14 PRB bump
14 PRB bump
Reversal mechanism, switching field distribution, and dipolar frustrations in Co/Pt bit pattern
media based on auto-assembled anodic alumina hexagonal nanobump arrays
T. Hauet,1 L. Piraux,2 S. K. Srivastava,2,3 V. A. Antohe,2 D. Lacour,1 M. Hehn,1 F. Montaigne,1 J. Schwenk,4 M. A. Marioni,4
H. J. Hug,4,5 O. Hovorka,6 A. Berger,7 S. Mangin,1 and F. Abreu Araujo2
1
Institut Jean Lamour, Université de Lorraine & CNRS, Vandoeuvre lès Nancy, F-54506, France
2
Institute of Condensed Matter and Nanosciences, Université catholique de Louvain, Place Croix du Sud, B-1348, Louvain-la-Neuve, Belgium
3
Amity Institute of Nanotechnology, Amity University, Noida, India-201303
4
Empa, Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf, Switzerland
5
Institute of Physics, Universität Basel, CH-4056 Basel, Switzerland
6
Faculty of Engineering and the Environment, University of Southampton, Southampton, SO17 1BJ, UK
7
CIC nanoGUNE Consolider, Tolosa Hiribidea 76, E-20018 Donostia-San Sebastián, Spain
(Received 23 January 2014; revised manuscript received 1 April 2014; published 19 May 2014)
We fabricated a perpendicularly magnetized bit pattern media using a hexagonally close-packed auto-assembled
anodic alumina template with 100 nm and 50 nm periods by depositing a Co/Pt multilayer to form an ordered
array of ferromagnetic nanodots, so-called nanobumps. We used Hall resistance measurements and magnetic
force microscopy to characterize the dot-by-dot magnetization reversal mechanism under applied field. The role
of interdot exchange coupling and dipolar coupling are investigated. Then we focus on separating the various
origins of switching field distribution (SFD) in this system, namely dipolar interactions, intrinsic anisotropy
distribution, and template packing faults. Finally we discuss the influence of triangular dipolar frustrations on
the energy stability of demagnetized and half-switched states based on an Ising model, including local exchange
coupling. The impact of SFD and lattice defects lines between misoriented ordered domains on the magnetic
configurations is studied in detail.
the effect of dipolar coupling in between the bumps. Then, array of magnetic caps and magnetization pointing up or
using magnetic force microscopy (MFM), we demonstrate the down perpendicular to the substrate surface [12]. We estimated
bump-by-bump magnetization reversal and hereby reveal the the mean interbump distance of 105 nm and a full width at
competition between interdot exchange and dipolar couplings. half-maximum of 15.5 nm, as described in Ref. [12]. Height
Easy and hard switchers are detected, and their influence on modulation profiles extracted from atomic force microscopy
magnetic states during field cycles or after demagnetization (AFM) images show a maximum bump to bump height
is discussed. Finally, we investigated features of AAO lattice variation of 5 nm (only 1 nm maximum in region with no
stacking faults and their consequences on nanobump arrays in lattice defects) and an average bump height distribution of
conjunction with their dipolar interactions and SFDs. about 2 nm over a few microns, but larger variations (up to
50 nm) can be observed from region to region for areas of tens
of microns.
II. EXPERIMENTAL DETAILS
A. Sample fabrication and structural features
B. Magnetic characterization methods
To obtain ordered arrays of ferromagnetic nanodots, we
deposited thin Co/Pt multilayers onto the bumpy barrier- The extraordinary Hall resistivity measurements were
layer surface of AAO templates [12]. The AAO templates performed by a standard four-probe method. The Hall effect in
were fabricated by a two-step anodization process in order magnetic materials is commonly described by the phenomeno-
to obtain highly ordered structures [13,14]. The templates logical equation, ρH = Ro H + Rs Mz , where ρH is the Hall re-
with 50 nm and 100 nm average pore spacing consist of sistivity, Ro is the ordinary Hall coefficient, Rs is the extraordi-
long channels (50 μm) closed at the bottom end by a nary Hall coefficient, and Mz the component of magnetization
round-shaped Al2 O3 barrier layer [Fig. 1(b)]. The barrier- perpendicular to the four contacts plane (here perpendicular
layer surface self-organizes in a hexagonal close-packed to the film plane). As in our experiment the ordinary part is
lattice of nanobumps that possesses the same spacing as much smaller than the extraordinary part, and the extraordinary
the porous layer [Figs. 1(a) and 1(c)]. It is used as a Hall voltage serves as a direct measurement of magnetization
prepatterned substrate to modulate the thickness of thin component perpendicular to film plane. Indeed, the hysteresis
Co/Pt multilayers deposited on it. The multilayers consist loop observed in the ρH (H ) curve was well correlated with
of a Ta(5 nm)/Pt(5 nm)/[Co(0.4 nm)/Pt(0.7 nm)]4 /Pt(3.5 nm) the magnetization curve obtained in the same condition of field
sequence grown by magnetron sputtering. Due to the bumpy and temperature using a commercial SQUID-VSM.
surface, the deposited film experiences a variable thickness Two types of MFM setups have been used for the experi-
along the surface, up to the total thickness of the magnetic ments described here. The first one is a nanoscope AFM/MFM
stack (10 nm) at the top and much thinner close to the that allows measuring topography and the remanent magnetic
bottom of the bumps [15]. In our previous work, it was shown configuration at room temperature. The second is a modified
that the magnetic coating of the bumpy surface maintains an nanoscan high-resolution hr-MFM, operated in a vacuum in
out-of-plane magnetic anisotropy, thus forming an ordered dynamic mode, whereby the cantilever resonance frequency
shifts arising from the tip/sample interaction are recorded and
which allows image magnetic configurations in an applied
magnetic field. We used a Team-Nanotech hr-MFM-ML1 tip,
keeping a tip-sample distance of approximately 8 ± 1 nm on
average. Fields were applied using the calibrated permanent
magnet driven by the perpendicular field option of the
instrument. Prior to the measurements, the tip was separately
magnetized in the direction and sense of the field applied
during the ramp of field. For each applied field, a stable scan
condition was established for the desired tip-sample distance,
and the scan was subsequently carried out. In scan series where
the sequence of applied magnetic fields included a change of
sign, we removed the sample from the field area at zero applied
field, flipped the tip magnetization, repositioned the sample,
and continued the field sequence. Thus we avoided tip magne-
tization flip events during the sample magnetization reversal.
The tip is scanned at constant average height corrected for
large scale topographical variations of the sample but not for
the local topography variations from single bumps. The MFM
contrast then arises from changes of the local magnetic stray
field, i.e., it reflects the local magnetic state of the sample
but also includes contributions of the van der Waals force,
which varies with topography-induced changes of the local tip-
FIG. 1. SEM images of nanobump arrays of a 100 nm period sample distance. The latter becomes apparent [Fig. 7(a)] in the
[(a) top and (b) tilted views, respectively] and a 50 nm period data recorded at positive saturation (+350 mT). The black dots
[(c) top view]. visible on a gray background reflect the center positions of the
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bumps, i.e., a more attractive van der Waals force arising from
the smaller tip-sample distance. In order to remove as much
as possible of this nonmagnetic contribution to the measured
MFM contrast and to focus on the magnetic signal, we use the
following procedure. First, we align all images, then we crop
them to the area that they all have in common. Subsequently,
we subtract from them the image obtained in saturation, which
contains essentially the same topographical information as all
other images. Finally we center and scale the contrast to ±1
except in the saturated images.
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FIG. 7. (Color online) 1 μm × 1 μm MFM images obtained successively after saturation at +350 mT (a), under 0 mT to −300 mT (b)–(o).
Since the magnetization is saturated at −350 mT, (a) corresponds to an average topography signal that is used to correct all the other MFM
images. Yellow hexagons in (a) mark lattice stacking faults.
M) form by first inverting the plots, i.e., plotting field H MFM figures using the procedure described in Sec. II B. The
vs M/Ms and then subtracting the field values along a recoil yellow spots in Fig. 7(a) indicate AAO lattice defect positions.
curve from the field values along the adjacent (decreasing) Figures 7(b)–7(o) show MFM images of the same nanobump
hysteresis loop branch (note the equivalence M ≈ VEHE due array region taken under applied fields (i.e., not at remanence)
to the normalization, from which follows M= 1−η/100%). from +350 mT to −350 mT. Figure 7(b) shows data obtained
The results of the transformation are the H (M, M) data at 0 mT. Fifteen from a total of 131 bumps visible in the
shown in Fig. 6(b) as open circles. Next, the data are fitted image have switched because of their low intrinsic reversal
by the set of reference functions of the generalized H (M, field combined with the dipolar field from the neighboring
M) method for variable exchange and dipolar interactions bumps. Some images show also that the stray field coming from
assuming a lognormal intrinsic SFD. The best-fit reference the MFM tip influences the bumps magnetization reversal.
function gives the statistically most reliable estimate of the The measurements were carried out with a commercial tip,
intrinsic SFD. As shown in Fig. 6(b), the fit is of very good maintaining a tip-sample distance of approximately 8 ±
quality with R 2 = 0.9689, yielding the standard deviation of 1 nm on average. At this distance, the maximum stray fields
the intrinsic SFD equal to σintrinsic = 14 .1mT. So the H (M, observed for this class of CoCrPt tips is typically of the order
M) method demonstrates that the intrinsic SFD is only of 5 mT, which adds to the external applied field. As the field
about one-third of the overall SFD (37 mT) extracted from amplitude increases from 0 mT towards negative values, more
EHE loop derivative (Fig. 4). The large dipolar effect deduced and more black spots occur until all dots have been reversed
from the comparison between the macroscopic SFD and the [see Figs. 7(c)–7(o)]. From the MFM images, we can calculate
H method sigma is fully consistent with the large shift the normalized magnetization as the number of white bumps
highlighted in Fig. 5. minus the number of black bumps divided by the total number
of bumps. The calculated values are plotted as a function of
applied magnetic field in Fig. 8.
B. Bump-by-bump reversal mechanism imaged by MFM The calculated MFM reversal branch is slightly different
An improved understanding of the roles of the intrinsic from the EHE one. Especially, the two reversal steps are much
SFD and the dipolar interactions for the magnetization reversal more visible in the MFM data, and the separation between
mechanism of Co/Pt nanobump arrays is obtained from the two peaks of the reversal branch derivative is much more
a field-dependent MFM study. Figure 7 shows the results pronounced than in the EHE data. Half reversal is reached
obtained for increasing negative fields after saturation in at about 80 mT, which is close to the coercive field value
positive fields, and Fig. 7(a) shows the positive saturation measured by EHE. Nevertheless, the reversal starts slightly
image (+350 mT). Black dots visible on a gray background before zero field (−20 mT for the EHE measurement) and ends
reflect the center positions of the bumps due to van der at around −300 mT (−170 mT for the EHE measurement).
Waals forces arising from the smaller tip-sample distance. All these differences must originate from a slightly larger
This nonmagnetic contribution has been reduced in the other thickness of Co in the sample measured by MFM. Indeed at
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notation]:
Cr1 = max(abs([d1 ,d2 ,d3 ]))/mean([a,b,c])
where
d1 = a − b, d2 = a − c, d3 = b − c,
Cr2 = 1 − min([a,b,c])/ max([a,b,c]),
Cr3 = max (abs(π/3[α,β,γ ]))/(π/3).
An additional criterion over the surface is used to avoid the
appearance of aberrant triangles, meaning triangles satisfying
the three criteria above but having a surface much larger than
the mean triangle surface. Triangles are accepted when their
surface differs from the mean surface by less than two times the FIG. 14. (Color online) Postprocessing results after triangles
standard deviation, i.e., S [S − 2σ S,S +2σ S]. Introducing base angle (α) analysis giving rise to three main base angle
the tolerance τ the final selection conditions become orientations according to the number of occurrences distribution of
the α angle. The three different base angle orientations correspond to
(Cr1 < τ ) ∩ (Cr2 < τ ) ∩ (Cr3 < τ ) ∩ (S ∈ [S − 2σS ,S + 2σS ]). different magnetic domains delimited by the structural defects (black
Applying a tolerance of 30% (τ = 0.3) in the above filled circles). Domains with orange triangles correspond to α ranging
equation, one obtains 71.6% (587/820) of triangles satisfying from −30° to −17.5°, from 25° to 30°, the ones with blue triangles
correspond to α ranging from −17.5° to 6.5°, and the ones with green
the criteria [see Fig. 13(a)]. Computing the statistics over the
triangles correspond to α ranging from 6.5° to 25°. (b) Number of
occurrences of a given base angle α ranging from −30° to 30° (α =
60°). In the inset, triangle base angle α definition showing the six
equivalent triangles (due to hexagonal symmetry) for a given α base
orientation relative to the x axis. The angle range for the triangle base
is then limited to 60° (360°/6) due to symmetry.
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shows the number of occurrences of a given α base angle in fields. One has to consider an additional interbump exchange
the range −30° to 30° (α = 60°). From the latter result coupling [31]. Nevertheless, such a double peak structure
three main base angle orientations are distinguished using requires 20 repeats of the same Co(0.4 nm)/Pt(0.7 nm) bilayer
three colors: orange for α [−30° −17.5°] [25°, 30°], as a thin film [30], whereas our bump array is only covered
blue for α [−17.5° 6.5°], and green for α [6.5° 25°]. with four repeats of Co(0.4 nm)/Pt(0.7 nm). Therefore, we
Then, using the same color code to fill in the corresponding can conclude that the exchange coupling is strongly reduced
triangles, one obtains a few colored regions on the AFM image in our bumpy system as compared to a continuous film.
[Fig. 14(a)]. At this point we can distinguish different “hyper Intermixing between the bumps is the most probable origin
grains” (ordered regions of different colors) defined by their of this partial exchange decoupling, as explained in Ref. [15].
respective orientation (α). The morphology of our surface High-resolution MFM allowed imaging the magnetization
thus mimics the surface of (111) textured body-centered-cubic reversal over hundreds of bumps during sweeps of an external
(bcc) polycrystals. The MFM demagnetized state pattern is magnetic field of uniform value over the whole imaged
then superimposed on the colorized AFM image on Fig. 14(a). area. Bump-by-bump individual magnetization switching is
From the MFM-AFM image comparison, it is clear that the demonstrated. After the first switching events, competition
magnetic lines are oriented along the α angle (modulo 2π /3) between exchange coupling and dipolar interaction is found
characterizing the hyper grain which they belong to. Hyper to favor lines of switched bumps until 50% of the bumps have
grain boundaries formed by a line of unique defects seem not been switched. At this stage, a labyrinthine domain pattern is
to affect the magnetic stripe too much. When passing through observed that has a low field susceptibility, i.e., it is more stable
a single defect boundary, the magnetic stripe just deviates to than the previous and subsequent configuration. This loss of
a new direction. The interbump exchange coupling may help magnetic susceptibility at 50% reversal leads to the double
to stabilize the boundary crossing. Zones with packed defects peak feature of the macroscopic hysteresis loops. Using an out-
affect the magnetic configuration more due to a strong change of-plane demagnetization, we achieved a zero-magnetization
in the exchange coupling and dipolar field environment, as configuration consisting of successive black and white stripes
observed in both Figs. 9(b) and 14(a). The remaining question with only one bump width. This configuration is even more
is whether the magnetic Y-shaped domains and zigzag domain stable than the labyrinthine one. When considering each bump
shape located inside the hyper grains are due to the finite size magnetization as an Ising spin, the dipolar interactions in a
of the hyper domain [51], due to lattice stress [53], or due triangular lattice are sufficient to explain the stability of the
to another feature. More statistics on hyper domain size and stripe state. Nevertheless, this configuration stability is not
shape are required to conclude on this point. drastically affected by the nonvanishing interbump exchange
coupling as long as it remains less than a fourth of the dipolar
interactions amplitude.
Magnetometry and MFM measurements have been used to
IV. SUMMARY AND CONCLUSIONS
quantify the SFD, to locate easy and hard switchers, and to
In our recent paper [12], we presented a method to grow distinguish the different origins of SFD and their influence
a perpendicularly magnetized BPM system, i.e., an ordered on the magnetic configurations. The H (M, M) method
assembly of magnetic islands. It was achieved by depositing shows that the intrinsic SFD is only one-third of the total
a Co/Pt multilayer on top of the barrier layer of AAO SFD. We could not find any structural reason to explain
templates with a 100 nm period to form an ordered array easy and hard switchers’ locations, so we conclude that the
of ferromagnetic nanodots, so-called nanobumps. Our self- intrinsic SFD mostly comes from misorientated Co/Pt grains
assembly method would have a number of advantages over the inside the bumps [27,28]. The strong dipolar-induced SFD
lithographic-based methods, including low cost and extremely is due to the close packing of the AAO template and might
simple processing. The AAO nanotemplates would display be a showstopper for a BPM technology implementation. In
tunable geometrical parameters, mild preparation conditions, addition, AAO lattice stacking faults are found to form mostly
robustness, and resistance to high temperatures. In addition, boundaries between well-ordered bump arrays. Lines of single
the extremely small attainable interbump period constitutes defects seem not to drastically affect the magnetic features
substantial advantages. Indeed regular nanopore arrays in of the neighboring bumps, whereas larger defect density
AAO with ultrasmall pore diameter (even less than 10 nm) does.
and pore interdistance as small as 15 nm have already been Finally, magnetic features of our nanobump assembly are
demonstrated [54,55]. very similar to those observed in continuous PMA thin films.
In the present paper, we have studied in detail two magnetic Therefore, besides being interesting as support for a BPM
features of a [Co(0.4 nm)/Pt(0.7 nm)]4 multilayer deposited template, we think that the present AAO system could be
on top of 100 nm and 50 nm AAO nanotemplates. EHE and a model for getting a deeper understanding of the influence
SQUID-VSM reveal values of coercivity five times lower than of the different thin film parameters (exchange coupling,
the anisotropy field. The latter’s dependence on field angle and dipolar interaction, and, more importantly, intrinsic SFD or
as a function of temperature reveal an incoherent magnetiza- thermal fluctuations) on the reversal mechanisms in PMA films
tion reversal mechanism, most probably based on a nucleation- [30,38,43,44]. Two main advantages of the bump assembly
propagation process inside each bump, as usually observed in system would be the control of interbump exchange coupling
nano-objects of this size. Surprisingly, the derivative of the and the precise characterization of SFD, which is difficult in
hysteresis loops shows a double peak structure that cannot usually strongly coupled systems [43,56]. More generally, the
be explained by taking into account only interbump dipolar present nanobump array is also a rich parameter space for
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