Electrochimica Acta 56 (2011) 5178–5183

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Electrochimica Acta
journal homepage: www.elsevier.com/locate/electacta

Electrodeposition and characterization of Fe80 Ga20 alloy films

D. Iselt a,b,∗ , U. Gaitzsch a , S. Oswald a , S. Fähler a , L. Schultz a,b , H. Schlörb a
a
IFW Dresden, Leibniz Institute for Solid State and Materials Research Dresden, PF 27 01 16, 01171 Dresden, Germany
b
TU Dresden, Faculty of Mechanical Engineering, 01062 Dresden, Germany

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

Article history: Due to its high magnetostriction and good mechanical properties Fe80 Ga20 is interesting for magne-
Received 6 December 2010 tostrictive microactuators and sensors. Here we use electrodeposition to grow Fe–Ga films onto Au and
Received in revised form 8 February 2011 Pt coated Si substrates by potentiostatic and pulse potential deposition. Composition, microstructure
Accepted 11 March 2011
and structure are analysed. The desired composition of Fe80 Ga20 was obtained at −1.4 VSCE and −1.5 VSCE ,
Available online 22 March 2011
respectively. The origin of low reproducibility and high oxygen content up to 50 at.% is investigated. Opti-
mum deposition conditions to achieve dense, homogeneous films with low oxygen content are identified.
Keywords:
In these films the saturation magnetization reaches a maximum value of 1.7 T confirming the high quality
Galfenol
Fe100−x Gax
of electrodeposited films.
Thin film © 2011 Elsevier Ltd. All rights reserved.
Electrodeposition
Magnetostriction

1. Introduction rods. Focusing on smaller dimensions a few groups investigated

the deposition of thin films by physical methods. Butera et al. [18]
Magnetostrictive materials change their dimensions with deposited 900 nm thin films on (1 0 0)MgO substrates using sputter
changes in magnetization and are therefore interesting for actuator deposition, and were able to find the correlation between sputter
and sensor applications. Since the discovery of magnetostriction pressure and growth behaviour. A linear dependence of the FeGa
of iron by James Joule in 1842, intensive research work has been lattice parameter was found by Dunlap et al. [19] in 2006: with
undertaken to understand the effect [1–5], to increase the length increasing Ga content the lattice parameter increases. Wang [20]
changes by addition of non-magnetic elements (like Al or rare earth analysed the influence of the sputter gas, thermal treatment and
elements) [2,6–8] and, recently, to use these materials as actua- deposition under external magnetic field. Using a sputter pressure
tion and sensing devices [9–13]. However, any application requires of 1.2 Pa under argon atmosphere he obtained a saturation mag-
besides a high magnetostrictive constant, also good mechanical netostriction S of up to 50 ppm. By depositing in a magnetic field
properties. Common ferromagnetic metals show good mechani- the sample texture changes from (1 1 0) to (1 0 0) orientation. Addi-
cal properties, such as ductility, but the magnetostrictive strain tional heat pre-treatment has further improved the soft magnetic
is rather low (several 10 × 10−6 up to 100 × 10−6 ) [7,14]. Rare properties. The influence of the partial pressure of the sputtering
earth alloys show a “giant” magnetostrictive strain in the order gas on magnetic properties of Fe100−x Gax (19 ≤ × ≤ 23) has been
of 1000 × 10−6 (Terfenol-D, Tb0.3 Dy0.7 Fe2 ) [5] but they are brittle. investigated by Javed et al. [4]. Here, the best soft magnetic prop-
A promising candidate to overcome the mechanical limitations of erties for sensor applications are obtained when growing at low
rare earth alloys is Galfenol, an alloy of iron and gallium, which sputter pressures of 3 ␮bar. Adolphi et al. [21] investigated the
combines mechanical strength (Fe83 Ga17 endures tensile stresses influence of film thickness and seed layers on the film texture and
up to 440 MPa with strains approaching 0.25% before failure) [15] consequences of texture on the magnetic properties. They obtained
with “large” magnetostrictive strains (up to 400 ppm for quenched a high spontaneous polarization of JS = 1.45 T in 1.3 ␮m thick films
Fe80 Ga20 single crystals) [8]. Further advantages are H(sat) < 1 kOe, and summarised that the value of magnetostrictive parameters and
low temperature dependence in the range from −20 to 80 ◦ C [16,17] the relative permeability are promising for sensor bending appli-
and comparatively high oxidation stability. Most of the work on this cations.
material has been done on bulk single crystals, polycrystals and Compared to physical methods, electrochemical deposition pro-
vides an easy and low cost method to produce thin films over large
areas, in complex geometries and does not require high vacuum
∗ Corresponding author at: IFW Dresden, Helmholtzstrasse 20, D-01069 Dresden, conditions. However, the electrodeposition of FeGa had been rarely
Germany. Tel.: +49 351 4659 290; fax: +49 351 4659 500. investigated, since it is hard to deposit Ga [22–24] and its alloys
E-mail address: d.iselt@ifw-dresden.de (D. Iselt). [25] from aqueous electrolytes. The main reasons for this are the

0013-4686/$ – see front matter © 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.electacta.2011.03.046
 D. Iselt et al. / Electrochimica Acta 56 (2011) 5178–5183 5179

highly negative standard potential of Ga3+ /Ga (E00 = −0.560 V) [23]

and its strong tendency to hydrolyse [24]. McGary reported first
on the electrochemical deposition of Fe–Ga alloys, the fabrication
of nanoscale Galfenol structures [26] and their use as sensor sys-
tems for sonar applications [10]. Using a Watt’s type electrolyte
containing iron(II) and gallium(III) sulphates, boric acid and ascor-
bic acid Fe–Ga nanowire arrays have been deposited into anodic
aluminium oxide templates at a constant potential of −1.36 V.
The Ga content was found to decrease along the length of the
wires and the nanowire arrays were magnetically soft and slightly
anisotropic [26]. However, even for films no crystalline Fe–Ga phase
was observed [10] and no statement was made about the oxygen
content of the deposit. Another group investigated the electro-
chemical fabrication of magnetic multilayered films and nanowire
arrays containing Fe–Ga in order to achieve novel magnetostrictive
behaviour [27,28]. By adjusting both, the electrolyte composition
and deposition potential, Fe78 Ga22 films with a crystalline (Fe, Ga)
solid-solution phase were obtained. Multilayered nanowire arrays
were deposited from a single electrolyte by applying different con-
stant potentials. A novel magnetostrictive behaviour was explained
by the formation of twisted spin structures. Very recently, a detailed
study of Fe–Ga codeposition was published by McGary [29]. Using
a Hull cell, where the deposition current density varies across the
cathode, metallic iron, Galfenol, oxide and Ga-rich metal films have
been produced. Complexing the Ga ions with citrate and varying the
ratio of Ga3+ /Fe2+ ions and the current density allowed to control
the composition as well as grain size and texture of the alloy.
Our present study aims on the preparation and detailed char- Fig. 1. (a) Current–potential curves of single element and complete electrolytes on
acterization of Fe–Ga alloy films with a gallium concentration of Au substrates, scan rate 10 mV s−1 and (b) ratio of Ga in potentiostatically deposited
around 20 at.%. The particular focus is to investigate the origin of the Fe100−x Gax films on Au substrates in dependence on the deposition potential.
high oxygen content and to identify appropriate deposition param-
eters for homogeneous, dense alloy films with low oxygen content
Cu-K␣ radiation. For magnetic measurements a vibration sample
that are promising to achieve a high magnetostriction constant.
magnetometer (VSM, Quantum Design PPMS) at 300 K was used.
Hysteresis loops were measured parallel and perpendicular to the
substrate plane using low background signal quartz holders.
2. Experimental details

Oxidized (1 0 0)Si wafers were coated with either Au or Pt which 3. Results and discussion
acts as working electrodes for the deposition experiments. Based
on McGary’s work [10] the electrolyte consists of an aqueous solu- In order to identify the suitable potential range for the co-
tion of 0.3 M FeSO4 ·7H2 O, 0.06 M Ga2 (SO4 )3 ·18H2 O, 0.5 M boric acid deposition of Fe and Ga potentiodynamic current–potential curves
(H3 BO3 ) as a buffer and 0.04 M ascorbic acid (C6 H8 O6 ) as an antiox- of both single element and complete electrolytes have been per-
idant agent, where the pH was adjusted to 1.5 by adding sulphuric formed, shown in Fig. 1. The cathodic polarization of pure Fe
acid. For each experiment 20 ml of fresh electrolyte was used. All solution (red dotted curve in Fig. 1a) starts with a first step at
deposition experiments were performed at room temperature in −0.6 V which is attributed to proton reduction. The following
a three electrode arrangement placed in a Teflon cell. A Pt sheet strong current increase, starting at around −1.05 V, represents
was used as the counter electrode and a Saturated Calomel Elec- the iron reduction overlapped by water decomposition. The
trode (SCE) as reference electrode. The electrode potentials all refer current–potential curve of the pure Ga3+ solution (blue dashed
to the potential of the SCE (−241 mVSHE ). Deposition experiments curve in Fig. 1a) is characterized by a continuous current increase
were carried out using an EG&G Potentiostat/Galvanostat Model starting at −0.7 V. The first step observed in Fe2+ solution does not
263A. occur, pointing out the inhibition of proton reduction. This, as well
Sample surface and cross sectional morphologies as well as as the much smaller slope compared to the Fe2+ solution, might be
film thickness were examined using high-resolution scanning elec- explained by a passivation of the electrode surface by hydrolysis
tron microscopy (HR-SEM Leo 1530 Gemini, Zeiss) and focused products of Ga. The starting point of Ga3+ reduction cannot be iden-
ion beam technique (FIB, Zeiss Cross Beam 1540XB), respectively. tified because of its potential overlapping with the one for water
The integral composition was obtained by energy dispersive X-ray decomposition. The behaviour of the complete electrolyte (black
spectroscopy (EDX, Leo 1530 Gemini, Zeiss with Si(Li)-detector). solid curve in Fig. 1a) is similar to the Ga3+ solution down to −0.95 V.
To estimate the oxygen content and the detailed oxygen binding Afterwards a two step behaviour is observed that approaches the
behaviour depth profiles were measured by Auger electron spec- current density of the iron solution at potentials around −2.0 V.
troscopy (AES, PHI Model 660 Scanning Auger Microprobe, Physical Potentiostatic deposition experiments from the single element
Electronics) and X-ray Photoelectron Spectroscopy (XPS, PHI 5600 solutions provide stable films at potentials E ≤ −1.0 V for iron and
CI, Physical Electronics, Excitation: Mg-K␣ radiation, sputtering: E ≤ −1.8 V for Ga, in contrast to the results reported by Flamini
Ar+ -ions 3.5 keV, 3 nm/min sputter abrasion). The structure was et al. [24] who quote the suitable deposition potential for Ga
analysed by X-ray diffraction in Bragg–Brentano geometry (XRD, as E ≤ −1.58 V. Potentiostatically deposited films from the com-
Phillips PW 3400, Co-K␣ radiation) and the texture by pole figure plete electrolyte are unstable at potentials more positive than
measurements using a Philips X‘Pert 108 Texture Goniometer with −1.3 V, dissolving immediately under gas evolution after stopping
5180 D. Iselt et al. / Electrochimica Acta 56 (2011) 5178–5183

Fig. 2. SEM surface image (a) and FIB cross section (b) of a E1 = −1.5 V, E2 = −0.9 V (t1 = t2 = 10 s) pulse-deposited Fe80 Ga20 film.

Fig. 3. FIB cross sections of pulse-deposited Fe–Ga films at different pre-conditions: (a) deposition started 1200 s after immersing electrode into electrolyte and (b) immersing
electrode into electrolyte under potential applied.

the deposition. However, at E = −1.3 V and lower potentials stable sequent strong interactions of the amphoteric Ga3+ ions and/or its
films are obtained. As shown in Fig. 1b the Ga ratio in Fe100−x Gax hydrolysis products with the substrate surface. The detailed reduc-
increases to a maximum value of around 50 at.% with decreasing tion mechanism is beyond the scope of this article and will be the
potential but with high uncertainty due to film inhomogeneities subject of a further study.
caused by a strong hydrogen evolution. The desired composition Potentiostatically deposited films were hardly reproducible
of about Fe80 Ga20 is obtained at −1.3 V ≤ E ≤ −1.4 V with compara- showing irregular morphologies and oxygen contents of up to
tively minor changes. 50 at.% as determined by SEM/EDX. Both, the inhomogeneous mor-
For all following depositions the substrate was changed from Au phology and the high oxygen content were expected to be avoided
to Pt. This allows later X-ray diffraction analysis of the crystalline by applying appropriate potential pulses. While keeping the depo-
structure of the deposited films by avoiding the overlap of substrate sition potential constant (E1 = −1.5 V) a second “off”-potential
and film reflections. To achieve the desired composition of Fe80 Ga20 E2 = −0.9 V was introduced and both potentials were applied 60
on Pt an offset of the deposition potential to −1.5 V was essen- times for t1 = t2 = 10 s. SEM analysis reveals an almost smooth sur-
tial. This potential offset is obviously associated with the catalytic face morphology with a high number of large grains growing out
activity of the Pt substrate, enhancing proton reduction and sub- of the film (see Fig. 2a). FIB cross sections (Fig. 2b) show a dense

Fig. 4. XPS depth profiles of pulse-deposited Fe–Ga films at different pre-conditions: (a) deposition started 1200 s after immersing electrode into electrolyte and (b) immersing
electrode into electrolyte under applied potential.
 D. Iselt et al. / Electrochimica Acta 56 (2011) 5178–5183 5181

Fig. 5. XPS spectra of iron (a and b) and gallium (c and d) at different sputter depth (marked in Fig. 4): (a) and (c) deposition started 1200 s after immersing electrode into
electrolyte and (b) and (d) immersing electrode into electrolyte under applied potential.

layer with compact particles. At the bottom of each particle pores mated as 85:15 in reasonable agreement with the EDX data given
were observed that are most probably originate from gas bubbles above. The deviation of ∼7 at.% might be related to the sum of the
evolved at the initial stages of deposition. systematic errors (use of standard sensitivity factors, preferential
Aiming at homogeneous, dense films without outgrowing par- sputtering) of both methods. The increase of the Pt and later the Si
ticles these pores have to be avoided. This again requires further signal indicates that the substrate surface is reached.
investigation of the initial stages of deposition. To do this two bor- In general, the XPS profiles show a high oxygen content of
der cases have been intensively investigated: (A) the deposition 20–30 at.% for sample (A) and a much lower oxygen content of
potential is applied 1200 s after immersing the working electrode 1–10 at.% for sample (B). Directly at the sample surface both sam-
into the electrolyte and (B) the working electrode is immersed to ples show a high oxygen content up to 80 at.% indicating a strong
the electrolyte under applied deposition potential. affinity to surface oxidation. Afterwards both samples strongly dif-
Whereas the Fe/Ga atomic ratio of both films is identical at ∼0.78 fer from each other. The oxygen content in sample (A) only slowly
the overall thickness of film (A) with ∼400 nm exceeds the thick- reduces to a relatively high minimum value of 20 at.%. The most
ness of film (B) with ∼200 nm by almost a factor of 2. Furthermore, probable reason for this slow decrease is the high porosity and
FIB cross sections reveal strong differences in film morphology therefore high surface-to-volume ratio observed in the cross sec-
(Fig. 3). An inhomogeneous, porous and dendritic like growth in tion (Fig. 3a). With increasing sputter depth the oxygen content
three different stages is observed for sample (A) (Fig. 3a). Sample (B) again increases up to 30 at.%. In the lower third of the film thick-
(Fig. 3b) is a dense and homogeneous film without any pores. Here, ness the oxygen content again slightly decreases to a final value
grain like contrasts can be seen in the FIB cross section indicating of around 28 at.%. Due to the high porosity of the film oxygen sur-
a metallic deposit. face diffusion might be strongly enhanced therefore influencing the
In order to analyse the oxygen content and its distribution over accuracy of the results.
film thickness in more detail AES and XPS depth profiles have Contrary, the oxygen content in sample (B) sharply decreases to
been measured. The related XPS profiles starting from the film sur- less than 1 at.% within the first 20 nm (4–6 min sputter depth). This
face down to the film–substrate interface of samples (A) and (B) value remains constant over 2/3 of the film thickness and slightly
are compared in Fig. 4a and b, respectively. Similar results were increases to 11 at.% near the film–substrate interface.
obtained by AES depth profiles measurements and therefore are not Detailed information about the oxygen binding behaviour was
shown here. For both samples the Fe:Ga atomic ratio can be esti- extracted from single spectra recorded during the XPS depth profile
5182 D. Iselt et al. / Electrochimica Acta 56 (2011) 5178–5183

measurements. For both, iron and gallium characteristic selected

spectra over the thickness of the films are shown in Fig. 5. The
selected depth steps for both samples are marked in Fig. 4 with
numbers from 1 to 5. As expected from the very high oxygen con-
tent both iron and gallium are oxidized at the sample surfaces. No
metallic Fe and Ga had been determined in spectrum 1 for both
samples.
For the porous and inhomogeneous sample (A) the oxygen con-
tent decreases only slowly (see Fig. 4a) and therefore oxidized
species still appear in spectra 2 of Fig. 5a and c. Unlike Ga that is still
completely oxidized metallic Fe already arises. The Fe spectra 3–5
(Fig. 5a) show mostly metallic Fe and only a minor fraction of oxi-
dized Fe species. Spectrum 3 of Ga (Fig. 5c) shows mainly metallic
gallium with a minor portion of oxidized Ga whereas this trend is
again reversed in spectra 4 and 5 with more oxidized than metallic
Ga.
In contrast to these results the spectra 2–5 of the dense and
homogeneous sample (B) show nearly pure metallic peaks for both
iron (Fig. 5b) and gallium (Fig. 5d) over the whole film thickness.
No trace of oxidized species is observed in spectra 2–4 in agree-
ment with the low oxygen content of only about 1 at.% found in
this region. Spectrum 5 of gallium near the interface to the sub-
strate (Fig. 5d) reveals a slight decrease of the metallic quantity Fig. 6. XRD pattern (a) and (1 1 0) pole figure (b) of a dense, homogeneous film.
Substrate reflections in the XRD pattern are marked with (*).
and a marginal shoulder of oxidized Ga shows up.
Even though the particular deposition mechanism is not known
in detail, the combination of the obtained results gives important
hints for the process occurring: strong interactions of the elec-
trolyte components, mainly Ga3+ ions or its hydrolysis products,
with the Pt substrate lead to the formation of a passivating film at
the interface between electrolyte and substrate. Once a passivating
film is formed electrodeposition can occur only at defects in this
film or at high overpotentials favoring dendritic growth as well as
hydrogen evolution and the formation of highly porous films with
high surface area. After terminating the deposition the high sur-
face area immediately tends to form a surface oxide layer. On the
other hand, if the deposition is immediately started once the elec-
trolyte comes into contact with the substrate, these interactions are
almost completely prevented. Thereby avoiding strong passivation
can prevent both dendritic growth and high oxygen content. As
a result dense films with oxygen contents as low as 1 at.% can be
obtained that are required for magnetostrictive applications.
The XRD pattern of the homogeneous, dense sample is pre- Fig. 7. Hysteresis loops of a dense layer with low oxygen content measured parallel
sented in Fig. 6a. Besides the substrate reflection of Si(82◦ ) and (||) and perpendicular (⊥) to the substrate.

Pt(46◦ , 104◦ ) only one intense reflection at 52.1◦ occurs that can be
assigned to the (1 1 0) reflection of the thermodynamically stable is required to saturate the field out of plane. Close to saturation in
␣-Fe3 Ga phase exhibiting a disordered bcc structure. A very weak both directions a noticeable curve bending is observed. This indi-
reflection related to (2 1 1) Fe3 Ga is additionally observed at 98.4◦ . cates the presence of some additional anisotropy, which may either
As the (1 0 0) and (2 0 0) reflections of Fe3 Ga are absent these results originate from magnetocrystalline anisotropy or, more likely, on
indicate a strongly preferred (1 1 0) orientation. Additional texture magnetostrictive anisotropy induced by film stress.
measurements of the (1 1 0) pole figure (see Fig. 6b) show an intense The magnetic measurements particularly confirm the high qual-
central spot at  < 10◦ and a ring at  = 60◦ . The angle between the ity of the electrodeposited films containing only a negligible
different {1 1 0} planes in the cubic system is 60◦ . Therefore the number of defects and impurity phases.
ring at 60◦ with equally distributed intensities combined with the
central spot proves a (1 1 0) fibre texture with no preferred in plane 4. Conclusion
orientation. Additionally measured (2 0 0) and (2 1 1) poles confirm
the (1 1 0) fibre texture (not shown). FeGa alloy films with a desired composition close to Fe80 Ga20
Magnetic properties have been obtained by measuring hys- and a (1 1 0) Fe3 Ga fibre texture have been fabricated electrochem-
teresis loops parallel and perpendicular to the film plane and are ically. Strong interactions of the electrolyte with the substrate
shown for the dense film with low oxygen content in Fig. 7. The surface are identified to cause low reproducibility and high oxygen
film shows a low coercivity of 4 mT parallel and 30 mT perpendic- content. Using optimized pre-treatment and pulsed potential con-
ular to the substrate indicating soft magnetic behaviour. A high ditions the films are dense and homogeneous. The oxygen content
saturation magnetization of about 1.7 T is achieved that exceeds was reduced to less than 1 at.% and the saturation magnetization
values reported for sputtered films of 1.45 T [21] and approaches reaches up to 1.7 T, confirming the high quality of these films. These
the values for bulk single crystals of 1.75 T [2]. As expected due to results show that electrodeposition can be most effectively used to
shape anisotropy the easy axis of magnetization is strongly aligned grow Fe80 Ga20 films for application in magnetostrictive actuating
within the film plane and a field close to spontaneous polarisation and sensing devices
 D. Iselt et al. / Electrochimica Acta 56 (2011) 5178–5183 5183

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