Arch Appl Mech

DOI 10.1007/s00419-015-1092-6

SPECIAL

Stefan Odenbach

Microstructure and rheology of magnetic hybrid materials

Received: 19 October 2015 / Accepted: 11 December 2015

Springer-Verlag Berlin Heidelberg 2016

Abstract In this paper, an overview on a class of materials with high actual research interest will be given.
Magnetic hybrid materials, i.e. liquid or elastic matrices filled with magnetic nano- or micro-particles provide
the possibility to influence their mechanical behaviour by application of technically easily realizable magnetic
fields. In particular, the viscous and elastic behaviour of magnetic hybrid materials can be influenced by
magnetic fields. The physical reason for these changes are field-induced reconfigurations of the microstructure
formed by the magnetic particles. Experimental techniques to observe these changes and their relation to
changes in the mechanical behaviour of magnetic hybrid materials will be in focus of this review.

Keywords Magnetic hybrid materials Magnetovisocus effect Magnetorheological effect

1 Introduction

Magnetic hybrid materials, i.e. magnetic nano- or micro-particles embedded in a nonmagnetic matrix, have
attracted scientific interest since more than 50 years. The main reason for this long-lasting scientific activity is
given by the fact that these materials allow a change of their properties and mechanical behaviour, for example
of their flow, if a liquid matrix is used, due to the action of external magnetic fields.
Since magnetic fields can easily be controlled concerning their strength and spatial distribution, tailored
forces can be exerted to magnetic hybrid materials giving rise to the development of applications as well as
new opportunities for basic research.
To classify magnetic hybrid materials, one has to distinguish first of all the matrix that is used. This matrix
can either be a liquid material or a solid matrix like an elastomer.
Going back in history, magnetorheological fluids have been the first magnetic hybrid material described
[13]. In these fluids, magnetic micro-particles are suspended in a Newtonian carrier liquid, usually in an oil.
Due to the application of a magnetic field, these fluids exhibit non-Newtonian behaviourespecially field-
depended yield stress caused by structure formation of the magnetic particleswhich is induced by their
dipoledipole interaction. The most prominent application for magnetorheological materials is dampers with a
magnetically adjustable damping constant which are actually used in a growing number of modern cars [48].
A related material is ferrofluids, in which the suspended magnetic particles are nanosized leading to high
sedimentation stability and thus to an excellent long-term stability of the suspension itself [9,10]. In these fluids,
magnetic forces can be used to control the flow behaviour, which is of severe importance for basic research
in fluid mechanics [11,12], but can also be used for innovative applications, for example in the biomedical
field, where magnetic drug targeting using ferrofluids as a drug carrier [10,13,14] has become a promising
therapeutic approach for cancer treatment. In these fluids, changes of the viscous behaviour do also appear
S. Odenbach (B)
TU Dresden, Chair of Magnetofluiddynamics, Measuring and Automation Technology, 01062 Dresden, Germany
E-mail: Stefan.Odenbach@tu-dresden.de
 S. Odenbach

[15], but compared to magnetorheological fluids they are small. Thus, it has been assumed for a long time that
these changes are of academic importance only. Nevertheless, as we will see later on, field-induced changes
of the viscous behaviour may severely influence applications of these fluids, especially if the carrier liquid is
not a simple Newtonian fluid, but a liquid with complex viscous behaviour. The actually ongoing research of
ferrofluids suspended in non-Newtonian liquids led to a third class of magnetic hybrid materials, ferrofluids
in complex matrices.
The fourth class of magnetic hybrid materials are those with a matrix as an elastic solid. In these magne-
torheological elastomers [16] or gels [17], changes of the E-modulus of the material can be induced by the
action of magnetic fields. This class of magnetic hybrid materials, which finds scientific interest since about 10
years only, is actually growing dramatically. Changes of the matrix from elastomers to gels and hydrogels [18],
the use of nano- and micro-particles as well as the choice of magnetically hard and magnetically soft particles
or mixtures of them [1922] have shown that a tremendous range of properties and possibilities for magnetic
influence can be created by a sufficient choice of the composition of the magnetorheological elastomers.
Within this contribution, we will focus on the question how magnetically induced changes in the viscous
or elastic behaviour of magnetic hybrid materials can be explained by changes of the microstructure of the
respective materials. We will especially focus on experimental methods for the determination of changes in
the microstructure, and it will be outlined how important such changes can be if particular applications are in
focus of interest. For this review, we will reduce the broad field of magnetic hybrid materials to ferrofluids
and, related to them, ferrofluids in complex matrices as well as magnetorheological elastomers.

2 Magnetoviscous effects in ferrofluids and their microscopic reason

As mentioned above, ferrofluids are suspensions of magnetic nanoparticles with a diameter of about 10 nm
in an appropriate carrier liquid. The particles are usually magnetite, but in certain experimental fluids iron
or cobalt particles are used too. The carrier liquid can be water, oils or organic solvents, depending on the
application of the liquid. Usual volume concentrations of magnetic particles in ferrofluids range about 7 vol%.
Due to their small size, the particles would agglomerate due to van der Waals interaction and have thus to be
coated with long-chained surfactant molecules. With an appropriate coating, long-term stable suspensions can
be generated, which do not show any change of their properties over decades (for an overview on ferrofluids,
see e.g. [10,15,23]).
Magnetic particles with a size in the range of 10 nm are magnetic single domain particlesthat means that
the suspension is an ensemble of thermally agitated magnetic dipoles, and thus, the fluid shows paramagnetic
behaviour in the presence of a magnetic field. In contrast to paramagnetic salt solutions, the initial susceptibility
of ferrofluids is in the order of one and thus about four orders of magnitude larger than in a paramagnetic
salt solution. The reason for this difference is given by the fact that the magnetic particles, containing about
104 Bohr magnetons, interact with the magnetic field, compared to single molecules, which bear a few Bohr
magnetons only, in a salt solution. This high initial susceptibility gives rise to the fact that small magnetic fields
and field gradients are able to exert significant forces on a ferrofluid as shown in Fig. 1. These strong forces
led to the development of numerous applications since the first synthesis of ferrofluids and opened fascinating
possibilities for basic research in fluid mechanics.
In addition, the interaction between the magnetic field and the magnetic particles will give rise to changes
in the viscosity of a ferrofluid. To understand this basically, one can have a look on a magnetic particle in a
shear flow as shown in Fig. 2. When a magnetic field is applied perpendicular to the vorticity of the flow, the
magnetic moment of the particle will be aligned with the field direction. In case that the magnetic moment
is fixed within the particle, the mechanical torque exerted by the flow will try to turn the magnetic moment
out of the magnetic field direction causing a magnetic torque counteracting the mechanic torque. This will
lead to a hindrance of the free rotation of the particles in the flow and thus to an increase in viscosity. This
effect, first measured by McTague in 1969 [24] and explained in detail by Shliomis in 1972 [25], would lead to
maximum relative change in viscosity equal to 1.5 times the volume concentration of magnetic particles in the
fluid. Thus, for example for a fluid containing 7 vol% of magnetic particles a maximum change of viscosity
of about 10 % would be expected for rotational viscosity.
Measuring the change of viscosity in a commercial ferrofluid would lead to significantly higher viscosity
changes as shown in Fig. 3 [26]. These changes cannot be explained by the theoretical approach of rotational
viscosity. If one looks on such strong changes, the assumption that interaction of the magnetic particles will
lead to structure formation enhancing the viscosity changes seems to be a logic approach [15]. Nonetheless,
Microstructure and rheology of magnetic hybrid materials

Fig. 1 A ferrofluid attracted to the pole shoe of a small electromagnet. Even a weak magnetic field of about 10 mT is able to exert
a force strong enough to generate a flow of the ferrofluid against gravitational acceleration towards the pole shoe. The structure
of spikes appearing is given by a counterplay of magnetic forces, surface tension and gravitational acceleration

Fig. 2 Principle explanation for the appearance of magnetic field-induced changes in the viscous behaviour of ferrofluids [15].
Explanations are given in the text

one has to take into account that only sufficiently large magnetic particles, that is particles with a diameter of
about 16 nm for magnetite particles, will exhibit magnetic dipoledipole interaction strong enough to form
structures, for example chains, in the fluid. The portion of these particles in a ferrofluid is usually very small,
since larger particles have a negative effect on the sedimentation stability of the fluid. Nonetheless, it could
be shown that increasing mechanical load on a ferrofluid, given by a change in shear rate, will decrease the
appearing changes of viscositya phenomenon that can be related to mechanic break-up of chains formed by
magnetic dipoledipole interaction [15].
Experiments with purified ferrofluids [27,28] were able to show that a decrease in the amount of large
particles with a mean diameter of about 16 nm would lead to significant reduction in those viscosity changes,
usually called magnetoviscous effect. Theoretically this approach has been described by Zubarev [29,30],
assuming that only the large magnetic particles will contribute to viscosity changes due to structure formation
forced by the magnetic dipole interaction. Calculating the free energy of an ideal gas of magnetic particle chains
and minimizing this free energy as a function of the chain length distribution function led to a possibility to
calculate the viscosity changes and to compare them with experimental findings. As shown in Fig. 4, good
agreement between theory and experimental data for sufficiently small shear rates can be obtained with a mean
diameter of the large particles about 16.5 nm and a volume fraction of this species of magnetic particles of
about 0.7 vol%values which fit well with the experimentally determined size distribution for these fluids
[30].
 S. Odenbach

Fig. 3 Change of viscosity in commercial ferrofluid with 7 vol% of magnetic particles in a magnetic field. Only about 0.4 vol%
of these particles are large enough to be able to contribute to rotational viscosity resulting in the dashed line for the prediction of
Shliomis theory [15]

Fig. 4 The change of viscosity in a commercial ferrofluid for three very low shear rates. The lines are the result of a theoretical
fit (for = 0.1s1 ) for the theory of Zubarev [29,30], while for the higher shear rates the shear thinning effect is modelled by
limiting the summation over the chain length distribution function at a maximum value given by the equilibrium condition in [31]

To finally prove the assumption that chain formation of magnetic particles lead to the magnetoviscous
effects, one needs first an experimental approach to detect the chain structures. Due to the small size of the
magnetic particles, all kinds of microscopic techniques are not sufficient for this task. A way out is small-angle
neutron scattering (SANS) experiments where changes in the scattering pattern will prove changes in the
microstructure.
Figure 5 shows in the upper part small-angle neutron scattering images taken for a ferrofluid containing
0.38 vol% of cobalt particles for two different directions between magnetic field and neutron beam [32]. The
shown images represent the difference between the scattering pattern taken at rest for the respective field and
the scattering pattern for a shear rate of 1 s1 . As seen, there are significant differences which indicate that
different structures are present in the fluid.
To interpret such scattering patterns of a highly complex material, Monte Carlo simulations of the respective
situation of a ferrofluid are needed. The figures in the lower part of Fig. 5 represent the result of such simulations.
As seen, the anisotropy of the scattering patterns is excellently reproduced in the Monte Carlo simulations
[23]. Thus, the structure found in the Monte Carlo simulations can be assumed to be the particle structure in
the ferrofluid, under test. Figure 6 shows the structural information obtained by the simulations and, as can
easily be seen, chain formation of magnetic particles is the reason for the magnetoviscous effects [30].
Microstructure and rheology of magnetic hybrid materials

Fig. 5 The difference between small angle neutron scattering patterns taken at rest and for a shear rate of 1s1 with a magnetic
field strength of 200 mT applied for two different directions between neutron beam and magnetic field. The upper part shows
the experimentally obtained patterns, while the low images are the result of Monte Carlo simulations for the same boundary
conditions [23]

Fig. 6 The particle structure obtained from Monte Carlo simulations from which the scattering patterns in Fig. 5 are calculated
[23]

3 Magnetorheological elastomers: three-dimensional analysis of microstructural changes

The second class of magnetic hybrid materials to be discussed here is magnetorheological elastomers. In these
hybrid materials, typically magnetic micro-particles are embedded in a polymeric matrix [16]. The particles
ranging in size from a few micrometres to about 50 m are made of carbonyl iron and their mass content in
 S. Odenbach

the hybrid material depends mainly on the investigation to be undertaken. While magnetorheological elas-
tomers dedicated to technical application are usually loaded with about 80 m% of magnetic particles [16],
samples for basic investigations may contain only a few mass per cent to enable investigations for example
of the microstructure. Beside polymeric matrices, actually gels [17] and hydrogels [18] come more and more
into focus of investigations, especially in basic research. In addition to soft magnetic carbonyl iron particles,
hard magnetic particles, for example NdFeB particles, can be used [2022]. Depending on the magnetic field
conditions during the curing process of the elastomer, either isotropic samples with homogeneously distrib-
uted magnetic particles can be produced if the elastomer is cured under zero field conditions. Alternatively,
anisotropic samples can be obtained in which chain-like structures are generated by a magnetic field applied
during the curing process.
In magnetorheological elastomers loaded with soft magnetic particles an active change of the E-modulus
can be achieved by application of magnetic fields [16]. In magnetorheological elastomers loaded with hard
magnetic particles, a passive magnetorheological effect can be obtained, if a sample is magnetized after
curing [20]. By mixing magnetically hard and soft particles, a combination of the active and the passive
magnetorheological effects becomes possible, which gives rise to numerous additional possibilities tailoring
the material for certain applications [21].
It is known from literature that the magnetorheological effect changes significantly with the volume con-
centration of magnetic particles, the elasticity of the matrix and especially with the anisotropy of the magne-
torheological elastomer. In case of anisotropic magnetorheological elastomers, it is of quite severe importance
in which direction magnetic field, particle structure and mechanical load are aligned to each other.
A focused tailoring of these materials for certain applications requires much more knowledge about
microstructural processes driving the change in the elastic properties. Finally, it will be necessary to gen-
erate a scale bridging understanding of the mechanical properties of magnetorheological elastomers.
Due to the comparably large size of the particles, completely different techniques can be applied to inves-
tigate the microstructure as well as microstructural changes generated by the application of external stimuli
like magnetic fields or mechanical loads.
In the past years, X-ray microtomography has been established as a powerful tool for microstructural
investigations of magnetorheological elastomers [3335]. Due to the high X-ray contrast between the mag-
netic particles and the elastomer, the particles and their distribution inside the elastomer can be identified.
Moreover, by appropriate tools of digital image processing it becomes possible to identify the particle distri-
bution inside the material on a single particle basis. Therefore, a three-dimensional digital image stack of a
magnetorheological elastomer is binarized and the particles are divided by Euclidian distance transformation
followed by a watershed algorithm. At the end, one obtains a matrix containing the single particles, as shown
in Fig. 7, which leads to a database containing all particles in the sample, including geometrical properties and
position within the elastomer.
Recent investigations have shown that the combination of X-ray microtomography with digital image
processing allows a detailed investigation of the microstructure of magnetorheological elastomers and its
dependence on the sample composition, the curing parameters and external stimuli. As an example, Fig. 8
shows the change of the inner structure of magnetorheological elastomers cured in the presence of a magnetic
field as function of the magnetic field strengths applied during the curing process [35]. As can be seen,
decreasing field strength leads to thinner particle chains and a higher chain density. A final break-up of the
chain structure can only be observed for magnetic field strengths as low as 1kA/m. This can be understood for
particles of comparably large size of about 35 m by the fact that their dipole-dipole interaction given by

0 e 2 aH2 p e
= ; =
2kB T p + 2e

where 0 = 4 107 is the vacuum permeability, p = 5000 denotes the relative permeability of the iron
particles, e the relative permeability of the elastomer, considered to be 1, the magnetic contrast factor, a
the average radius of the iron particles, H the magnetic field strength, kB the Boltzmann constant and T the
absolute temperature, is in the order of 105 even for such low magnetic field strengths.
The fact that no chains are formed at lower field strengths, where the dipoledipole interaction is still
sufficiently high, is a temporal phenomenon since the particles have to move through the matrix to form the
chains. Due to the fact that the polymeric matrix cures during this structure formation process, a minimum
velocity of movement of the particles is needed to obtain an ordered microstructure during the curing process.
Microstructure and rheology of magnetic hybrid materials

Fig. 7 X-ray microtomographic image of magnetic particles in an elastomer cured under influence of a magnetic field. The
particles have been separated and labelled by digital image processing

Fig. 8 X-ray tomographic data for anisotropic magnetorheological elastomers cured under different magnetic field strength. It
is clearly seen that a decrease in magnetic field strength applied during curing leads to thinner chains formed by the magnetic
particles [35]

But aside the general structural characterization of magnetorheological elastomers, X-ray microtomography
provides in addition the possibility to observe changes of the microstructure due to external stimuli on singular
particle basis. Figure 9 shows as an example the motion of particles which were originally homogeneously
 S. Odenbach

Fig. 9 Two combined X-ray microtomographic data sets. The particles marked in red were found in the original sample at H =
0 kA/m, while the green ones represent the same particles after application of magnetic field of H = 270 kA/m. By means of
digital image processing, the particles could be identified and thus the motion of each particle due to the action of the magnetic
field could be observed (indicated by the arrows). It is clearly seen that the particle motion leads to formation of chains in the
elastomer [36]

distributed in the matrix forced by the action of magnetic fields [36]. To obtain these images, an isotropic
magnetorheological elastomer with particles with a mean diameter of 55 m and a concentration of particles
of 5 m% that has been cured at zero field, has first been analysed by X-ray microtomography.
Afterwards a magnetic field of 270 mT has been applied, and after by a relaxation time of 4 hours again
a microtomographic image has been taken. Using a reference provided by a copper wire inside the sample,
those tomographic images could be registered and the particles in both tomograms could be identified. In this
way, it becomes possible to see the motion of each single particle under the action of external stimulia tool
which opens dramatic new possibilities for a detailed microstructural understanding of magnetorheological
elastomers. Recent investigations have already shown that microtomographic data can serve as an excellent
basis for theoretical investigations [37,38], and in future it is planned to use the obtained information about
changes in the microstructure as a benchmark for theoretical predictions.

4 Conclusion and outlook

As shown before, magnetic hybrid materials containing nano- or micron-sized magnetic particles can signifi-
cantly be influenced concerning their mechanical properties by the application of magnetic fields. The reason
for the changes in viscosity for liquid media or E-modulus for solid magnetic hybrid materials is given by
structure formation of the magnetic particles inside the hybrid material.
As discussed, the magnetic dipoledipole interaction is a core parameter for the structure formation.
Experimental analysis of changes in the microstructure can either be obtained by scattering experiments for
nanoparticles or in a three-dimensional way using X-ray microtomography. The resulting structural information
can serve as input data for a theoretical description of the field-induced changes or as a benchmark for
predictions made by theory.
It is obvious that changes of the E-modulus of magnetorheological elastomers, as well as viscosity changes
in magnetorheological fluids, are strong enough to be used in technical applications.
In contrast it has been mentioned that the magnetoviscous effects in ferrofluids have been assumed for long
time to be of academic interest only. Nonetheless, the development of new applications, where ferrofluids are
diluted in non-Newtonian liquids, has shown in recent past that even the magnetoviscous effect in ferrofluids
Microstructure and rheology of magnetic hybrid materials

Fig. 10 The magnetoviscous effect in biocompatible ferrofluid [42]

can be of severe importance for the design and realization of such applications. Thus, as an outlook, we will
shortly discuss changes of viscosity of non-Newtonian fluids doped with magnetic nanoparticles.
The starting point for the respective investigations has been the development of biomedical applications
of ferrofluids. In these applications, the magnetic particles are used as a drug carrier, especially in cancer
treatment.
Using tailored magnetic fields, the particles injected into an artery supplying, for example a tumour, can
be directed towards and captured inside the tumour region. Having a chemotherapeutic agent as drug attached
to the particles, one can generate a targeted chemotherapy with significantly reduced side effects [13,14].
Model experiments [39,40] and numerical calculations [41] have shown that the targeting efficiency
depends significantly on the viscous behaviour of the carrier fluid. As it is well known, blood is a strongly
shear thinning medium and it has to be asked how the viscous behaviour of blood combined with magnetic
nanoparticles will change in the presence of the magnetic fields, used to target the particles towards the tumour
region.
Obviously the amount of particles injected into the artery is extremely small. Nonetheless, the experiments
with ferrofluids have shown that even a small amount of sufficiently large magnetic particles will lead to
reasonable magnetoviscous effects.
In ferrofluids used for biomedical experiments, the particles are usually clustered into aggregates with a
mean hydrodynamic diameter of about 100 nanometre. Thus, the injection of a biocompatible ferrofluid into an
artery will lead to a low concentration of the sufficiently large magnetic particles, which can probably interact
in the presence of a magnetic field and thus lead to magnetoviscous effects changing the flow behaviour of the
blood in the artery.
In a first set of experiments [42], we have checked the magnetoviscous effect in a pure biocompatible
ferrofluid. As shown in Fig. 10, the effects are tremendously high, even at low magnetic field strengths and
sufficiently high shear rates. Diluting these fluids with water leads to reduction in the magnetoviscous effect,
which nonetheless will stay at about 100 % for a dilution by a factor 5 and shear rate of about 10 s1 .
Undertaking the same experiment with a dilution in blood, one finds magnetoviscous effects which are
significantly higher than for the same fluid diluted with water [43]. Viscosity changes in the order of several
100 % will in any way affect the application itself and thus have to be taken into accountfor the design of
the magnets used for magnetic drug targeting, as well as for the design of the application procedure.
With the models discussed before, this enhancement of the magnetoviscous effect due to the presence of
a non-Newtonian carrier liquid cannot be directly understood. A much more complex interaction between
blood cells and structures formed by the magnetic particles seems to take place in this situation. A first hint
concerning the microscopic reasons for the enhanced magnetoviscous effects can probably be the observation
that similar effects take place in liquid crystal suspensions doped with magnetic nanoparticles.
 S. Odenbach

For such combinations, first theoretical investigations are available, showing that conformational changes in
the liquid crystals, forced by the presence of chains of magnetic particles, could be the reason for the enhanced
magnetoviscous effects. At this end, the use of liquid crystal suspensions provides an excellent model system
to understand the effects found in blood doped with magnetic nanoparticles. Changing the size of liquid crystal
micelles will open the possibility to influence the structure of the liquid crystal independently from the properties
of the magnetic fluid. Nonetheless, numerous questions concerning the microscopic reasons of enhanced
magnetoviscous effects in magnetic hybrid materials, consisting of non-Newtonian carrier with magnetic
nanoparticles, are obviously open and will be a challenging field for future theoretical and experimental
research.

Acknowledgments The financial support by Deutsche Forschungsgemeinschaft within numerous projects and in the frame of
the priority programs SPP1104 and SPP1681, which made this research possible, is gratefully acknowledged. Particular gratitude
goes to Dr. D. Borin for helpful discussions and active support in the preparation of the manuscript.

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