Journal of Colloid and Interface Science 350 (2010) 51–57

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Journal of Colloid and Interface Science

www.elsevier.com/locate/jcis

Study of ferrofluids in confined geometry

Sangeeta Rawat a, Dietmar Fink b,1, Amita Chandra a,*
a
Department of Physics and Astrophysics, University of Delhi, Delhi 110 007, India
b
Helmholtz Center for Materials and Energy, D-14109 Berlin, Germany

a r t i c l e i n f o a b s t r a c t

Article history: The passage of swift heavy ions through dielectric layers (SiO2 or SiON) on silicon, creates ion tracks in
Received 18 March 2010 them. After the etching and filling of these ion tracks with a suitable material, a novel electronic structure
Accepted 12 June 2010 acronymed TEMPOS – ‘Tunable Electronic Materials with Pores in Oxide on Silicon’ has been realized.
Available online 19 June 2010
Several electronic devices, both, active and passive, have been fabricated and systematically studied in
the last few years. Sensors have also been successfully made and characterized using the TEMPOS struc-
Keywords: ture as it offers a high surface to volume ratio resulting in fast response time and high sensitivity of the
Swift heavy ions
sensor. In continuation with these studies, in the present paper, ferrofluids have been inserted in the ion
Etched ion tracks
TEMPOS structure
tracks to study their behaviour in confined geometry and for subsequently obtaining magnetic sensors. A
Ferrofluid comparative study has been done between the aqueous and non-aqueous ferrofluids. Insertion of the fer-
Magnetic sensor rofluids in the ion tracks exhibits a change in the I–V behaviour in the presence of a magnetic field which
can be exploited for obtaining the above said sensor.
Ó 2010 Elsevier Inc. All rights reserved.

1. Introduction ducting material (so-called ‘‘Tunable Electronic Materials with

Bombardment of a dielectric material with swift heavy ions
(SHI) creates damage/tracks in the material. For sufficiently high
energy transfer, the tracks of these ions will consist of continuous
channels of transformed material of a few nanometers width. Ion
irradiation of a given insulator does not lead to any significant
change in its electrical conductivity. Since, tracks in some materials
can be chemically revealed, the initial damages are also referred to
as latent tracks [1]. Both the diameter and track length depend
upon the type and energy of the beam as well as on the thermal
and electrical conductivity of the material.
It is often possible to dissolve (etch) insulators by a strong
chemical agent (etchant), e.g., by HF in case of SiO2 and SiON or
by NaOH in case of polycarbonate or polyethylene terephthalate.
Due to the modified material’s properties, the ion tracks will etch
at a faster rate than the bulk material and the track may therefore
be selectively etched forming nanopores, the so-called ‘‘etched ion
tracks”. Subsequently, the nanopores can be filled with a semicon-
ductor/metal to create in this way an anisotropically conducting
composite material. In a new type of nanoelectronics, A/B bilayer
structures were used, with B being a Si substrate and A being a
swift heavy ion irradiated insulating layer such as SiO2, SiON or a
polymer, which has been etched and filled with some (semi)con-
* Corresponding author. Fax: +91 11 27667061.
E-mail address: achandra@physics.du.ac.in (A. Chandra).
1
Present address: Physics Department, Universidad Autónoma Metropolitana-
Iztapalapa, Apartado Postal 55534, 09340 México, D.F., Mexico.
Pores in Oxide on Silicon” (TEMPOS) structures). Alternatively, A
can be a layer of a semiconducting or insulating material (such
as SnO2, C60 or organometals) in which the ion tracks exhibit con-
ductivities that differ by orders of magnitude from those ones of
the bulk (so-called ‘‘tunable electronically anisotropic material
on semiconductor” (TEAMS) structures. These structures may exhi-
bit properties of tunable resistors, capacitors, diodes, double-
diodes, transistors, logic gates etc. As the TEMPOS structures are
often influenced by physical and chemical parameters, they also
act as sensors. There is a range of parameters on which the TEM-
POS structure’s behaviour depends such as; the track type, track
shape, deposited materials etc. [2]. The construction and electronic
behaviour of these TEMPOS structure have been studied systemat-
ically in detail [3–10]. Other track bearing material such as cellu-
lose nitrate, polymers (polyimides, polysiloxanes, polysilanes,
PET) came into focus recently [11–17].
In the present paper, ferrofluids have been prepared and in-
serted in etched ion tracks as a first step towards obtaining mag-
netic sensors. The magnetic colloid, also known as ferrofluid, is a
colloidal suspension of fine magnetic particles dispersed in a liquid
carrier. The engineering application of ferrofluids rely upon their
basic properties such as retention of magnetic field, levitation of
magnetic and non-magnetic objects, micromagnetic and catalysis
associated with small particles, magnetic shielding and effects on
electrical parameters [18–22].
There are essentially two methods for preparing these magnetic
nanoparticles, viz; by size reduction [19] and by chemical precipi-
tation [23]. The size reduction method uses wet ball-mill grinding

0021-9797/$ - see front matter Ó 2010 Elsevier Inc. All rights reserved.
doi:10.1016/j.jcis.2010.06.035
52 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57
to obtain required magnetic nanoparticles while the chemical pre-
cipitation method is based on the chemical co-precipitation reac-
tion that produces magnetite from the mixture of ferric chloride
and ferrous chloride. To prepare nanoparticles, nowadays the
chemical precipitation is used.
Without an external field, the magnetic particles in a magnetic
fluid aggregate to form clusters due to the particle–particle inter-
action whereas in an external magnetic field, the magnetic parti-
cles tend to form chain-like clusters along the magnetic field
direction. This tendency of forming chain-like structure becomes
more evident by increasing the field strength. Fang et al. [24] found
that for a relatively weak magnetic field, a short chain forms along
the magnetic field while for strong magnetic fields, much longer
and straighter chain structure form along the magnetic field
direction.
A suitable coating of the metal oxide core of a ferrofluid’s ferro
phase results in its protection against metal oxidization (which de-
creases the magnetic properties) within the carrier fluid as well as
in the improvement in biocompatibility in case of bio-medical uses
[25]. The synthesis, protection, functionalization and application of
magnetic nanoparticles as well as properties of nanostructured
system have been discussed in detail by An-Hui Lu et al. [26].
Magnetic sensors detect changes or disturbances in magnetic
fields that have been created or modified and from them informa-
tion is derived on properties such as direction, presence, rotation,
or angle of the magnetic fields, or induced electrical currents. They
can be classified into low, medium and high field sensing range
sensors [27–31]. The present study is on the electrical behaviour
of magnetic nanoparticle filled ion tracks in the presence of mag-
netic field. Also, its potential as earth’s magnetic field sensor in
the range (1G–5G) has been explored.
2. Material and methods
The TEMPOS structure consists of a dielectric layer (SiO2 of
thickness 100 nm) on a silicon substrate (thickness 375 lm). The
dielectric layer has been irradiated by 350 MeV Au26+ swift heavy
ions. The latent tracks thus obtained have been etched by 4% HF
for 14 min to create open tracks into which ferrofluids have been
inserted. A thin layer of ferrofluid has been deposited on the sur-
face of the dielectric layer and into the etched ion tracks. Electrical
contacts have been made by two gold electrodes on the top surface
of SiO2/Si substrate. For insertion into the ion tracks, two types of
ferrofluids namely, ‘‘aqueous” and ‘‘non-aqueous” have been syn-
thesized by chemical precipitation method as given below. Note
that the carrier fluid conductivity for aqueous ferrofluids was much
Fig. 1. XRD of: (a) aqueous ferrofluid (Fe3O4) and (b) non-aqueous ferrofluid (oil based Fe3O4).
higher as compared to the carrier fluid of the non-aqueous
ferrofluids.
2.1. Aqueous ferrofluid synthesis
Magnetite (Fe3O4) particles have been prepared by chemical
precipitation of FeCl2 and FeCl3 (1:2 M ratio) by addition of 25%
ammonia solution using the method described by Racuciu et al.
[32] giving citric acid coated iron oxide particles:
2FeCl3 þ FeCl2 þ 8NH3 þ 4H2 O ! Fe3 O4 þ 8NH4 Cl
2.2. Non-aqueous ferrofluid synthesis
Analytical grade ferric chloride (FeCl36H20), ferrous chloride
(FeCl24H2O), oleic acid (C18H34O2), ammonium hydroxide (NH4OH)
and dodecane (C12H26) have been used to prepare oil based ferro-
fluid. These are oleic acid coated iron particles with oil (dodecane)
as carrier liquid as described by Maity and Agrawal [33].
In order to identify the crystal structure and determine the crys-
tallite size of the magnetic nanoparticles obtained by the above
two methods, the samples have been examined by a powder X-
ray diffractometer (D8Advance) with Cu Ka radiation at room tem-
perature. The crystal structure (fcc) of the nanoparticles has been
found to be the same as of bulk Fe3O4. The XRD diffractograms of
precipitated powder samples are given in Fig. 1a and b. The crystal-
lite size (employing the Scherrer relation) of Fe3O4 prepared in
aqueous ferrofluid (at a pH value 3.0), has been found to be
14 nm and oil based ferrofluid (at a pH value 3.8), has been found
to be 10 nm.
3. Results and discussion
The magnetic particles obtained as above have been inserted in
the etched ion tracks and the following studies have been done:
3.1. AFM studies
The atomic force micrographs of the ion tracks on SiO2 are
shown in Figs. 2–4. The imaging has been done in contact mode
with a cantilever of 5 lm tip diameter using Veeco instrument
(2002). The Fig. 2a and b shows the SiO2/Si surface (irradiated by
350 MeV Au 26+ ions beam of fluence 108/cm2) which has been
etched (by 4% HF for 14 min). In these images, parallel open tracks
can be seen. The individual track diameter has been found to be
20 nm.
 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57 53

Fig. 2. AFM of irradiated and etched SiO2 layer with different scan area and scan rate: (a) scan area 1.7  1.7 lm2 and scan rate 3.4 lm/s and (b) scan area of 500  500 nm2
and scan rate 750 nm/s.

Fig. 3. AFM image of aqueous ferrofluid filled tracks with different scan area and scan rate: (a) scan area 1  1 lm2 and scan rate 0.4 lm/s and (b) scan area of 500  500 nm2
and scan rate 1000 nm/s (empty tracks are marked by arrows).

The AFM micrographs in Fig. 3a and b are of the same SiO2/Si
substrate filled with aqueous ferrofluid (AFF) with different scan
area and scan rates. Fig. 3a shows that the tracks have been filled
by AFF. Fig. 3b, which has 500  500 nm2 scan area, shows 2 tracks
which are unfilled. So, there is possibility that, some of tracks re-
main empty. Similarly, Fig. 4a and b show tracks filled with oil
based ferrofluild (OFF).
3.2. BET measurements
To quantify the change in the pore/track volume when filled/
partially filled with magnetic particles, the Brunauer–Emmett–
Teller (BET) measurements have been done. It has been found that
the empty unetched pore volume is 0.0524 cm3/g and the surface
area is 182.9 ± 2.5 m2/g. When etched by aqueous hydrofluoric acid
solution, one gets well defined tracks leading to an increment in
both, pore volume (0.0853 cm3/g) and surface area (275.6 ± 3.)
m2/g). After depositing aqueous ferrofluid in the tracks, the pore
volume has been found to be 0.0445 cm3/g and surface area has
been found to be 195.0 ± 2.6 m2/g. These values lie between the
values for the unetched and etched tracks. This leads to the conclu-
sion that there are partially filled ion tracks. This observation cor-
roborates the AFM images of partially filled tracks (Fig. 3b).
3.3. Current/voltage characteristic
To study the response of the magnetic particles in a confined
geometry (ion tracks) to the magnetic field, the I–V behaviour of
the TEMPOS structure described above has been studied.
Fig. 5a shows the I–V behaviour of SiO2/Si substrate with empty
ion tracks, it is ohmic in nature. In the presence of magnetic field, it
behaves like a diode because ion tracks act as charge extraction
channels, Fig. 5b. This is also the first time when it is seen that
empty ion tracks have specific magnetic properties. Fig. 5b shows
that empty tracks are sensitive to the external magnetic field, i.e.,
display magnetic properties.
Earlier studies [34–38] on modified Si structures have also re-
vealed magnetic properties. Measurements have revealed that
spark processed-Si displays ferromagnetic ordering with a satura-
tion magnetization occurring at low fields. This is attributed to
the high density of paramagnetic centres (dangling bonds). Ferro-
magnetic hysteresis loop has also been observed at room temper-
54 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57

Fig. 4. AFM image of oil based ferrofluid filled tracks with different scan area and scan rate: (a) scan area of 2  2 lm2 and scan rate 0.5 lm/s and (b) scan area of
1  1 lm2 and scan rate 0.25 lm/s.

Fig. 5. I–V characteristic of SiO2/Si substrate (a) with empty ion tracks and (b) with empty ion tracks in the presence of external magnetic field.

ature in single crystalline silicon substrates implanted with Ar ions
and in silicon wafers irradiated by thermal neutrons [35]. It has
been suggested that the paramagnetic defects, i.e., the unpaired
spins of dangling bonds created during the implantation or irradi-
ation processes interact to yield the quasi-ferromagnetism ob-
served in defect or damage associated silicon [36]. It has been
shown that annealing spark processed-Si removes, in an irrevers-
ible manner, the ferromagnetic behaviour while, at the same time,
dramatically reducing the number of dangling bonds. It is there-
fore, being suggested that dangling bonds substantially contribute
to the ferromagnetic behaviour in the presently investigated quasi
ferromagnetic materials. Note that the dangling bonds in the pres-
ent case have also been substantially reduced by etching.
Thus, it can be said that an optimal number of dangling bonds
can lead to an appearance of ferromagnetic properties. Such den-
sity of dangling bonds is quite real on the internal surface of tracks
in Si and SiO2 [39].
When the magnetic nanoparticle filled TEMPOS structures are
placed in a magnetic field, the iron oxide particles in the fluid
change their orientation according to the field direction resulting
in different I–V behaviour for different ferrofluids. I–V measure-
ments have been done in the range 1G–5G in two different config-
urations for aqueous and non-aqueous ferrofluid as given below:
(i) In parallel magnetic field (1G, 2G, 3G, 4G, 5G).
(ii) In perpendicular magnetic field (1G, 2G, 3G, 4G, 5G).
As the magnetic particles are dispersed in different carrier flu-
ids, the properties of carrier fluids and ferrofluids play an impor-
tant role in I–V measurements and are given in Table 1.
3.3.1. Current/voltage study of aqueous ferrofluid in ion tracks
Fig. 6 shows the schematic diagram for the I–V measurement
setup. In the presence of magnetic field, bias from 32 to +32 V
has been applied and the current has been found to vary depend-
ing upon the field direction and the field strength. The residual
magnetic field has been subtracted to get the actually applied
magnetic field. This variation occurs due to the movement of
the magnetic particles in the ferrofluid in the direction of the ap-
plied field.
3.3.1.1. I–V in parallel magnetic field. Fig. 7a shows the variation in
the current of aqueous ferrofluid filled TEMPOS structure in a par-
allel magnetic field. As seen in this figure, the current magnitude in-
creases with field for both positive and negative applied potentials
till saturation is reached. It is observed that in this case, the magnetic
nanoparticles on the surface as well as the tracks start aligning in the
external magnetic field direction and saturate (align) at 2G. How-
ever, for a SiO2/Si (P) substrate without ion tracks, as the magnetic
particles are only at the surface, the magnetic dipoles align in the
field direction at a lower magnetic field i.e., 1G and thereafter, on
application of higher magnetic field P 2G, there is no significant
 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57 55

Table 1
Properties of carrier fluids and ferrofluids.

Type of ferrofluid Capping agent Carrier fluid Viscosity of carrier fluid pH value of Conductivity at 25 °C with cell constant 1.1 of
Carrier fluid Ferrofluid Carrier fluid (lS/cm) Ferrofluid
Aqueous ferrofluid Citric acid Distilled water 7.98  103 poise at 30 °C 6.7 3.0 21.4 3.84 mS/cm
Non-aqueous ferrofluid Oleic acid n-Dodecane 14  103 poise at 20 °C 6.9 3.8 0.4 0.4 lS/cm

Fig. 6. Schematic diagram for I–V measurement setup in presence of magnetic field.

Fig. 7. I–V characteristics of aqueous ferrofluid in the presence of parallel magnetic field: (a) TEMPOS structure and (b) SiO2/Si (P) substrate (without tracks) and aqueous
ferrofluid on the surface.

change in I–V, as seen in Fig. 7b. Note that the magnetic field has been
applied in the ascending order.
3.3.1.2. I–V in perpendicular magnetic field. The above has also been
done in perpendicular magnetic field. For positive as well as nega-
tive applied potential, the current increases with increment of field
till 3G. Thereafter, for higher magnetic field P4G, there is no signif-
icant change in I–V, Fig. 8a. As expected, higher magnetic fields are
required to saturate or align the dipoles when the magnetic field is
in the perpendicular direction. Fig. 8b is the I–V measurement with
SiO2/Si substrate without ion tracks and aqueous ferrofluid on the
surface. Unlike the I–V in parallel field, the I–V behaviour shows no
saturation in the perpendicular field up to 5G. Higher field
strengths would be required to attain saturation in this case.
Note that, after removal of magnetic field, the current retraces
its value in 24 h in both the (parallel and perpendicular)
cases.
3.3.2. Current–voltage study of oil based ferrofluid
Oil based ferrofluid has also been inserted into ion tracks and
the I–V measurements have been done, details of which are given
below.

Fig. 8. I–V characteristics of: (a) TEMPOS structure with aqueous ferrofluid in ion tracks in the presence of perpendicular magnetic field and (b) SiO2/Si (P) substrate (without
tracks), aqueous ferrofluid on the surface.
56 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57
Fig. 9. I–V characteristic of oil based ferrofluid in parallel magnetic field of TEMPOS
structure.
3.3.2.1. I–V characteristics in parallel magnetic field. In TEMPOS
structures filled with oil based ferrofluid, in parallel field, the cur-
rent for negative applied potential remains almost the same for all
fields. This may be attributed to the low conductivity and high vis-
cosity of the carrier fluid. However, it changes for positive applied
potential and saturates at field strength P4G, Fig. 9. I–V of SiO2/Si
without ion tracks and oil based ferrofluid on the surface shows no
significant change, this is attributed to the high viscosity of the oil
which restricts the movement of the magnetic nanoparticles.
The above has also been done for perpendicular magnetic field
but no significant changes in I–V have been observed due to the
low conductance and high viscosity of the carrier fluid.
Fig. 10a shows that both, the aqueous and oil based ferrofluid,
exhibit conductivity enhancement in the parallel magnetic field
in comparison to the perpendicular magnetic field. This is due to
the fact that in parallel magnetic field the magnetic particles can
easily align in the field direction. The figure also shows that the dif-
ference in conductivity between parallel and perpendicular field
(for a given carrier fluid) is more for oil based ferrofluid compared
to the aqueous ferrofluid. This is because inspite of the relatively
higher conductivity of water with respect to oil (Table 1), in the
aqueous ferrofluid, the water molecules get attached to the iron
oxide particles [40]; thereby hindering the movement/alignment
of magnetic particles, Fig. 10b.
4. Conclusions
It is well known that ion track technology enables us to obtain
deep vertical structures in solid surfaces due to the high aspect
Fig. 10. (a) Comparative behaviour of aqueous ferrofluid (AFF) and oil based ferrofluid (OFF) in parallel and perpendicular magnetic field of 1G and (b) bonding of H2O with
Fe3O4.
Fig. 11. Track profile and possibilities of agglomeration of nanoparticles in the ion
tracks.
ratio of the ion tracks. In the study reported in this paper, ferro-
fluids have been inserted into the tracks. As the shape of the
tracks is conical, there exists the possibility of agglomeration of
the ferrofluid́s magnetic nanoparticles in the tracks, Fig. 11. In
the presence of an external magnetic field, these magnetic
particles align in the field direction giving rise to modified I–V
behaviour.
From the above, it can be said that:
 ion tracks in non-metallic materials can possess ferromagnetic
characteristics. This result is in coincidence with work of other
authors where magnetic properties of Si-like structures have
been studied,
 ferromagnetism of tracks is weak and depends on the density
and configuration of paramagnetic centres (dangling bonds),
 by filling tracks with ferrofluids of different compositions, it is
possible in a wide region to vary magnetic and electrical prop-
erties of ion tracks and
 the resultant ferromagnetism of the ion track filled with ferro-
fluids can be determined by interaction of the magnetization
vectors of the empty track and the inserted ferrofluids.
In summary, it can be said that ferrofluids are inexpensive and
relatively easily synthesized magnetic materials which can be in-
serted in ion tracks. For both magnetic fluids studied in this work,
the current–voltage measurements have been found to be sensitive
to the applied magnetic field strength and direction making these
systems promising candidates for earth’s magnetic field sensors
(1G–5G).
 S. Rawat et al. / Journal of Colloid and Interface Science 350 (2010) 51–57
Acknowledgments
The authors wish to thank the University Grants Commission
(F.No. 32-52/2006), Council of Scientific and Industrial Research,
India and the University of Delhi for grant of funds. The authors
also wish to thank Mr. P.K. Bora, Department of Physics & Astro-
physics and Dr. Amit Saxena, Department of Chemistry, University
of Delhi, for help in AFM studies. The authors are grateful to the
operators at the Helmholtz Centre for Materials and Energy, Berlin
for irradiation of the samples. We also wish to thank Dr. S.A. Hash-
mi for BET measurements. Critical reading and inputs from Prof. A.
Kiv is also gratefully acknowledged.
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