and an initial estimate
would be 1.0 L household ammonia diluted to
3.0 L.) Open containers of ammonia will smell
bad and their concentration will decrease
leading to poor results.

25% tetramethylammonium hydroxide in water

(commercially available from Aldrich, Fisher,
etc.). A strong, fishy, amine odor indicates
hydrolysis products which may interfere with
the synthesis. In this case adding an additional
1-2 mL may help. This is a caustic chemical, so
exercise caution, especially in use with students
or young people.

EQUIPMENT:
A way for students to measure iron solutions
(one buret dispensing each iron solution works
well; individual pipets could also be used)

100 or 150 mL beakers

A way to slowly add the ammonia solution (a

buret or separatory funnel or eyedropper)
 Glass rods for stirring

Plastic weighing boats

Wash bottles

Disposable gloves

Strong craft magnets

Cow magnets

Option: XRD spectrometer and glass slides

YOUTUBE LINK:
http://www.youtube.com/watch?v=srUj4EsOW0M
(http://www.youtube.com/watch?v=srUj4EsOW0M)

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