Acta Materialia 52 (2004) 2847–2862

www.actamat-journals.com

Overview No. 138

Information storage materials: nanoscale characterisation by

three-dimensional atom probe analysis
a,*
D.J. Larson , A.K. Petford-Long b, Y.Q Ma b, A. Cerezo b

a
Seagate Technology LLC, Recording Heads, One Disc Drive, NRE304, Bloomington, MN 55435, USA
b
Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH, UK
Received 15 December 2003; received in revised form 11 March 2004; accepted 13 March 2004
Available online 22 April 2004

Abstract

The development of nanoscale magnetic materials for applications in information storage systems relies heavily on the ability to
engineer the properties of the layered structures from which such materials are fabricated. These properties are strongly dependent
on the nature of the interfaces between the individual nanoscale magnetic layers, so knowledge of the interface chemistry is crucial.
In this paper, we discuss the application of three-dimensional atom probe analysis to the characterisation of layered magnetic
materials, including details of specimen preparation techniques required for this type of analysis. Recent results are presented on the
characterisation of interfaces in Co/Cu or CoFe/Cu multilayers, which form part of the read sensor in magnetic recording heads, and
Co/Pd multilayers, which are being considered for use as perpendicular recording media.
Ó 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Atom probe; Layered structures; Magnetic thin films

1. Introduction microstructure (e.g. interfacial roughness, chemical

In recent years there has been increasing interest in
thin-film layered structures because of the novel prop-
erties that they exhibit. Multilayer film (MLF) structures
are formed by alternate deposition of two or more dif-
ferent elements or compounds, usually with layers that
are 1–5 nm in thickness. Of particular interest are layered
structures formed from one or more transition-metal
magnetic materials because they have applications in the
field of data recording. Examples include high density
longitudinal or perpendicular magnetic recording media,
and sensors based on the giant magnetoresistance
(GMR) phenomenon such as those used for read heads
[1,2]. For a recent review of modern magnetic materials
in data storage see [3].
Layered structures based on Co, Ni, Fe, Cu and
their alloys form sub-structures of devices such as the
spin-valve [4], which exhibit GMR [2]. Changes in
*
Corresponding author. Tel.: +1-952-402-7140; fax: +1-952-402-
7734.
E-mail address: david.j.larson@seagate.com (D.J. Larson).
intermixing, etc.) are believed to influence the magni-
tude of the GMR effect and there has been much
research devoted to the dependence of the GMR ratio
on the specific nature of the interfaces in layered
structures. However, inadequate structural character-
ization has led to contradictory results arising from
different research groups even for the same materials
system (see, for example, [5–7]). This arises in part
because of the difficulty in distinguishing between
chemical mixing and roughness for most of the tech-
niques used to characterise the films. Interface
‘‘roughness’’ may be defined as a spatial variation of
the interface dividing two layers and ‘‘intermixing’’ as
the chemical mixing of the elements that comprise the
two layers, at or near the interface. These two mi-
crostructural features are likely to have very different
effects on the properties, therefore establishing the
correlation between structure and properties requires
the ability to distinguish between roughness and
intermixing.
When characterising layered structures, the very
small layer thicknesses makes it extremely difficult to

1359-6454/$30.00 Ó 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2004.03.015
2848 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
determine the nature of each individual interface unless a
technique is used that allows independent interface
analysis with high spatial resolution. Low-angle X-ray
diffraction (X-ray reflectivity) has been widely used to
study layered thin film materials (see for example [8]).
However, the X-ray reflectivity profiles that are obtained
are summed data that include contributions from all the
interfaces in the structure. It can therefore prove ex-
tremely difficult to obtain a unique fit to the data for
multilayer films if the interfaces between different layers
do not contain the same degree of roughness and/or
interdiffusion through the multilayer stack. Neutron
reflectivity has also been applied to the study of inter-
faces in epitaxial superlattice structures and to poly-
crystalline sputtered films but this technique is not as
good at determining structural information as X-ray
reflectivity, and is therefore more usually applied using
polarised neutrons to determine magnetic structure (see
[9] for a recent review).
One of the most commonly used techniques that can
be used to analyse each interface independently is
transmission electron microscopy (TEM) of cross-sec-
tion samples, which can be used to study both the mi-
crostructure and compositional profile across the layers
[10]. However, a limitation of TEM is that it is a pro-
jection technique and integration through the specimen
thickness can make it difficult to distinguish interfacial
mixing and fine-scale roughness except under very spe-
cific conditions. An example is given by Hytch of sep-
arating these two effects in Co/Cu multilayer films using
detailed image analysis of through-focal series of Fresnel
fringe images [11].
The technique of three-dimensional atom probe
(3DAP) analysis [12–15] is unique in having the capa-
bility to characterise internal interfaces, grain bound-
aries and precipitates with sub-nanometre resolution in
all three dimensions. With this technique it is therefore
possible to measure the extent of interdiffusion or in-
terface segregation at the atomic scale, and separate
these effects from nanometre-scale topological features.
In a 3DAP, pulsed field evaporation is used to re-
move individual atoms from the surface of a specimen,
which is in the form of a needle with end radius
50 nm.
A position-sensitive detector is used for measurement of
both flight time (to identify atomic species) and impact
position (which enables the original position of each
atom on the specimen surface to be recorded). The po-
sition of an atom in the depth direction is calculated
from the sequence of ion detection. The 3DAP has a
depth resolution of a single atomic layer and sub-
nanometre lateral resolution. An intrinsic requirement
of the 3DAP microscopy technique is the production of
a very high electric field (20–50 V/nm) at the surface of
the specimen in order to achieve field evaporation. The
field is produced by applying a high voltage (typically

10 kV) to a needle-shaped specimen with an apex ra-
dius of curvature of 10–100 nm. For most materials,
these sharp needles can be produced by electrochemi-
cally polishing fine wires, whiskers or blanks cut from
bulk material [12–16]. However, preparing a specimen
from certain sample geometries can be quite compli-
cated. Examples include certain multi-phase alloys,
semiconductors, ceramics and, in particular, thin film
materials. Over the years, various methods have been
applied to 3DAP specimen preparation in order to
overcome these problems [13,14].
This paper gives an overview of the results of recent
3DAP studies, both from our group and from other
groups, of magnetic layered film structures (e.g. Ni/Cu,
Co/Cu, CoFe/Cu, Co/Pd, etc.), concentrating on mate-
rials with potential applications in information storage
systems. These materials science studies have been made
possible by recent progress in the application of high
resolution focused ion beam systems to the preparation
of 3DAP specimens from complex layered systems, and
this is also reviewed briefly.
2. Development of 3DAP specimens from thin film
samples
In order to investigate thin layered structures in the
atom probe, these features must be present in the apex
region of the specimen. The preparation of 3DAP
specimens from thin film structures is difficult, but is a
crucial step in obtaining 3DAP data that provide the
highest possible spatial resolution across the feature of
interest, in this case the interfaces in the layered struc-
ture. The specimen preparation process is difficult be-
cause the total sample thickness (region of interest
containing the thin layers) is often only of the order of
20–100 nm. There are three main methods that have
been used to prepare 3DAP specimens from thin film
structures and these are outlined below.
A number of papers have been produced detailing the
results of 3DAP studies carried out on thin film mate-
rials in which the films of interest were deposited directly
onto pre-evaporated needle-shaped specimens [17–30].
Fig. 1(a) shows a schematic of the geometry of a speci-
men that has been prepared in this way, but note that
the curvature of the tip relative to the layer thickness is
not necessarily to scale (the tip radius is of the order of
50 nm and the layer thickness is typically a few nano-
metres). The small volume from which the 3DAP data
are taken (of the order of 20 nm in diameter) means that
within the volume analysed the substrate approximates
to a flat surface, and the structure of the layers is often
assumed to be reasonably similar to that of the same
layers deposited on a planar substrate. However the
microstructure is unlikely to be exactly the same, in part
because the substrate material (in this case a metallic tip)
does not correspond well to the substrates used in ap-
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 1. (a) Schematic diagram of the method of thin film deposition
onto curved sample surface, (b) schematic diagram of the modified
lithographic specimen preparation method described by Hasegawa
et al. [31] and Larson et al. [47] and (c) schematic diagram of the
specimen geometry that results from silicon post method used by the
current authors [50].
plications (most commonly an amorphous underlayer
followed by an oriented seed layer). This fact, combined
with the curvature of the end of the tip, will mean that
the stress configuration in the film is likely to be different
from that in a ‘standard’ layered film. In addition, in
order to make a direct correlation of the structural and
composition results obtained by 3DAP with magnetic or
transport measurements, 3DAP analysis must be per-
formed on layered films deposited on flat substrates
because it is not possible to make standard magnetic and
transport measurements on the films deposited on tips.
2849
It is also often desirable to investigate the microstructure
of films that have been deposited in standard industrial
deposition systems, rather than in special deposition
chambers designed specifically to enable the study of
films deposited onto pre-evaporated needles, as has also
been pointed out by Lang and Schmitz [30]. In spite of
these detriments, this technique has been widely used
and does have certain advantages.
A preparation method that addresses some of the
above issues has been reported by Hasegawa et al. for
specimens containing a single layer alloy film [31]. In this
method the film to be analysed is deposited on a sub-
strate, such as a Si wafer, covered in photoresist. The
film is then lithographically patterned to form small
samples with a shape similar to that shown in Fig. 1(b).
Following patterning the photoresist is dissolved, leav-
ing the samples that are comprised of the layer(s) of
interest. An individual sample must then be picked up
and attached to the end of a sharpened metallic tip using
conducting epoxy. Final shaping of the post section of
the sample, which will form the specimen to be analysed,
is carried out using a pulsed micropolishing technique.
This method results in a specimen with the film(s) in its
plane and has been used to investigate Co- and Fe-based
magnetic films [32–34].
The Hasegawa technique does result in the fabrica-
tion of a specimen from a layered film deposited on a flat
substrate using a standard deposition system, but it
requires the film material(s) to be deposited onto a
non-standard seed layer and to be amenable to electro-
chemical polishing. Problems arise when the different
layers in the film require very different polishing solu-
tions, as is the case for Cu and Co, two commonly used
materials in information storage applications. In such
cases, another method of specimen sharpening, such as
ion beam milling, must be used.
In principle, specimen preparation using ion milling
[35–38] has several advantages over electrochemical
techniques [12,39]. These advantages include the elimi-
nation or reduction of contamination and the reduction
of preferential etching problems in multi-phase materi-
als such as layered films. The application of ion milling
to prepare 3DAP specimens from thin film(s) or near-
surface regions has not been widely investigated. Liddle
et al. [40], Larson et al. [41] and Kvist et al. [42] used a
broad ion beam to mill without the capability to image
the specimen during preparation. In-situ imaging and
ion milling of atom probe specimens using a gallium
liquid metal ion source was first reported by Waugh
et al. [43] using an instrument with a focused ion spot
size of
50 nm. Further work on ion milling of atom
probe specimens was performed by Alexander et al. [44]
using a Gatan model 645 precision ion mill with a
minimum spot size of approximately 1500 nm. Although
the above investigations show the feasibility of concur-
rent ion milling and secondary electron imaging, the full
2850 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862

capability of the new generation of commercial high on post size but are typically of the order of 3 lm
resolution (<10 nm) focused ion beam (FIB) systems for (outer radius) and 1 lm (inner radius). The centre of
fabricating 3DAP specimens has only recently been the post is protected by the annular milling pattern
explored. during this stage of the milling process (typically 1 to 2
A modified version of the technique developed by min) and the result is shown in Fig. 3(b). The inner
Hasegawa, described above, has been used to enable radius of the annulus is then decreased (typically to
3DAP analysis to be carried out on 400 nm thick Co/Cu
0.4 lm) and further milling is carried out until the
multilayer films [45,46] deposited on a layer of photo- radius of the unmilled region of the specimen ap-
resist on a Si substrate. The dimensions of the pro- proximately matches the inner radius of the annular
truding portion of the sample are approximately pattern, Fig. 3(c). Fig. 4(a) shows the specimen ge-
3.0  0.4  150 lm, see Fig. 1(b). The protuding post ometry from the side at this point during the process
section of the sample was shaped using focused ion (the arrow shows the region of interest). Fig. 3(d)
beam milling with 10 keV gallium ions, to form a suit- shows a specimen after a final milling stage carried out
able 3DAP specimen [47,48]. A similar method has with reduced radii of the annulus (typically to
1 lm
subsequently been used as well by Schleiwies [49] to and
0.1 lm for the outer and inner radii, respectively)
prepare NiFe/Cu thin film specimens. The disadvantages and a reduced beam current (typically 10–30 pA) to
of this process are (1) that the films are deposited on a minimise Ga beam-induced damage. Figs. 4(b) and (c)
non-standard underlayer (photoresist); (2) that in the show low and high magnification images of the final
case of a layered film, the interfaces between the layers specimen shape. The radius is less than 100 nm and the
are oriented parallel to the axis of the specimen (see region of interest for 3DAP analysis is positioned at or
Fig. 1(b)) so that the resolution across the interfaces is near the apex of the needle.
reduced by lateral trajectory aberrations [13]; and 3) the
requirement for mechanical stability of the element
means that the fabricated layers must have a total
thickness of the order of 0.5 lm. Once this thickness is
reached, the microstructure increases in correlated
roughness and the magnetic properties may not be the
same as those of a very thin layered film (<10 nm thick),
such as would be of interest from a technological point
of view.
A third specimen preparation method (used in the
majority of the recent work by the current authors) uses
high aspect ratio, flat-topped Si posts as the substrate
for the 3DAP specimens [50]. This specimen orientation
enables the highest spatial resolution to be obtained
across the interfaces during analysis (see Fig. 1(c)). In
order to ensure transmission of the voltage pulses re-
quired for 3DAP analysis, low resistivity Si wafers
(
0.01 X cm) are used. The wafers are patterned using
standard optical lithography followed by deep-trench
reactive ion etching (commonly referred to as the
‘‘Bosch’’ process [51]) to create posts having a very high
aspect ratio (up to
50 to 1) with an end size ranging
from
3  3 to
24  24 lm. Prior to metal deposition,
the native Si oxide on the surface is usually removed by
sputter etching in order to promote good adhesion of
the metal to the silicon. Single posts are removed from
the wafer and attached to a metallic needle using elec-
trically-conducting epoxy [52] as shown schematically in
Fig. 2(a). 3DAP specimens are then prepared from the
end of the post using 30 keV gallium ions with beam
currents of 30–1000 pA.
A brief overview of a typical specimen sharpening
Fig. 2. (a) Schematic diagram showing the use of electrically-con-
process [50] is shown in Figs. 2(b) (schematic), 3, and ducting epoxy to attach a silicon post to a metallic needle in prepa-
4. For the first milling step an annular milling pattern ration of focused ion beam milling, (b) schematic diagram of the
is used (shown in Fig. 3(a)) whose dimensions depend annular focused ion beam milling technique.
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862 2851

There are, of course, disadvantages associated with
ion milling methods. For example, milling may intro-
duce implantation and defects into the near-surface
region of the specimen but these can usually be re-
moved by field evaporation before atom probe analysis
proceeds. The FIB techniques described above lead to
a region of the specimen that has been partially dam-
aged by the Ga ion beam [48]. An example of the
problems associated with the use of a focused ion beam
for specimen fabrication using the modified Hasegawa
technique is shown in Fig. 5. No layers were visible in
the field ion image of a specimen containing a (Co2 nm /
Cu2 nm )100 multilayer film milled using the FIB at
10 keV [45]. Subsequent atom probe analysis showed
the gallium content vs analysis depth to range from

6.5 at.% Ga initially to
0.5% Ga at a depth of
15
nm, as seen in Fig. 5(a). For comparison, the results of
analysis of a specimen fabricated using 30 keV gallium
ions are also shown. The gallium implantation level
was still 10–20% even up to a depth of
20 nm into
the specimen. Fig. 5(b) shows atom maps of the Ga
and Cu taken from the 3DAP analysis of the specimen
milled at 10 kV and whose Ga content is shown in
Fig. 5(a). The layered structure appears after
20 nm
of field evaporation, as shown by 3DAP (note that
Fig. 5(b) does not include the first 10 nm of the profile
shown in Fig. 5(a)).
The FIB-damaged region can be removed and mon-
itored during 3DAP analysis. Alternatively, the dam-
aged region can be removed by DC field evaporation
while field ion imaging, or by low-energy ion sputtering
using field emission in the presence of Ne gas [53]. Note
that only analyses that are relatively free of Ga im-
plantation (less than
1–2% Ga) should be considered
as representative of the original thin film microstructure.
3. Studies of layered thin films
Over the last decade or so, the three-dimensional
atom probe technique has been applied to various lay-
ered systems of interest for information storage mate-
rials. These include Ni/Cu [21], Co/Cu [27,46], Ni/Al
[29], CoFe/Cu [54–56], NiFe/Cu [57], CoFe/NiFe [58],
Fe/Cr [59], Co/Pd [60], as well as various magnetic ma-
terial-based single film structures. The results of some of
these studies are discussed in more detail below.
3.1. Co/Cu and CoFe/Cu multilayer films
The modified Hasegawa technique was used by
the current authors to prepare specimens from an
Fe/(Cu2 nm /Co2 nm )100 multilayer film. An Fe seed layer
was used in these samples to impart a strong (1 1 1)

Fig. 3. Silicon post (a) prior to pattern placement at low ion current (inset at high ion current), (b) the evolution of the end of the post as milling
proceeds using the
1 lm inner radius pattern, (c) the post after milling has reduced the radius of the unmilled region of the specimen to
0.4 lm and
(d) the post after milling at low current has reduced the radius of the unmilled region of the specimen to less than
0.1 lm.
2852 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 4. (a) Side view of the specimen after the
0.4 lm inner radius
pattern stage of milling. The metal film(s) are visible as a bright region
on the end of the specimen. (b) Low and (c) high magnification images
of the final specimen shape. The radius is less than 100 nm and the
region of interest for 3DAP analysis is positioned at the apex of the
needle.
crystallographic texture to the MLF. The as-deposited
films showed a magnetoresistance ratio of
5% at room
temperature, and the magnetic data suggested that a
significant fraction of the films were coupled ferromag-
netically (contrary to the expectation of antiferromag-
netic coupling for this copper interlayer thickness). The
coercivity was
60 Oe, which is relatively high for films
of this type. A field-ion image of the multilayer,
Fig. 6(a), shows the brightly-imaging cobalt layers: in
some regions the layers are relatively straight and in
other regions the layers are non-parallel, with a ‘‘wavi-
Fig. 5. (a) Composition profile in Co/Cu multilayer film specimen
showing the degree of Ga incorporation caused by FIB milling. (b)
3DAP atom maps for Ga and for Co from final
20 nm depth of
specimen milled at 10 kV showing onset of appearance of the Co/Cu
layers following the Ga implantation damage. (Reproduced from [47]
with permission from Institute of Physics Publishing.)
ness’’ amplitude of
2 nm and period of
20 nm [45].
The specimen preparation method used in this work
results in layers that run parallel to the long axis of the
specimen and the layers are thus viewed in cross-section
in the field ion image. The waviness of the layers was
also evident in the 3DAP data obtained from the same
film, as seen in Figs. 6(b) (map of Cu atoms only) and
Fig. 6(c), which shows the Co composition profile. The
fact that the layers are wavy, as shown in Fig. 6, suggests
that the ferromagnetic coupling is a result of N
eel ‘‘or-
ange peel’’ type magnetostatic coupling between adja-
cent cobalt layers. In addition, in some areas adjacent
cobalt layers appear to be in contact, which will further
increase the ferromagnetic coupling. The relatively high
coercivity is expected to be a result of the poor layer
planarity, which leads to a high number of domain wall
pinning sites.
Co/Cu layered structures have also been studied by
3DAP using the method of film deposition onto a pre-
formed W needle [27]. In this work, a layered structure
of NiFe25 nm /Cu20 nm /Co10 nm was ion beam sputtered
onto a W needle and analysed in the as-deposited and
annealed (0.5 h at 350 °C) states. Schleiwies at al. [27]
observed an ‘‘interfacial solid solution zone’’ approxi-
mately 1.5 nm in width at the interfaces in these samples
(as-deposited), as well as segregation of Fe through the
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 6. (a) Field ion microscope image showing Co (bright) and Cu
(dark) layers, (b) 3DAP atom map of the Co/Cu multilayer showing
degree of curvature of the Co and Cu layers (Cu atoms only for clarity)
and (c) selected-region Co composition profile across the layers.
Cu layer to the Co/Cu interface after annealing,
although no physical mechanism for this effect was
proposed.
Fig. 7(a) shows atom maps of Ni, Co and Cu from a
3DAP dataset of a repeated (Ni–20Fe5 nm /Co–10Fe4 nm /
Cu3 nm /Co–10Fe4 nm ) multilayer film fabricated from a
sample deposited onto Si posts and prepared by the
annular FIB milling method as described above [50]. As
can be seen in the figure, for samples prepared in this
geometry, the interfaces run across the apex of the
specimen (normal to the axis) and thus the 3DAP
technique can achieve atomic resolution across the in-
terfaces, enabling accurate measurement of their
roughness and intermixing. This is clearly seen in
Fig. 7(b), which shows the (1 1 1) atomic planes across a
NiFe/CoFe bilayer, indicating the high degree of crys-
tallographic texture in the sample. In addition, micro-
2853
structural results from specimens prepared in this
geometry can be compared directly with devices grown
for magnetic and transport measurements.
Fig. 8(a) shows an atom map indicating the atomic
positions of the Co (blue), Fe (yellow) and Cu (red)
atoms in a CoFe/Cu/CoFe trilayer (a subsection of the
multilayer structure described in the previous para-
graph). The atom map shows qualitatively that there is
more intermixing at the CoFe-on-Cu interface than
there is at the Cu-on-CoFe interface, resulting in the
CoFe-on-Cu interface being wider than the Cu-on-CoFe
interface. However the strength of the 3DAP technique
lies in the fact that in addition to being able to show
such effects in a qualitative manner, the extent of the
interdiffusion can be measured quantitatively by taking
composition profiles through small sections of the data
perpendicular to the local interface plane. Fig. 8(b)
shows a composition profile across the same trilayer
region. The direction of growth is from left to right in
the profile. Measurement of the interface widths from
the composition profile (using 10–90% of the Cu con-
centration) gave values of 1.08 (0.18) nm for the CoFe-
on-Cu interface and 0.4 (0.14) nm for the Cu-on-CoFe
interface [61].
3.2. Comparison of 3DAP data with modelling
Molecular dynamics (MD) simulation of the growth
of the same materials system [61], Fig. 9, supports the
3DAP results presented above. As can be seen, the
match between the 3DAP data and the simulation is
extremely good, with the MD simulation giving a width
for the CoFe-on-Cu interface of
1.44 nm and for the
Cu-on-CoFe interface of
0.33 nm. Further 3DAP
quantitative analyses of this type gave values of 0.82
(0.10) and 0.47 (0.15) nm for the CoFe-on-Cu and
Cu-on-CoFe interfaces, respectively [54,58]. The differ-
ence in interface width is believed to be the result of the
lower surface free energy of Cu compared to that of Co
or Fe [62]. The molecular dynamics modelling suggests a
difference in the exchange probability during deposition
of Cu with Co and Fe at the two interfaces, with the
exchange probability at the CoFe-on-Cu interface being
higher, resulting in more mixing at the interface. Of
course, this will result from a combination of driving
forces (due to the lower surface energy for Cu) and the
lower activation barrier for exchange (due to the lower
melting temperature of Cu), and it is difficult to distin-
guish the two effects in the model. Note that the model
only takes into account rearrangements resulting from
atomic impacts, and does not cover the much longer
time scale over which thermally activated surface and
bulk diffusion may occur and contribute to intermixing.
However, since the agreement between model and ex-
periment is so good, such effects are not likely to con-
tribute greatly to the observed intermixing, at least at
2854 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 7. (a) 3DAP atom maps of Ni, Co and Cu atoms in the multilayer (volume is
20 nm 
20 nm 
35 nm), (b) selected-region composition
profile across two of the layers shown in (a).
the deposition rates (0.1 nm s1 ) and substrate tem-
peratures (300–330 K) used here. The good agreement
between the simulated and experimental data shows that
3DAP analysis is really the first type of experiment that
can be used to check this model at the correct length
scale. A favourable comparison between model and
experiment also served to validate the MD simulation
parameters used for these materials and has encouraged
both research groups to proceed with further compari-
sons, as described below.
The data in Figs. 8 and 9 show a layered film in which
the top surface of the CoFe layer is relatively flat.
However growth of multilayer films with a strong [1 1 1]
crystallographic texture often results in the top surface
of the layers being rough, or wavy, with a period of a
few nanometres. In many multilayer systems this peri-
odicity is transferred through to subsequently deposited
layers, resulting in correlated roughness that usually
becomes worse as more layers are deposited [8]. An
example of this is shown in Fig. 10. The roughness at the
top of the NiFe layer has been transferred up to the next
CoFe layer, as can be seen from the isoconcentration
surface (surface of constant concentration of one or
more elements) shown in Fig. 10(a), plotted at a com-
position of
45 at% Co. A very interesting feature is the
fact that the upper surface of the Cu layer is not con-
formal with the upper surface of the underlying CoFe –
the deposition of the Cu has acted to smooth out the
correlated roughness [54]. This smoothing effect had
been suggested by Eckl et al. [7] on the basis of in-situ
resistivity measurements but was not confirmed by a
microstructural study.
The question then arises as to how the Cu grows in
order to smooth out the roughness. Eckl et al. pro-
posed that the initial Cu layer was deposited confor-
mally on the underlying Co, followed by nucleation of
islands of Cu in the troughs at the grain boundaries.
While the 3DAP data in Fig. 10 show the Cu
smoothing effect, the actual growth process cannot be
understood just from the 3DAP data as the technique
does not allow us to follow the process as a function
of time. However, this can be achieved using the same
MD simulation technique as discussed above [61].
Fig. 11 shows a series of images obtained during a
MD simulation of the growth of a Cu layer on a
rough CoFe layer [63]. Fig. 11(a) shows that the initial
monolayers of Cu are indeed deposited conformally
on the CoFe surface, as proposed by Eckl et al. The
MD simulations indicate that as the Cu layer gets
thicker, facets with (1 1 1) crystallographic planes
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862 2855

Fig. 10. (a) Isoconcentration surface at
45% Co for a NiFe/CoFe/Cu/

Fig. 8. (a) 3DAP atom map of Co (blue), Fe (yellow) and Cu (red) CoFe multilayer, and (b) and (c) 3DAP atom maps of Co (blue), Fe
atoms in a CoFe/Cu/CoFe trilayer and (b) a composition profile across (yellow) and Cu (red) atoms in the same region. (b) Shows the first few
the same region (growth direction is left to right in the profile). (Re- atoms of the Cu layer and (c) shows the structure up to the point at
produced from [61] with permission from Elsevier Publishing.) which deposition of the Cu ends.

Fig. 9. (a) Molecular dynamics simulation showing an atom map of Co

(blue), Fe (yellow) and Cu (red) atoms in a a CoFe/Cu/CoFe trilayer Fig. 11. Molecular dynamics simulation [63] of the growth of a thin Cu
and (b) a composition profile across the same region (MD-simulated layer onto a rough CoFe layer. (a) The first few monolayers of Cu
growth direction is left to right in the profile). (Reproduced from [61] grown conformally on the CoFe and (b) and (c) further Cu growth
with permission from Elsevier Publishing.) results in a smooth film surface.
2856 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862

begin to form at the peaks and troughs of the un-

dulations. The (1 1 1) surfaces are low-energy surfaces
and to maximise their area, Cu atoms lying on the
sides of the troughs diffuse across the growing surface
and fill in the troughs as seen in Figs. 11(b) and (c).
The final result is that the upper surface of the Cu
layer is much flatter than the CoFe surface on which
it grew. Both this MD simulation and the 3DAP data
(Fig. 10(b)) show that deposition of Cu onto a rough
CoFe layer results in relatively little intermixing with
the CoFe. When the next CoFe layer is deposited, the
enhanced interdiffusion at the CoFe-on-Cu interface
serves to remove any remaining correlated roughness
at the upper surface of the Cu layer, as shown in
Fig. 10(c). The combination of the 3DAP data and
the MD simulation can thus be used to provide a full Fig. 12. Field ion image of four repeats of the CoFe/Cu bilayer
picture of the way in which the growth of the Cu showing the expected [1 1 1] crystallographic texture.
layer smoothes out the CoFe roughness and at the
same time yields an intermixed upper Cu surface.
7
3.3. Effect of oxygen during growth on thin film micro- O-doped as-
structure 6 grown
O-doped,
5 annealed
One factor that can significantly affect the GMR No-O, as-
dR/R (%)

properties of thin films structures is the presence of 4 grown

impurities, such as oxygen, in the sputtering chamber
during deposition. Different proposals have been put
forward to explain this effect, such as a smoothing of
the interfaces during growth via a reduction of surface
free energy [64], a reduction in pinhole density across
the Cu spacer layers [65] and a reduction in grain size
and interface roughness caused by partial oxidation of
the interfaces [66]. However, to date, relatively little
nanoscale characterisation has been carried out to
support these suggestions. There are therefore several
issues to be clarified with respect to oxygen-doped
multilayer growth such as the amount and position
of residual oxygen trapped in the layered structures
and the exact effects of oxygen on the nature of the
interfaces.
The 3DAP has been used to investigate the thin
film microstructure resulting from the addition of an
oxygen surfactant during growth of the Cu layers in
{Si//Ni alloy5 nm /Co–10Fe3 nm /(Cu1:8 nm /Co–10Fe3 nm )5 /
cap50 nm } films [55]. In this structure, the Ni-based seed
layer leads to a h1 1 1i crystallographic orientation in
the films, and this can be seen in the field ion image of
the multilayer in Fig. 12 which shows strong crystal-
lographic orientation along the specimen axis, together
with with the bright (CoFe) and dark (Cu) contrast
regions which indicate the layers in the structure. The
sputter gas pressure during deposition of the Cu and
CoFe layers was of the order of several mTorr, and
deposition of the Cu layers was carried out either in Ar
or in an Ar + oxygen gas mixture with the total pres-
sure being kept constant.
No-O,
annealed
3
2
1
0
-1500 -1000 -500 0 500 1000 1500
H (Oe)
Fig. 13. GMR curves for as-deposited and annealed CoFe/Cu multi-
layer films for which the Cu layers were deposited either in Ar or in
Ar + oxygen.
Magnetoresistance values measured on films depos-
ited on unpatterned samples (using a standard four-
point probe measurement) were found to be
1% and

7% for the Ar and Ar + oxygen Cu deposition condi-
tions, respectively, as shown in Fig. 13. Fig. 14 shows
composition profiles across the CoFe/Cu layers for de-
positions (a) without and (b) with oxygen present for
deposition of the Cu layers [55]. The most obvious dif-
ference is the degree of intermixing in the Cu layers,
which is considerably reduced for the Ar + oxygen de-
position, resulting in a higher Cu content at the centre of
the layers. As expected from the surface free energy
argument discussed above, the CoFe-on-Cu interface
shows more intermixing than the Cu-on-CoFe interface,
and the effect of the oxygen has been to reduce the width
of both interfaces (see Table 1). See [55] for further de-
tails of the interfacial width measurements in these
structures.
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 14. Composition profiles across CoFe/Cu multilayers for deposi-
tions of the Cu layers in (a) Ar and (b) Ar + oxygen. The growth di-
rection is from right to left in both profiles. (Reproduced from [55]
with permission from The American Physical Society.)
As can be seen from Table 1, the Ar + oxygen depo-
sition has resulted in a decrease in the width of the
CoFe-on-Cu interface by a factor of approximately two
relative to the deposition without oxygen. This clearly
shows that the presence of oxygen suppresses mixing
during growth. Egelhoff et al. [67] have suggested that
this occurs because the oxygen favours the formation of
Co–O (or Fe–O) bonds rather than Cu–O bonds (the
heats of formation of the oxides are: CoO ¼ )58 kcal/
mol and CuO ¼ )38 kcal/mol [68]). The lowest energy
state thus has Co at the surface rather than Cu, leading
to less interfacial mixing. This argument would tend to
suggest that the width of the Cu-on-CoFe interface
might increase in the presence of oxygen. However the
higher cohesive energy of Co compared to that of Cu
may restrict the atomic exchange [61] at the Cu-on-CoFe
interface, so that no increase in intermixing is observed.
Table 1
Interface widths for CoFe/Cu MLFs for which the Cu layers were deposited either in Ar or in an Ar + oxygen mixture, for the as-deposited films and
for films annealed at 300 °C for 30 min
Cu deposition condition Interface widths (nm)
CoFe-on-Cu
Ar – as-grown 1.21 (0.05)
Ar + O2 as-grown 0.55 (0.03)
Ar (300 °C/0.5 h) 1.16 (0.09)
Ar + O2 (300 °C/0.5 h) 3.01 (0.12)
2857
Indeed the intermixing is found to be reduced slightly,
which suggests that the presence of oxygen on the
growing surface reduces the number of atomic ex-
changes at the surface. This will also contribute to
the reduction in interface width at the CoFe-on-Cu
interface.
Another interesting observation is that there is an
increase of only approximately a factor of 2 in the re-
sidual oxygen level (average of
260 appm oxygen for
the no-oxygen condition compared to an average of

530 appm oxygen) for the Ar + oxygen condition [55].
The oxygen present in the films grown without added
oxygen is most likely a result of the dissociation of water
vapour in the deposition chamber and of oxygen in-
corporated into the sputter deposition targets. The rea-
son that the incorporated oxygen content increases only
by a factor of two, despite a large difference in the ox-
ygen pressure in the chamber, may be the very low
solubility of O in Cu and Co [69]. Further evidence for
the low incorporation of oxygen for the Ar + oxygen
deposition can be seen in the elemental map shown in
Fig. 15. The oxygen atoms are not positioned prefer-
entially at the layer interfaces but are distributed rela-
tively randomly through the layers, and there is no
evidence for the formation of an oxide phase in these
samples, as has been suggested in the literature [66].
However, there is some evidence for preferential reten-
tion of oxygen near grain boundaries, as previously
suggested [64].
A further effect of the presence of oxygen during
sputtering is a decrease in the conformal roughness of
the layers, as observed previously by Miura et al. [66],
which would also be expected to increase the GMR
ratio. An estimate of the conformal interfacial rough-
ness was made from TEM cross-section images by
measuring the maximum peak-to-peak amplitude of the
spatial variations in each layer. The mean amplitude
values (averaged across all five bilayers) are 1.89 (0.08)
nm and 1.62 (0.08) nm for the Ar and Ar + oxygen
deposition conditions, respectively [55]. The presence of
oxygen is believed to reduce long-range surface diffusion
[70] and thus decrease grain boundary grooving – this
would drive the system away from equilibrium and thus
lead to decreased grooving, as observed in the TEM
data.
Ave. Cumax Conc. (%)
Cu-on-CoFe
0.49 (0.03) 65.1  13.3
0.31 (0.02) 77.1  11.72
0.61 (0.02) 72.1  7.6
2.38 (0.12) 55.6  7.4
2858 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862

%Co %Cu
100

Concentration (at%)
90
80
70
60
50
40
30
20
10
0
0 1 2 3 4 5 6 7 8
(a) Distance (nm)

70 Co% Cu%
60

Concentration (at%)
50
40
30
20
10
0
0 5 10 15 20 25 30 35
Fig. 15. Atom map from 3DAP data for the as-deposited CoFe/Cu
MLF deposited using Ar + oxygen. The oxygen atoms (large, spheres) (b) Distance (nm)
and Cu atoms (small, dark spheres) are shown. The presence of a
columnar grain boundary is indicated. (Reproduced from [55] with Fig. 16. Composition profiles (showing only Co and Cu) across CoFe/
permission from The American Physical Society.) Cu multilayer films following annealing at 300° C for 30 min (a) for
deposition of Cu layers in Ar, and (b) for deposition of Cu layers in
Ar + oxygen.

3.4. Annealing studies

Diffusivity in Ni/Cu layered films (as-deposited and
annealed) has been studied by Keilonat et al. [21]. Ac-
tivation energies for interdiffusion, as a function of Cu
concentration, were measured and compared well with
previous literature data. Interfacial mixing in NiFe/Cu
multilayers was reported using 3DAP by Larson et al.
[57]. Highly intermixed interfacial regions at the NiFe-
on-Cu and Cu-on-NiFe interfaces were reported al-
though the geometry of the samples was such that the
interfaces were parallel to the specimen axis (Fig. 1(b))
so that the accuracy of the measurements can only be
considered to be
1 nm.
The interaction of an Al film deposited onto Ni (using
ion beam sputtering and electron beam evaporation) has
been studied by Jeske et al. [29] also using the method of
film deposition onto a preformed needle of Ni or W. It
should be noted that although Ni/Al layers are not of
interest per se in magnetic information storage systems,
the formation of the aluminium oxide tunnel barriers in
spin tunnel junction structures [3] is usually carried out
by depositing metallic Al on the underlying ferromag-
netic layer (such as a Ni, Fe or Co alloy) and then ox-
idising. Interdiffusion of the Al and the underlying layer
can therefore occur, which can lead to a decrease in the
spin polarisation in the ferromagnetic layer. In the as-
deposited state, Jeske et al. identified an initial solid
solution zone about 1 nm in width in both types of
samples. After annealing, an off-stoichiometry B2 NiAl
phase was observed to form in samples formed by
electron beam deposition of an Al layer onto a Ni nee-
dle, in which no grain boundaries were observed.
However, in samples where a Ni/Al bilayer was sputter
deposited onto a W needle, NiAl3 regions were observed
to form at grain boundaries in the Al layer. The authors
ascribed this to a difference in the flux of Ni into and out
of the thin inter-reaction layer at the Al/Ni interfaces.
In films containing grain boundaries, rapid diffusion
of Ni along the grain boundaries to the NiAl3 precipi-
tates leads to depletion of nickel in the interfacial region
and thus inhibits the formation of the intermetallic
phase [29].
Annealing of the Cu2 nm /Co2 nm multilayer films de-
scribed above has been studied by the current authors.
Samples that were annealed for 1h at 360 °C showed an
increase in grain size but no apparent change in the in-
terlayer mixing between Cu and Co [71]. Studies of the
CoFe/Cu films deposited in the presence of oxygen,
following annealing, tend to confirm that the presence of
oxygen drives the system further from equilibrium. This
can be seen from the changes in the GMR ratio for the
two types of film, as shown in Fig. 13. For the film de-
posited in Ar, the decrease in GMR ratio following
annealing at 300 °C for 30 min was from 1% to 0.5%,
whereas for the film deposited in Ar + oxygen, the de-
crease was from 7% to 0.2%. The changes to the trans-
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
port properties can be accounted for by changes to the
microstructure that occur during annealing. Fig. 16
shows composition profiles taken from 3DAP analyses
across annealed CoFe/Cu multilayer films with the Cu
layers deposited (a) in Ar and (b) in Ar + oxygen. As can
be seen from Table 1, the increase in interfacial mixing is
relatively small for the film deposited in Ar (the Cu
layers are still well defined), but for the film deposited in
the presence of oxygen, the CoFe-on-Cu interface width
increases by a factor of 5, and the Cu-on-CoFe in-
terface by a factor of 6.8. This is observed even though
the distribution of the oxygen surfactant does not ap-
pear to change after annealing, as can be seen from a
comparison of the atom maps shown in Fig. 15 (as-de-
posited) and Fig. 17 (following annealing at 300 °C for
30 min). It is likely that in the layers that are grown with
oxygen, and thus are further from equilibrium, the re-
duced conformal roughness provides a driving force for
Fig. 17. Atom map from 3DAP data for the CoFe/Cu MLF deposited
using Ar + oxygen, following annealing at 300 °C for 30 min. The
oxygen atoms (large, pale spheres) and Cu atoms (small, dark spheres)
are shown.
2859
intermixing at the Cu–CoFe interfaces to occur during
annealing. On the other hand intermixing in the layers
grown without oxygen appears limited to that which
occurs by atomic exchange during sputter deposition
[61]. However it is not clear from our results whether the
intermixing has occurred by long-range changes in the
interface position in order to establish the equilibrium
shape, or whether the non-equilibrium configuration
raises the free energy of the system sufficiently to make
the CoFe and Cu layers miscible [56].
3.5. Media materials
New information storage systems require not only the
development of new read/write heads but also of new
storage media. The media used currently in hard disk
drives consist of Co–Cr alloys (to which additional al-
loying elements such as Ta are frequently added) in
which the information is stored with the magnetisation
vectors in the plane of the film (longitudinal media). The
high storage density is achieved in the media by having a
polycrystalline film in which the grains are small and are
ideally magnetically decoupled from each other. Mag-
netisation studies of the films suggested that this occurs
because of compositional inhomogeneities in the CoCr
alloy layer [72] and this was confirmed by TEM studies
[73]. However the exact way in which the inhomogenei-
ties were distributed in three-dimensions had not been
well understood. The grain size in this type of material is
typically of the order of a few nanometres and this is
therefore an ideal topic to be addressed by 3DAP.
A small number of atom probe field ion microscopy
studies had been made of Co–Cr alloy thin films, both by
deposition of the films on curved surfaces [22] and using
the Hasegawa method [32] and more recently studies
have been made using 3DAP. Hono et al. [74] used the
Hasegawa method to prepare thin films of a Co–
22at%Cr alloy that had been deposited on a heated
substrate, as would be the case for the thin film media
layer on a hard disk. Their results showed that the films
consisted of a ferromagnetic phase and a paramagnetic
Cr-rich phase, both with a lamellar-type structure, which
coexist within each grain of the film. The lamellar shape
of the Co-rich ferromagnetic phase results in the particles
having a high shape anisotropy which increases their
thermal stability, and the presence of the paramagnetic
phase acts to isolate the ferromagnetic lamellae mag-
netically from each other. Further work on a similar
system was carried out by Nishikima et al. [75] on a Co–
12Cr–2Ta alloy thin film deposited at elevated temper-
ature. The addition of the Ta to the alloy resulted in
segregation of the Cr to the grain boundaries, leading to
Co-rich ferromagnetic grains, as shown in the Co con-
centration map in Fig. 18(a), enveloped by a Cr-rich non-
magnetic phase, seen in Fig. 18(b), but still with some
non-uniformity in the Cr composition within the grains.
2860 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 18. 3DAP concentration mapping in a Co–12Cr–2Ta alloy thin film
deposited at elevated temperature [75] showing (a) Co-rich ferromag-
netic grains, (b) a Cr-rich non-magnetic phase at the grain boundaries
(white arrows) and (c) a uniform distribution of Ta. (Reproduced from
[75] with permission from American Institute of Physics.)
The authors proposed that the enhanced segregation
occurred because the Ta atoms are larger than both Co
and Cr and thus reduced the migration energy of the Cr
to the boundaries. The Ta was found to be uniformly
distributed through the film, as seen in Fig. 18(c), and did
not segregate to the grain boundaries with the Cr.
One recent innovation has been the use of perpen-
dicular magnetic storage in which the bits of informa-
tion are written into a magnetic layer with the
magnetization vectors pointing perpendicular to the
plane of the magnetic film [76]. This allows for a con-
siderably higher information density than can be
achieved with conventional longitudinal storage media
[77]. A number of materials are currently being consid-
ered for perpendicular storage media, one of the most
popular being a Co/Pt or Co/Pd multilayer film in which
the Co layers are very thin (typically <1 nm) and the Pd
or Pt layers are of the order of 1 nm in thickness
[60,76,78]. In such a material an interfacial anisotropy
term is induced which forces the magnetic moments in
the Co layers to lie perpendicular to the plane of the
layers. A further advantage of such materials is that a
magnetic moment is induced on the Pt or Pd atoms, thus
Fig. 19. Hysteresis curve recorded using a vibrating sample magnetom-
eter for Co/Pd multilayer film deposited on glass at room temperature.
increasing the total moment of the multilayer. The na-
ture of the interfaces in these multilayers plays a major
role in controlling both the perpendicular interfacial
anisotropy and also the induced moment on the noble
metal.
Co/Pd layered films have recently been investigated by
the authors [79] with the specimens prepared on etched Si
posts in the same way as for the CoFe/Cu multilayer
films described above. The films were deposited at room
temperature and have the following structure: //Ti3 nm /
Ti–15Cr6 nm /Pd4 nm /(Co0:35 nm /Pd1:1 nm )12 /NiFe cap. In
order to check that the layers deposited on the Si posts
were similar to those deposited on standard substrates,
X-ray rocking curves were recorded through the [1 1 1]
peak. The Co/Pd multilayers have a significant degree of
crystallographic texture, comparable to that of a ‘‘full’’
media stack on standard NiP substrates (FWHM ¼ 6.8°
for the Co/Pd multilayer on Si, 7.8° for the Co/Pd mul-
tilayer on a standard glass substrate and 8.9° for the full
media stack on NiP/Al). Fig. 19 shows a VSM curve for a
film deposited on a glass substrate. The magnetisation
shows a sharp drop at a low coercive field with a long tail
that is characteristic of highly exchange-coupled per-
pendicular media. The exchange coupling within each Co
layer results from a lack of isolation between adjacent Co
grains, which would normally be induced by using a Co-
alloy instead of pure Co to promote the segregation of a
non-magnetic phase to the grain boundaries. The mag-
netic data show that the saturation magnetization is
enhanced by more than 30% with respect to that of pure
Co, indicating that a moment has been induced on the Pd
atoms. In addition the easy axis of the films lies close to
the direction normal to the film plane and the anisotropy
is enhanced relative to that of pure Co (for which
(K1 + K2 ) ¼
5.6  106 erg cm2 ), indicating the presence
of an induced interfacial contribution to the anisotropy.
Fig. 20 shows (a) an atom map and (b) the corresponding
 D.J. Larson et al.: Overview No. 138 / Acta Materialia 52 (2004) 2847–2862
Fig. 20. 3DAP data from Co/Pd multilayer film deposited on Si at
room temperature showing (a) the positions of Co atoms (large dark
spheres), Pd atoms (large light spheres) and the Ni capping layer (small
dark dots) and (b) the corresponding composition profile.
composition profile taken from 3DAP data for the Co/
Pd multilayer film. Four Pd layers and three Co layers
are visible plus part of the NiFe cap (which shows atomic
planes). As can be seen, the Co and Pd layers are not
clearly differentiated; the Co concentration varies from

20% to
40% across the Co layers. The binary phase
diagram for Co–Pd [69] shows complete solubility be-
tween the two elements and, in addition, the deposition
was carried out in a relatively low Ar pressure, leading to
high adatom energy and increased intermixing. Thus it is
not entirely surprising that a high degree of intermixing
was observed in the Co/Pd samples. However, such a
high degree of intermixing was unexpected from a con-
sideration of the magnetic data, which show a degree of
perpendicular anisotropy greater than would be expected
without inclusion of an interfacial contribution arising
from the Co/Pd interfaces.
4. Summary and conclusions
The aim of this paper has been to show that 3DAP
analysis is a technique that can be very effectively ap-
2861
plied to the understanding of the correlation between
microstructure, composition and physical properties in
thin films with applications in information storage. The
technique is particularly appropriate to films in which
the composition is inhomogeneous on the nanometre
scale, for example because the film consists of thin lay-
ers, or because of chemical segregation at grain
boundaries, and for which the properties can vary
greatly even with atomic scale differences in chemical
distribution. The validity of the technique has been
demonstrated by comparison with molecular dynamics
models of the growth mode in CoFe/Cu layered films,
which allows us to place reliance on the experimental
data that are obtained using 3DAP.
However, as for all techniques, there are outstanding
issues with using 3DAP for the analysis of thin films, of
which one is specimen preparation and another is the size
of the analysis volume. In order to make valid correla-
tions of the composition profile and microstructure with
the magnetic and transport properties, the authors be-
lieve that it is crucial to analyse films that have been de-
posited on planar substrates. As has been illustrated
above, this is now an achievable goal, and the results that
have been obtained have been invaluable in enabling
phenomena such as the effect of surfactants on GMR in
CoFe/Cu multilayers to be elucidated. The analysis vol-
ume in 3DAP remains limited, although novel instrument
designs are currently helping to address this issue too. In
any case, careful comparison with other techniques such
as TEM can ensure that the data that are obtained using
3DAP are typical of the structure as a whole.
In conclusion, we believe that atomic-scale nano-
characterisation using 3DAP, possibly combined with
molecular dynamics modeling, provides a unique tool
that can be applied both to the design of nanostructured
magnetic materials for information storage applications
and to the further understanding of the fundamental
physical properties on which their operation relies.
Acknowledgements
The authors thank Drs. T.P. Nolan, P.H. Clifton,
S.P. Bozeman, H.L. Brown, E.W. Singleton, R. Grove,
R. Hipwell (Seagate Technology LLC), M. Abraham, O.
Dimond, R.M. Langford and G.D.W. Smith FRS
(University of Oxford) for their various contributions to
this research. The authors especially thank Dr. X.W.
Zhou (University of Virginia) for his provision of the
MD model results on a rough substrate. We are also
grateful to the EPSRC for funding.
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