J Nanopart Res (2013) 15:1499
DOI 10.1007/s11051-013-1499-3
RESEARCH PAPER
Mesoscopic Ni particles and nanowires by pulsed
electrodeposition into porous Si
E. Michelakaki • K. Valalaki • A. G. Nassiopoulou
Received: 30 November 2012 / Accepted: 9 February 2013 / Published online: 10 March 2013
Ó Springer Science+Business Media Dordrecht 2013
Abstract We report in this article on the formation of
mesoscopic Ni particles and filling of continuous Ni
nanowires into porous Si layers of thickness in the range
of 0.5–4 lm with anisotropic vertical pores of average
diameter in the range of 30–45 nm using pulsed
electrodeposition from a Ni salt solution. The effect of
pulse duration, number of pulses, and total process time
on pore filling was investigated for porous Si with
different porosities and porous Si layer thicknesses in
the above thickness range. Scanning and transmission
electron microscopy were used to characterize the
samples. It was found that pore filling starts with Ni
nucleation and nanoparticle formation at different
points of the pore walls along the whole pore length
and continues with nanoparticle coalescence to form
continuous Ni nanowires that completely fill the pores.
The mechanism involved in pore filling is particle
nucleation and diffusion-controlled growth of Ni nano-
particles that coalesce to nanowires. From the beginning
of the process, a metal film starts to form on the porous Si
surface, and its thickness increases with increasing the
Special Issue Editors: Juan Manuel Rojo, Vasileios Koutsos
This article is part of the topical collection on Nanostructured
Materials 2012
E. Michelakaki  K. Valalaki  A. G. Nassiopoulou (&)
NCSR ‘‘Demokritos’’/IMEL, Terma Patriarchou
Grigoriou, Aghia Paraskevi, 15310 Athens, Greece
e-mail: A.Nassiopoulou@imel.demokritos.gr
process time. However, the presence of this film does
not impede further pore filling and nanowire formation
into the pores. This supports further the diffusion-
controlled growth mechanism. Finally, it was demon-
strated that full pore filling and continuous Ni nanowire
formation were also achieved under direct current
electrodeposition, and the results are quite similar to
those obtained with pulsed electrodeposition when the
same total deposition time is used in both cases.
Keywords Ni nanoparticles  Ni nanowires  Porous
Si  Electrodeposition
Introduction
With the accelerated development of nanotechnology,
nanoparticles and nanowires constitute a fast growing
research field involving Physics, Chemistry, Biology,
Engineering Science and Medical Science with a large
variety of applications. Electrodeposition is one of the
most important techniques for depositing metals at the
nano- and micrometer scale and has gained an
increasing interest in the recent years for use in many
fields. In the field of electronics, the interest in
electrodeposition has been accelerated since its appli-
cation in Cu metallization of integrated circuits (ICs)
(Andricacos et al. 1998) using the damascene process,
but other important applications are emerging, includ-
ing magnetic nanostructures for use in magnetic
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random access memory devices (MRAMs) (Tehrani
et al. 1999) and other information storage media
(Tehrani et al. 1999; Nguyen-Van-Dau et al. 1997),
spintronic devices, etc. Nanomodulated ferromagnetic
thin films fabricated by electrodeposition on a pat-
terned surface have been recently demonstrated to
show controlled magnetic anisotropy due to magnetic
dipole formation (Maity et al. 2012). Nanoparticles
and nanowires of ferromagnetic metals incorporated
into porous templates of nonmagnetic materials have
been the objects of intensive research in the recent
years as they can exhibit giant magnetoresistance and
coherent spin waves (Dolgiy et al. 2012) for applica-
tions in magnetic recording. Both porous anodic
alumina and porous Si are used as porous templates
(Ye et al. 2009; Kawail and Ueda 1975), with porous
Si providing a larger range of pore sizes and porosity
than alumina. In addition, porous Si is totally
compatible with Si processing and can be incorporated
in a Si IC fabrication process. A composite material
with Nickel metallization in macroporous Si has been
recently proposed as an effective material for radio-
frequency (RF) cross-talk isolation in mixed signal ICs
(Zhang et al. 2011).
Anodic dissolution of Si for the formation of porous
Si layers has been extensively studied since the
discovery of its intense room temperature light
emission by Canham (1990). The structure and
morphology of porous Si depend on the doping type
and resistivity of the Si wafer and the electrochemical
conditions used. Under appropriate conditions, an
anisotropic structure with straight vertical pores can be
obtained, which is appropriate for use as a template for
vertical metal nanowire formation. Metal filling of
macroporous Si with pore diameter in the micrometer
range has been studied in the literature (Jeske et al.
1995; Fukami et al. 2008; Zacharatos and Nassiopou-
lou 2008; Fang et al. 2007). However, less study has
been devoted to metal filling of vertical pores of
diameter in the nanometer scale (Granitzer et al. 2009;
Granitzer and Rumpf 2010). Cu, Au, Pt and Ni
electrodeposition on Si has been extensively investi-
gated (Oskam and Searson 2000; Krumm et al. 2000;
Ji et al. 2001; Penner 2002; Chenna et al. 2008,), and
most of the conclusions of this research apply also to
metal deposition into porous Si (Zhang et al. 2011;
Jeske et al. 1995; Fukami et al. 2008; Zacharatos and
Nassiopoulou 2008; Fang et al. 2007). In general, a
hydrogen-terminated low energy planar Si surface
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J Nanopart Res (2013) 15:1499
enables prompt metal particle precipitation at process
initiation, instead of a smooth electrodeposit on the Si
surface. The size of these particles becomes mono-
tonically broader during electrodeposition. We found
that a similar mechanism takes place in Ni filling of
freshly etched H-terminated porous Si samples.
Porous Si/Ni nanocomposites were extensively
investigated by Granitzer and Rumpf (2010) and
Rumpf et al. (2006). They mainly used thick porous Si
layers on n-type Si substrates and investigated the
magnetic properties of the Ni nanostructures in the
porous matrix. They demonstrated (Granitzer et al.
2012) enhanced magnetic anisotropy of Ni nanowires
in porous Si, fabricated by anodization under an
external magnetic field.
In this study, we systematically investigated the
formation of Ni nanoparticles and nanowires into
0.5–4-lm-thick porous Si layers, formed on p-type Si
with resistivity in the range of (0.001–0.005) X cm.
The mechanism of Ni nanoparticle and nanowire
formation into porous Si will be discussed. The aim of
this study is to develop a local substrate material on the
Si wafer for RF cross-talk isolation in on-chip passive
devices and mixed signal ICs.
Experimental results
Sample fabrication
Porous Si layers were fabricated on (100) p-type Si
with resistivity in the range of (1–5) mX cm by
electrochemical dissolution of bulk crystalline Si in an
HF:ethanol solution (volume ratio 40:60), using a
current density Je of 20 and 80 mA/cm2. Under the
conditions used, the material porosity changed from
70 % at 20 mA/cm2 to 88 % at 80 mA/cm2. An
example of material structure and morphology is
illustrated in the cross-sectional scanning electron
microscopy (SEM) image of Fig. 1, where vertical
pores with dendrite-like branching within the layer
that reach the Si substrate are depicted. By increasing
the porosity, the vertical pores become straighter, and
the dendrite structure at their sidewalls is smoothed
down. The thickness of the porous Si layers was in the
range of 0.5–4 lm.
Pulsed electrodeposition of Ni into the pores was
performed at a constant current density of 20 mA/cm2
using rectangular pulses with a period between 26 and
J Nanopart Res (2013) 15:1499
Fig. 1 Example of SEM image of a porous Si layer formed by
electrochemical etching of p? Si (resistivity in the range of
1–5 mX cm) using an HF:ethanol solution. Material porosity of
the specific sample was measured at 70 %. Pore morphology is
anisotropic, with vertical branched nanopores reaching the Si
substrate
30 s. The ‘‘on’’ duration of the pulse changed between
1 and 5 s, while the ‘‘off’’ duration (pulse delay time)
was fixed at 25 s. The electrolyte used was 0.2 M
NiCl26H2O, 0.1 M NiSO46H2O with 0.4 M H3BO3
of pH = 4.5 as a buffer. The solution was sonicated
for 1 h before each deposition step.
Ni electrodeposition was performed immediately
after porous Si etching to avoid porous Si oxidation in
air. Immediately after etching, the large internal Si
surface of the porous Si layer is passivated with
hydrogen from the HF electrochemical solution. The
surface of the starting material is thus a hydrogen-
terminated Si surface.
Electrodeposition into porous Si: kinetics of pore
filling with Ni and effect of porosity
Porous Si layers, 1 lm thick, etched at a current density
Je = 20 mA/cm2, were first investigated. Pulsed elec-
trodeposition, also at a current density Jd = 20 mA/cm2,
was used. Pulse duration was 1 s, with a pulse delay time
of 25 s. Cross-sectional SEM images were obtained
from the samples fabricated by increasing the number of
pulses (5, 15, and 150 pulses), and they are depicted in
Fig. 2a1–a3, respectively. In the micrographs of Fig. 2a4,
a5 the cross-sectional view of the top part of the layer of
samples fabricated with 15 and 150 pulses, respectively,
is depicted. In Fig. 2a1 (corresponding to 5 pulses) only
Page 3 of 9
a small number of reduced size Ni nanoparticles are
present within the pores. These nanoparticles are
attached at pore walls along the whole pore length.
By increasing the number of pulses from 5 to 15
(Fig. 2a2), the size and number of Ni nanoparticles
increases, whereas by increasing the number of pulses
to 150, continuous Ni nanowires are formed (Fig. 2a3).
If we examine the surface of the porous Si layer at
different pulse numbers, then we can see that Ni
deposition on the porous Si film starts from the
beginning of electrodeposition (5 pulses), while a
thicker layer is progressively formed on the surface by
increasing the number of pulses. This is illustrated in
Fig. 2a4, a5 for 15 and 150 pulses, respectively. The
fact that the porous Si surface is completely covered
by metal does not impede further pore filling with
metal.
We also compared the results obtained for the 70 %
porosity sample with those obtained for a porous Si
layer with much higher porosity (88 %). A new set of
experiments was performed, in which we followed
again the nucleation and growth kinetics of Ni
particles within the 88 % porosity layer (formed with
Je = 80 mA/cm2), using an increasing number of
pulses. The results are depicted in Fig. 2b1–b4 for 5,
11, 30, and 150 pulses. The general behavior is similar
to that of the 70 % porosity film, which means that the
number of Ni nanoparticles increases with increasing
the number of pulses and at 150 pulses the porous Si
layer is completely filled with Ni nanowires (Fig. 2b4),
however, the size of Ni nanoparticles for the same
number of pulses is larger (see Fig. 2a1, a3 in
comparison with Fig. 2b1, b4, respectively). At
150 pulses, both porous Si layers are completely filled
with Ni nanowires, their diameters being larger in the
case of the layer with higher porosity.
Transmission electron microscopy (TEM) images
were also obtained from two different samples and are
shown in Fig. 3. The fabrication conditions were
similar to those of Fig. 2a1, with the difference that the
number of electrochemical pulses was equal to 7 in (a),
(b), and (c), and 12 in (d). Samples for TEM
observation were prepared by just scratching the
composite layer Ni/porous Si from the Si substrate. In
Fig. 3a, a bright-field TEM image of a central part of
the porous Si layer is depicted. In this micrograph, we
can clearly identify the Ni nanoparticles within the
pores. A dark-field image of the same sample area is
shown in Fig. 3b, confirming the presence of Ni
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Fig. 2 Cross-sectional SEM images of two porous Si layers,
1 lm thick, after pulsed electrodeposition of Ni at a current
density of 20 mA/cm2, pulse duration 1 s, pulse delay time 25 s,
with the number of pulses being increased between 5 and 150.
a1–a5 correspond to a porous Si layer with 70 % porosity and 5,
15, and 150 pulses for a1–a3, respectively. b1–b4 Illustrate the
case of an 88 % porosity sample, etched at a current density of
nanoparticles within the porous matrix. Figure 3c
shows an image taken from a part of the composite
film situated near the surface area of the sample. It
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J Nanopart Res (2013) 15:1499
80 mA/cm2. The numbers of pulses were: 5 (b1), 11 (b2), 30
(b3), and 150 (b4). a4, a5 Show the top layer area of the same
samples of micrographs (a2, a3), respectively. In these two
micrographs, we also identify the Ni layer deposited at the
porous Si surface during electrodeposition, having increasing
thickness with the increasing number of electrochemical pulses.
The existence of this layer does not impede pore filling with Ni
shows a Ni film, starting to grow on the top porous Si
surface. By increasing the number of pulses (see the
micrograph of Fig. 3d for 12 pulses), the Ni layer
J Nanopart Res (2013) 15:1499
Fig. 3 TEM images from a sample fabricated with similar
conditions as those of the sample of Fig. 2a, but with a different
pulse time and pulse duration (here 12 pulses of 5-s duration).
The micrographs shown in a, b were taken from a central part of
deposited at the porous Si surface becomes thicker,
forming an almost continuous polycrystalline metal
layer.
Effect of porosity
A series of experiments was also carried out to
investigate the effect of porous Si layer porosity on
metal deposition into the pores. It was found that by
changing the porosity of the porous Si layer, under the
same electrodeposition conditions, the size and num-
ber of deposited Ni nanoparticles increase. The results
are depicted in Fig. 4 for samples with the increasing
porosity from 70 to 88 % (current density for Si
etching changing from 20 to 80 mA/cm2). At 70 %
porosity with the used electrodeposition conditions,
the average size of Ni nanoparticles is small (&23 nm,
Page 5 of 9
the sample, while those in c, d from a surface area of the sample.
Micrographs a, c, d are bright-field images, while in b a dark-
field image is shown
Fig. 4a), while it increases in size at 86 % and 88 %
porosities (&33 nm, Fig. 4c, d). The number of
nanoparticles also increases, the nanoparticles being
uniformly distributed on the whole internal pore
surface. The increase in the number and size of
nanoparticles with increasing porosity can be attrib-
uted to the larger quantity of electrochemical solution
within the pores, which leads to slower depletion of
the solution from metal ions.
Pulsed versus direct current electrodeposition
We also investigated the effect of direct (dc) current
compared to pulsed electrodeposition by applying the
same total deposition time in one sample with
150 pulses of 1-s duration and in another sample a
dc current for a total duration of 150 s. A porous Si
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Page 6 of 9
Fig. 4 SEM images of Ni-filled porous Si layers with different
porosities and pore morphologies and same electrodeposition
conditions (Jd = 20 mA/cm2, ton = 5 s, toff = 25 s, 3 pulses).
In the low porosity layer, the size and number of Ni
layer, 1 lm thick, was used. We found that in both
cases, the final result was an obtainment of porous Si
layers fully filled with Ni nanowires and a 170-nm-
thick Ni film deposited on top of the porous Si layer.
The results are depicted in Fig. 5a, b from which it is
clear that for the specific film thickness investigated,
there is no difference between pulsed and dc electro-
deposition. However, this could be different in the
case of very thick porous Si layers. This aspect needs
further investigation.
Effect of porous Si layer thickness
The effect of porous Si layer’s thickness on pulsed
electrodeposition was investigated for porous Si layers
of thickness between 0.5 and 3 lm. The results are
depicted in Fig. 6. Under the same experimental
conditions, the 0.5-lm-thick porous Si layer is fully
filled with Ni nanoparticles, while only few Ni
nanoparticles were formed within the 3-lm-thick
porous Si layer. This demonstrates that the important
parameter in pore filling is the total electrodeposition
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J Nanopart Res (2013) 15:1499
nanoparticles are smaller than those in the higher porosity
layer. This can be ascribed to faster depletion of the solution
from metal ions in the case of the low porosity layer that
increases the growth time
time, in combination with the porous Si layer’s
thickness.
Mechanism of Ni nanoparticle and nanowire
formation
The above experimental results fully support the
following electrodeposition mechanism into the ver-
tical pores of a porous Si layer, which is similar to that
described for a flat H-terminated Si surface (Penner
2002).
At the beginning of the process, metal particles are
promptly formed, and the size of these particles
becomes monotonically broader during the deposition.
Metal particle nucleation instead of layer-by-layer
deposition is induced by the low surface energy of the
hydrogen-terminated Si pore walls. Nucleation of new
particles occurs progressively during growth, leading
to a broad nanoparticle size distribution. Diffusion-
controlled growth governs the particle growth (Reiss
1951; Zoval et al. 1996) if the particle growth reaction
is rapid enough to deplete reactant at the particle
J Nanopart Res (2013) 15:1499 Page 7 of 9

Fig. 5 Comparison between dc and pulse electrodeposition of

Ni in porous Si. In a pulsed electrodeposition was used, with
150 pulses of 1-s duration (other conditions same as in Fig. 2a),
while in b, a dc current was used for the same total time of 150 s

surface. In this case the corresponding growth law is

given by:
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
rðtÞ ¼ 2  Vm  D  C  t;
where r(t) is the particle growth rate, Vm is the molar
volume of the metal, D is the diffusion coefficient for
metal ions, C* is the bulk concentration of metal and
t is the electrodeposition time.

Discussion

It was demonstrated in the literature that the electro-

deposition of metal particles can be carried out under
conditions of instantaneous nucleation and diffusion-
controlled growth at graphite electrode surface. The
case of graphite electrode surface is similar to that of
Fig. 6 SEM micrographs of porous Si layers of different
hydrogen-terminated Si, since in both cases, surface is thickness [0.5 lm (a), 0.8 lm (b), 1 lm (c), and 3 lm (d)] after
coordinately saturated. When this surface is immersed electrodeposition with the following conditions: 3 pulses with
in a metal plating solution, a sufficiently negative 5-s duration in porous Si with 88 % porosity

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voltage to the electrode causes the reduction of metal
ions to metal atoms that cluster to form nanoscopic
metal particles in preference to a metal monolayer
because of the coordinately saturated surface. This is
the well-known Volmer–Weber (V–W) (Volmer and
Weber 1926) mode of growth. Our experimental
results show that this mechanism also applies to the
case of Ni electrodeposition into porous Si. Although
the surface of the layer is not planar and the pores are
in the nanometer range, the electrochemical solution
enters into the pores and Ni nanoparticles are
uniformly formed on the pore walls in the whole pore
depth. In the case of a planar surface, the growth law
for individual metal particles on the surface depends
on the number and proximity of neighboring particles.
The ‘‘communication’’ of a metal particle with its
neighbors is mediated by the depletion layer (layer of
solution which is depleted from metal ions relative to
bulk solution) surrounding each particle, which
extends to ten particle radii from the surface of each
particle under conditions of diffusion control. In the
case of the porous Si matrix, the solution infiltrated
into the pores at the beginning of electrodeposition,
but metal particle’s ‘‘communication’’ did not stop
during growth. This is because the small pore diameter
prevents full depletion region formation around each
particle, thus leading to continuous interparticle
communication. The Ni film formed on the porous
Si layer surface does not stop the diffusion-controlled
growth of the nanoparticles because this layer is not
compact (it is deposited on a porous Si layer, and it
continues to have some pores, as illustrated by the
TEM images of the Ni surface layer in Fig. 3c, d).
Through the pores of the Ni film, the electrochemical
solution is infiltrated into the depth of the porous layer,
facilitated by potential-induced transport.
Conclusion
The kinetics of growth of Ni nanoparticles and
nanowires into porous Si layers with vertical branched
pores of average diameter in the range of 30–45 nm
and layer thickness in the range of 0.5–4 lm were
examined by monitoring pulsed electrodeposition with
an increasing number of current pulses. It was
demonstrated that at the beginning of electrodeposit-
ion, nucleation of Ni nanoparticles on the pore walls
takes place, following the V–W growth mode. These
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J Nanopart Res (2013) 15:1499
nanoparticles are dispersed in the whole pore length.
By increasing the number of pulses of a given
duration, the size of Ni nanoparticles increases by
diffusion-controlled growth and neighboring nanopar-
ticles coalesce into larger ones, until a continuous Ni
nanowire is formed within the pores. By increasing the
layer’s porosity from 70 to 88 %, for the same number
and duration of electrochemical pulses, the obtained
Ni nanoparticles were larger, resulting in all cases in
the formation of a continuous Ni nanowire, completely
filling the pore. By changing the porous Si layer
thickness, the final result was qualitatively the same,
but the intermediate result was different. Under the
same total electrodeposition duration, in the thinner
porous Si layer, the size of Ni nanoparticles was larger
than in the case of the thicker one. However, by
increasing the deposition time, the pores were com-
pletely filled with Ni also in the case of the thicker
porous Si layers. This demonstrates that the electro-
deposition does not stop until full pore filling, although
deposition kinetics are different, depending on porous
Si layer thickness and porosity. Finally, surprisingly,
we observed similar results of complete pore filling
with Ni also when using dc instead of pulsed
electrodeposition.
Acknowledgments The research leading to these results has
received the funding from the European Community’s Seventh
Framework Programme (FP7/2007-2013) under grant
agreement NANOFUNCTION no 257375. The TEM micro-
graphs were obtained by C. Giannakopoulos, while SEM images
by C. Skoulikidou.
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