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Abstract
In this review, we will report a series of investigations on the homemade homogeneous magnetic uids. The most spectacular
property discussed in our research is the ordered structure of the magnetic columns formed in the magnetic uid thin lm under
the inuence of the external magnetic eld, either perpendicular or parallel to the lm surface. It is worth noting that the ordered
structure can be manipulated by changing the control parameters. This reveals the variability of the ordered structure. With the
ordered structures, some signicant magneto-optical characteristics such as magnetochromatics, birefringence, and eld-
dependent transmittance are generated. These optical properties form the groundwork for further development of related
optical devices by using the homogeneous magnetic uid lms. q 2001 Elsevier Science Ltd. All rights reserved.
1. Introduction and technology during this period was the sprouting of the
nanoscale science and technology [810]. Nanoscience and
In the early part of the 20th century, almost all the efforts technology emphasize materials of small dimensions, typi-
of scientists were put into dealing with the diverse phenom- cally 1100 nm, which connect the macroscopic and the
ena of the solid matter. The conceptual paradigm of the solid microscopic areas of research. Strict control of the chemical
matter is the picture of a dense periodic lattice and basis of and structural perfection of the samples is the essence of the
atoms. This paradigm has been spectacularly successful in nanoscale technology. These novel techniques capable of
describing the properties of solid matter and continued to fabricating nanoscale building blocks have opened up a
underlie much of the ongoing work. However, in the 1960s, revolutionary method of exploring material properties and
a particular class of materials appeared [17], named soft device characteristics, and the work is expanding rapidly
material, whose properties and behaviors are absolutely worldwide. Therefore, nanoscience is a very broad and
different to those of solid matter. This leads to a remarkable interdisciplinary area of research and hence brings tremen-
evolution from the solid state science to the condensed dous common interests of research to chemists, physicists,
matter science. In general, the soft materials, which are metallurgists and engineers. Generally, the worldwide
characterized by the fact that they are easily deformed by research of nanoscience is carried out in nanoparticle,
external stresses, electromagnetic or gravitational elds, nanostructured materials and nanodevices [11]. Among
etc., may include uids, liquid crystals, polymers, emulsions these categories, the work on the dispersion of nanoparticles
and colloids. With the high sensitivity and actuation, the in liquids or polymers leads to a hybrid of nanoscience and
application of soft materials is growing and showing the the soft material. These materials possess properties of both
versatile industrial interest of these smart materials contain- soft materials and nanoparticles, and also, show fruitful
ing soft building blocks. commercial impacts.
In the meantime, the other signicant progress in science Magnetic uid (also called ferrouid), which consists of
colloidal magnetic nanoparticles dispersed with the aid of
* Corresponding author. Tel.: 1886-2-8931-6233; fax: 1886-2- surfactants in a continuous carrier phase, is a typical hybrid
2930-9439. of soft material and the nanoparticle. The ferrouid was rst
E-mail address: phyfv001@scc.ntnu.edu.tw (H.E. Horng). synthesized successfully in the 1960s [12,13]. A magnetic
0022-3697/01/$ - see front matter q 2001 Elsevier Science Ltd. All rights reserved.
PII: S 0022-369 7(01)00108-1
1750 H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764
powder was reduced to colloidal nanoparticles by using ball- gonal structure of magnetic columns acts as a two-
milling grinding in the presence of a surfactant and liquid dimensional grating.
carrier. The average diameter of the dispersed particles Owing to the versatility of the structural patterns and the
ranges from 5 to 10 nm. Each particle in the uid behaves magnetically induced optical properties of the ferrouid
as a constant magnetic dipole moment proportional to its lms under external magnetic elds, the research on ferro-
size and can align with an external magnetic eld freely, uid is spreading rapidly all over the world. In this report,
but due to the low production efciency through the ball- we will rst give an overview of the structural pattern
milling grinding process, another method of chemical preci- formation of the magnetic columns in the ferrouid thin
pitation was then developed in the 1970s [14]. Because of lm under magnetic elds, and then exhibit the framework
the improvement in the manufacture process, the ferrouid of the application of the ferrouid based on the remarkable
becomes popular and hence the interest of scientists is optical properties caused by these magnetically induced
attracted to the area of the research. This research is mainly structures.
focused on the structural forming systems of ferrouids
under magnetic elds [1520], the magnetically induced
optical properties [2124], and the applications in mechan- 2. Structure in the magnetic uid lms under external
ical related work [2529], optical devices [3032] or even magnetic elds
in medicine [33].
As mentioned above, the ferrouids contain enormous To observe the structural patterns of magnetic uids (or
magnetic nanoparticles in the uid, and hence can be inu- ferrouids) under external magnetic uid elds, magnetic
enced by either parallel or perpendicular magnetic eld. uid is usually sealed in a glass cell with a thickness of
Under parallel magnetic elds, magnetic chains were several to tens of micrometers. The applied magnetic eld
found in ferrouid lm [24,34,35]. This leads to the is either parallel (parallel eld) or perpendicular (perpendi-
magnetic-eld induced birefringence of the ferrouid cular eld) to the plane of the lm. The images of the struc-
[21,24], and also, the birefringence can be controlled by tures in the magnetic uid lm are taken with an optical
varying the eld strength [24,36,37]. A similar phenomenon microscope and are recorded with a CCD video camera.
has been observed for the liquid crystal, which is also one of A variety of different pattern-forming systems of
the soft materials exhibiting birefringence under or without magnetic uid lms under external magnetic elds have
electric eld. As we know, the electric-eld modulated bire- been studied. In this section, we illustrate structure evolu-
fringence of the liquid crystals is applied widely in optical tion in the lm and the ngering behavior of magnetic
devices, such as liquid crystal displays, switches, etc.. This microdrops under external magnetic elds.
suggests that there is a good chance of developing optical
devices by utilizing the magnetic-eld induced birefrin- 2.1. Structure evolution
gence of ferrouid.
On the other hand, under perpendicular elds, many In this part, the structure evolution in the magnetic uid
researchers indicated that disordered two-dimensional lm under parallel or perpendicular magnetic elds is sepa-
lattices of magnetic columns, which are agglomerated rately discussed.
by magnetic nanoparticles, are formed [17,38,39].
Other investigators have generated more highly ordered 2.1.1. Parallel magnetic elds
two-dimensional lattices in thin lms of magnetic emul- When a magnetic uid lm is subjected to a parallel
sions [40], ferrouids containing non-magnetic spheres magnetic eld, a portion of the magnetic particles in the
[41] or concentrated ferroluids based on a mineral uid agglomerate to form needle-like chains in the magnetic
solvent [42]. However, these lattices tend to solidify uid lm [34,46,47]. A typical picture of the needle-like
and therefore are not suitable for applications requiring chains is shown in Fig. 1. Some researchers suggest that
rapid interconversion between crystalline and amorphous the agglomeration of magnetic particles is due to phase
states. After the success in synthesizing highly homoge- separation, which results from the thermodynamical
neous ferrouids in our recent work [43], we found an instability of the dispersion of magnetic particles [48,49].
ordered hexagonal structure pattern of magnetic columns By looking upon the magnetic uid as a binary solution of
all over the ferrouid lm under uniform perpendicular solvent molecules and colloidal particles, Taketomi et al.
magnetic elds exceeding a critical value [19]. Later, an used Debye's critical opalescence theory to establish a ther-
unprecedented structure evolution in the ferrouid lm modynamical instability theory of colloidal particles disper-
under perpendicular elds was discovered [44]: agglom- sion for interpreting the agglomerating behavior [16].
eration, disordered columns phase, multi-level ordered As the eld strength is further increased, more particles
hexagonal structure through a transition phase. The participate in the agglomeration and needle-like chains are
ordered hexagonal structure of magnetic columns in the distributed randomly in the lm. Yusuf et al. showed that
ferrouid lm results in a novel optical property of two separated chains merge and that the chains become
magnetochromatics [23,45], which reveals that the hexa- longer under a higher eld [35]. It was also found that the
H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764 1751
Fig. 2. Periodic long-chain structural patterns formed in a magnetic uid lm subjected to perpendicular elds exceeding a critical value, at: (a)
different eld strength with constant sweep rate or (b) different sweep rate with a given eld strength [51]. The thickness of the lm is 5.0 mm
and the concentration of the uid is 22.4%.
1752 H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764
Fig. 4. (a) Initial (t 1 min) disordered columns and (b) nal (t 120 min) hexagonal column patterns when the magnetic uid lm of 10 mm
thickness cell was subjected to a perpendicular magnetic eld, H 200 Oe [18]. Five-fold and seven-fold co-ordinated columns were observed
along the grain boundaries in the nal pattern.
H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764 1753
Fig. 8. Magnied photo images of the detailed transition phase of magnetic uid thin lm subjected to a perpendicular magnetic eld at a low
sweep rate of 5 Oe/s [44]. (a) First-level hexagonal structural pattern, (b) transition phase, (c) column elongation, (d) column necking, (e)
column breaking, (f) second-level hexagonal structural pattern. In (b)(e), a typical column breaking process of a particular column in the
transition phase is circled.
H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764 1755
Fig. 11. Shape evolution of microdrops in the magnetic uid thin lm during the application of the perpendicular magnetic eld [60]. Time
increases downward. The dH/dt is 1 Oe/s. The diameters of initially near circular microdrops through a to d are 8.6, 12.8, 13.2 and 19.8 mm.
labyrinthine structure forms in the lm (Fig. 9(d)). If the application of the external magnetic eld at dH/dt 1 Oe/
strength is even higher, the labyrinthine structure becomes s. In Fig. 11(a) and (b), both of the drops with representative
an equilibrium hexagonal structure (Fig. 9(e) and (f)). On diameters of 8.6 and 12.8 mm evolved from a circular shape
the other hand, at a higher sweep rate, these drops evolve to to a dumbbell structure. For the drops with diameters of 13.2
a branched structure (Fig. 10(b) and (c)), to a labyrinthine and 19.8 mm (shown in Fig. 11(c) and (d)), the circular
pattern (Fig. 10(d) and (e)) and nally to an equilibrium drops evolved into a branched, instead of a dumbbell, struc-
hexagonal structure (Fig. 10(f)). It must be noted that the ture.
labyrinthine structure is indeed an intermediate state; this Since the surface tension minimizes the length of droplet
disagrees with the results given by prior reports [5558]. contour and also a drop's surface energy, the energy by the
The causes of the pattern formation are believed to be surface tension of the dumbbell structure is lower than that
mainly the competition between surface tension, the bulk- of the branched structure. Thus, a dumbbell structure is
induced magnetic dipole interactions and the attractive force formed when the surface tension dominates the ngering
from the external magnetic eld. At the initial circular shape process, whereas a branched structure results when the
phase, the surface tension dominates. From the labyrinthine bulk-induced magnetic dipole interaction suppresses the
pattern to hexagonal structures, the magnetic dipole inter- effect of the surface tension. By comparing the inference
action dominates the surface tension, causing the breakup of with the experimental results shown in Fig. 11, it can be
connectivity of dumbbells or branched structure in the concluded that the surface tension is a crucial factor in
labyrinthine phase. This breakup repeats until the system determining the shape evolution of smaller drops. On the
reaches an equilibrium state, and the system becomes hexa- other hand, the magnetic dipole interaction becomes more
gonal. Here, the repulsive force, due to dipole interaction, signicant than the surface tension during the ngering
and the attractive interaction, due to the external eld, domi- process for larger drops.
nate. When sweeping the eld back to the zero eld state, The experimental results also imply that a critical
the system changes from a hexagonal structure to a disor- diameter ac for a given sweep rate, which differentiates
dered column phase, and then to the initial circular form. these two evolved shapes, exits. Through a careful inspec-
Thus, the process of pattern formation in microdrops of tion, the ac for dH/dt 1 Oe/s was found to be approxi-
magnetic uid is irreversible. mately 13.0 mm. Furthermore, an empirical relationship
In addition to the sweep rate, the size effect of magnetic between the ac and the dH/dt was obtained to be ac / (dH/
uid drops on ngering behavior has also been investigated dt) p with p~ 2 0.14 [60].
[60]. The results are shown in Fig. 11. The upper images in In summary, the agglomeration of magnetic particles in
Fig. 11(a)(d) denote the initial contour of the microdrops the magnetic uid lm under external magnetic elds is
under a zero eld. The middle images represent the instant attributed to the thermodynamical instability of particles.
images of the corresponding initial contours during the In contrast to the disordered chain/column phase reported
H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764 1757
Fig. 14. C-M rotation angle Dh versus the applied magnetic eld
[37]. The inset is the relationship between the Dh and r, where r is
the area ratio of the long chains to the liquid carrier.
Fig. 15. The enlarged I-h curves at h around 2908 under H 150 Oe and dH/dt 50 Oe at various u's are plotted in (a), (b) and (c) [66]. The
concentration of the magnetic uid is 11.7% and the thickness of the lm is 5 mm.
Hence, to investigate the interplay between the magnetic arly polarized. By combining the transmitted electric elds
chains and the incident light, the electric eld of a linearly through phases I and II, we obtain elliptical polarization for
polarized incident light into phase I is decomposed into the the transmitted light. Also, the C-M rotation is then calcu-
longitudinal and the transverse electric elds. The trans- lated by nding the angle between the two transmission axes
mitted electric elds of these two components are then of the incident and the transmitted lights. The detailed deri-
calculated independently. For the phase II, the homoge- vation for the C-M rotation is developed in Ref. [37] and the
neous liquid carrier exhibits an isotropic refractive index. analytic expression of Dh is also given.
Hence, the light transmitted through phase II remains line- The experimental data shown in Fig. 16 are tted to the
theoretical Dh (u) curve (denoted by a solid line). A good
agreement between the experimental data and the theoreti-
cal prediction can be obtained. This strongly implies that the
birefringence of the magnetic uid lms under parallel
magnetic elds is due to the long chain formation in the
lm. Meanwhile, the interactions between the incident
light and both the long chains and the liquid carrier must
be taken into account to describe the C-M rotation of the
magnetic uid lms.
3.1.2. Transmittance
Due to the feasibility of optical devices such as the optical
switch and the magnetic eld sensor, the optical transmit-
tance of magnetic uid lms are attracting the interest of a
growing number of scientists, which is currently focused on
the concentration, thickness and magnetic eld and sweep
rate-dependent transmittance. Martin et al. indicated that the
transmittance of a magnetic uid lm is reduced substan-
tially for uids of a higher concentration [68]. Our recent
experimental results show that the transmittance decreases
exponentially with the increasing thickness of the lm under
a xed magnetic eld [69]. The attenuation distance of the
Fig. 16. Fitting between the experimental Dh (u) data and the theo-
retical curve [66]. Dots denote experimental data, while the line
incoming light through a diluted magnetic uid thin lm is
represents the theoretical predictions obtained from the two-phase then found to be hundreds of micrometers.
model. The nII is the tted refractive index of phase II (liquid To study the effects of the magnetic eld and the sweep
carrier) and the DnI denotes the difference between the refractive rate on the transmittance, the transmitted intensities through
index nIp of the longitudinal electric eld and that nIn of the trans- a homogeneous magnetic uid lm under perpendicular
verse electric eld of the incident light. magnetic elds were detected by one of the authors [70].
1760 H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764
Fig. 17. Normalized intensity of an unpolarized He-Ne laser light as Fig. 18. Normalized intensity of a polarized He-Ne laser light as a
a function of eld strength and its sweep rate for a magnetic uid function of parallel eld strength and its sweep rate with the insets
lm of thickness 6 mm subjected to a perpendicular magnetic eld of typical structure patterns, for a magnetic uid lm of thickness
[70]. The concentration of the uid is 27.8% 5 mm oriented with an angle u 458 between the direction of the
eld and the axis of polarizer [70]. The concentration of the uid is
22.4%.
In the experiment, an unpolarized He-Ne laser light was
incident perpendicularly to the lm and the transmitted
intensity was probed in the direction of light propagation When a magnetic eld is applied along the lm surface,
by using a photomultiplier tube and a monochromator. The chains are formed and a birefringence is then induced.
relative intensities of the transmitted light as a function of The birefringence leads to an elliptically polarized trans-
eld strength for various sweep rates are shown in Fig. 17. mitted light. Thus, non-zero intensity can be detected as
All the intensities are normalized with respect to zero eld the transmitted light passes through the analyzer. Fig. 18
intensity. The intensity decreases as the eld strength gives the normalized intensity of the transmitted light
increases. At low elds (,60 Oe), the intensity curves are measured directly after the analyzer as functions of the
almost independent of the sweep rate. Contrarily, at higher eld strength for various sweep rates. In contrast to the
elds (.60 Oe), the curves become sweep rate dependent. It reduction in the transmitted intensity with the increasing
shows that the intensity curves separate into two regions; eld strength for the magnetic uid lm under perpendicular
one is sweep rate dependent and the other is independent of magnetic elds, these curves show that transmitted intensity
sweep rate. increases under higher eld strength. Through a close
Through an investigation on the structures in the lm inspection, the intensity initially increases as the eld
under the corresponding eld strength and sweep rate, it strength increases (,20 Oe), independent of the sweep
was found that the disordered column phase occurred rate. When the eld strength is further increased
under H , 60 Oe and the hexagonal ordered structure (.20 Oe), the intensity tends to saturate. The intensity satu-
resulted as H $ 60 Oe. This suggests that structure forma- rates at a relatively low eld strength for a higher sweep
tion plays an important role in the magnetically modulated rate. These curves also show that a critical value ( < 20 Oe)
transmittance of the magnetic uid lm under perpendicular divides these curves into two regions; one is independent of
elds. Also, the effect of the sweep rate becomes signicant sweep rate and the other is sweep rate dependent.
to the transmittance of the lm exhibiting hexagonal ordered Since the structural patterns in the magnetic uid lm are
structures. dominant to the transmittance, we then investigated the
On the other hand, the transmittance generated by the structural pattern in magnetic uid lms under parallel
birefringence of the magnetic uid lm under magnetic magnetic elds. It was found that a transition from disor-
elds parallel to the plane of the lm was examined dered short chains to a nearly periodic long-chain structure
[51,70]. The experimental set-up is shown in Fig. 12. occurred at 20 Oe, which coincides with the critical eld in
Here, u is set at 458 and h is at 2908. Under a zero eld, Fig. 18. The typical structures of short chains and periodic
the transmitted intensity is zero due to the orthognality of long chains corresponding to these regions are shown as the
the two transmission axes of the polarizer and the analyzer. insets of Fig. 18. It is worth noting that the magnetically
H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764 1761
Fig. 19. Experimental set-ups [45]. (a) For the observation of hexagonal structure patterns in magnetic uid thin lms subjected to a magnetic
eld perpendicular to the plane of lm. A: CCD video camera; B: PC; C: microscope; D: solenoid; E: magnetic uid thin lm; and F: current
source. (b) For the observation of magnetochromatic effect of magnetic uid thin lms subjected to a magnetic eld perpendicular to the plane
of lm. A: white light source; B: telescope; C: lens; D: aperture; E: mirror; F: current source; G: solenoid; H: magnetic uid lm; I: photo lm;
J: PC; K: monochromator; L: photomultiplier tube; M: stepping motor controller; and N: stepping motor with optical ber.
modulated transmittance shown in Figs. 17 and 18 suggests evolution in the transmitted intensity follows I(t) Io[1 2
a possibility for the development of optical devices such as exp(2t/t)], where t is the response time of transmittance
optical switches. and the time is counted from the moment at which the
magnetic eld changes. The experimental results show
3.1.3. Response time that t is about tens of milliseconds, which was also observed
For the development of optical devices by utilizing the by Martin et al. [68] by using a similar experimental
magnetically modulated transmittance of the magnetic uid method.
lm, it is necessary to know the corresponding optical
response time. To probe the response [71], we used a He- 3.2. Magnetochromatics
Ne laser to emit light incident normally to the magnetic uid
lm under perpendicular magnetic elds. The transmitted When a homogeneous magnetic uid thin lm is
intensity through the lm was detected by using a photo- subjected to perpendicular magnetic eld, initial disordered
diode with a response time of several nanoseconds. The columns form. At a critical eld strength, an equilibrium
signal detected by the photodiode was then converted to a two-dimensional hexagonal structure forms with columns
voltage signal via an analog-digital converter. Thus, the occupying lattice vertices [44,72,73]. The distance d
time evolution of the transmittance through the magnetic between two columns was found to be several micrometers
uid lm can be measured. [31,54]. Thus, the hexagonal structure may act as a two-
The magnetic eld was provided by a solenoid. By chan- dimensional optical grating which is capable of diffracting
ging the current applied to the solenoid, the magnetic eld an incoming visible light. The set-up illustrated in Fig. 19
was varied. The time constant of charging or discharging the was used to demonstrate magnetochromatic effects resulting
current is tens of microseconds by using a constant current from the diffraction of light through the ordered structure
source (Keithley 228). It was found that the transmitted [23,73].
intensity I through the magnetic uid lm increases to a In the experiment, a white light was emitted from a light
saturated value Io when the magnetic eld is reduced source. After passing through the lens, the white light
suddenly from a higher value to a lower one. The time became parallel and was then incident normal to the lm.
1762 H.E. Horng et al. / Journal of Physics and Chemistry of Solids 62 (2001) 17491764
Table 1
The column distance d and grating angle u, including the conditions of H, dH/dt, f and L [45]. The ucal, is calculated via the relation ucal sin 21
(l/d) with l being 535 nm, while the uexp is obtained experimentally
No. L (mm) f (%) H (Oe) dH/dt (Oe/s) d (mm) ucal (8) uexp (8)
This reveals that the hexagonal structure in the magnetic denotes the required eld strength to achieve the ordered
uid lm under perpendicular magnetic elds can act as a structure in the magnetic uid lm. Hence the material
two-dimensional tunable grating. with Hh less than 50 Oe is suitable for applications.
In summary, the physical origin of the birefringence for Fundamentally, the present research seems to lack a strict
the magnetic uid lm under parallel magnetic elds is description of the mechanism of formation of the column/
conrmed to be the formation of long chains. The variation chain, the structure of the intra column/chain, etc. These are
in the structural pattern in the lm under various magnetic also important prospects for further research in the area.
elds leads to the magnetically modulated optical transmit- As reported in this review article, signicant optical prop-
tance. Besides, the hexagonal structure generates the erties of the ferrouid forecast a promising opportunity for
magnetochromatic effect as a white light passes through it. the wide application in optical devices, such as optical
The properties show a feasibility of application of magnetic switches, lters, or optical lens, and some other advanced
uids in optical devices, such as optical switch, lter or optical components. As one can see, these explorations
tunable grating. require integrated co-operation among aspects of specialists
in the future. It is believed that this spark of wisdom will
have many commercial impacts.
4. Conclusion We are looking forward to the ferrouid playing an
important role in both fundamental research and applica-
The structures of the agglomeration of the magnetic nano- tions in the coming century.
particles have been reviewed in this report. Through the
tremendous research on ferrouids in recent years, the
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