Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion
We demonstrate how cathodic corrosion in concentrated aqueous solutions enables one to prepare nanoparticles of various metals and metal alloys. Using various characterization methods we show that the composition of nanoparticles remains that of the starting material, and the resulting size distri...
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України
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| Цитувати: | Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion / A.I. Yanson, Yu.I. Yanson // Физика низких температур. — 2013. — Т. 39, № 3. — С. 399–405. — Бібліогр.: 18 назв. — англ. |
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Yanson, A.I. Yanson, Yu.I. 2017-05-29T14:04:21Z 2017-05-29T14:04:21Z 2013 Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion / A.I. Yanson, Yu.I. Yanson // Физика низких температур. — 2013. — Т. 39, № 3. — С. 399–405. — Бібліогр.: 18 назв. — англ. 0132-6414 PACS: 82.45.Aa, 82.45.Jn, 82.45.Yz, 82.65.+r https://nasplib.isofts.kiev.ua/handle/123456789/118253 We demonstrate how cathodic corrosion in concentrated aqueous solutions enables one to prepare nanoparticles of various metals and metal alloys. Using various characterization methods we show that the composition of nanoparticles remains that of the starting material, and the resulting size distribution remains rather narrow. For the case of platinum we show how the size and possibly even the shape of the nanoparticles can be easily controlled by the parameters of corrosion. Finally, we discuss the advantages of using the nanoparticles prepared by cathodic corrosion for applications in (electro-)catalysis. A.I.Y. and Yu.I.Y. acknowledge the Dutch NWO vidi grant and STW Valorization grant (project 12572), respectively. We thank P. Rodriguez for his pioneering contribution to the (100)-terminated nanoparticle studies, F. Tichelaar and P. Kooyman (TU Delft) for TEM analysis, E. Bouwman for providing generous access to the XRD facility. en Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України Физика низких температур К 75-летию со дня рождения И. К. Янсона Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion Article published earlier |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion Yanson, A.I. Yanson, Yu.I. К 75-летию со дня рождения И. К. Янсона |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion |
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Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion |
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cathodic corrosion: part 2. properties of nanoparticles synthesized by cathodic corrosion |
| author |
Yanson, A.I. Yanson, Yu.I. |
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Yanson, A.I. Yanson, Yu.I. |
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К 75-летию со дня рождения И. К. Янсона |
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К 75-летию со дня рождения И. К. Янсона |
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2013 |
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English |
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Физика низких температур |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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We demonstrate how cathodic corrosion in concentrated aqueous solutions enables one to prepare nanoparticles
of various metals and metal alloys. Using various characterization methods we show that the composition of
nanoparticles remains that of the starting material, and the resulting size distribution remains rather narrow. For
the case of platinum we show how the size and possibly even the shape of the nanoparticles can be easily controlled
by the parameters of corrosion. Finally, we discuss the advantages of using the nanoparticles prepared by
cathodic corrosion for applications in (electro-)catalysis.
|
| issn |
0132-6414 |
| url |
https://nasplib.isofts.kiev.ua/handle/123456789/118253 |
| citation_txt |
Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion / A.I. Yanson, Yu.I. Yanson // Физика низких температур. — 2013. — Т. 39, № 3. — С. 399–405. — Бібліогр.: 18 назв. — англ. |
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AT yansonai cathodiccorrosionpart2propertiesofnanoparticlessynthesizedbycathodiccorrosion AT yansonyui cathodiccorrosionpart2propertiesofnanoparticlessynthesizedbycathodiccorrosion |
| first_indexed |
2025-11-27T02:19:16Z |
| last_indexed |
2025-11-27T02:19:16Z |
| _version_ |
1850793756076277760 |
| fulltext |
© A.I. Yanson and Yu.I. Yanson, 2013
Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3, pp. 399–405
Cathodic corrosion: Part 2. Properties of nanoparticles
synthesized by cathodic corrosion
A.I. Yanson and Yu.I. Yanson
Leiden Institute of Chemistry, Leiden University, Postbus 9502, Leiden 2300RA, The Netherlands
E-mail: a.yanson@chem.leidenuniv.nl
Received November 16, 2012
We demonstrate how cathodic corrosion in concentrated aqueous solutions enables one to prepare nanoparti-
cles of various metals and metal alloys. Using various characterization methods we show that the composition of
nanoparticles remains that of the starting material, and the resulting size distribution remains rather narrow. For
the case of platinum we show how the size and possibly even the shape of the nanoparticles can be easily con-
trolled by the parameters of corrosion. Finally, we discuss the advantages of using the nanoparticles prepared by
cathodic corrosion for applications in (electro-)catalysis.
PACS: 82.45.Aa Electrochemical synthesis;
82.45.Jn Surface structure, reactivity and catalysis;
82.45.Yz Nanostructured materials in electrochemistry;
82.65.+r Surface and interface chemistry; heterogeneous catalysis at surfaces.
Keywords: cathodic corrosion, electrochemistry, nanoparticles, alloys.
Introduction
In recent decades the interest in nanometer-sized parti-
cles, i.e. nanoparticles, of different materials has grown
tremendously from both the fundamental and the applica-
tion points of view. The reasons for such great interest are
manifold. From the fundamental perspective, the reduction
of the size of particles results in the change of their physi-
cal and chemical properties due to the mesoscopic and
quantum mechanical effects. From the practical point of
view, nanometer-sized particles are attractive due to their
large surface-to-volume ratio. Both effects are actively
explored in heterogeneous catalysis [1], where a process
occurs at the surface of a (mostly noble metal) catalyst.
The use of smaller, nanometer-sized particles therefore
allows reducing the amount of catalyst needed for the reac-
tion. Although much progress has been made in the deve-
lopment of reliable methods of nanoparticle synthesis, the
lack of a universal and simple production method remains
to be the bottleneck for their industrial application in many
areas.
In the first part of this paper we have shown that cathodic
corrosion may lead to the formation of metallic (platinum)
nanoparticles. Here we present our further study on their
properties, and explore the possibilities of applications for
cathodic corrosion as a universal yet simple nanoparticle
synthesis method. We show that not only platinum, but all
tested metals are subject to cathodic corrosion which leads
to the formation of nanoparticles, whose size and perhaps
even shape can be easily controlled. Additionally, we find
that alloy nanoparticles of tunable composition can be easily
produced using the cathodic corrosion method. While many
possibilities of this versatile technique remain yet to be ex-
plored, the results presented here show that this method is
quick, clean, “green” and versatile enough to warrant further
investigation into possibilities for applications.
Experimental details
Unless noted otherwise, nanoparticles were prepared in
a small volume (10 ml) of a freshly-prepared NaOH solu-
tion in 18.2 MΩ·cm ultrapure water (MilliQ). A wire elec-
trode of the desired material was submerged to a pre-
defined depth and an ac voltage was applied to it, using
glassy carbon as a counter electrode, until complete disper-
sion of the submerged wire. After the desired amount of
nanoparticles was produced, the electrolyte was washed off
by repeatedly centrifuging, decanting and re-dispersing in
ultrapure water until the conductivity of the suspension
dropped below 1 μS/cm. By controlling the initial amount
of cathodically corroded metal we could determine the
mass concentration of the nanoparticles in suspension, and
thus use a known weight amount of nanoparticles for fur-
ther experiments. This aqueous suspension of nanoparticles
was then drop-cast on different supports for further charac-
terization with transmission electron microscopy (TEM),
x-ray diffraction (XRD), and cyclic voltammetry (CV).
A.I. Yanson and Yu.I. Yanson
400 Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3
X-ray powder diffraction was performed on a Philips
X’pert diffractometer, equipped with an X’celerator detec-
tor, in a θ–2θ configuration. For XRD measurements, na-
noparticles were drop-cast on a zero-background sample
holder (Si or quartz). For the TEM measurements,
Quantifoiltm carbon-on-copper grids were used in a FEI
Tecnai F20 microscope. Electrochemical characterization
of the nanoparticles was performed in a standard three-
electrode glass cell, with the platinum flag used as a coun-
ter electrode and a reversible hydrogen electrode (RHE) as
a reference electrode. A polished polycrystalline gold elec-
trode, onto which a controlled amount of nanoparticles was
drop-cast, was used as a working electrode. Potential was
controlled by an Ivium (CompactStat) potentiostal. The
electrolyte was prepared from Merck UltraPurtm reagents
and ultrapure water, and thoroughly deaerated by bubbling
with 5N argon for 15 min prior to each experiment.
Physical properties of nanoparticles prepared by
cathodic corrosion
Figure 1(a) shows TEM images of Pt nanoparticles that
were produced using the cathodic corrosion method. These
nanoparticles were synthesized in a 10 M solution of
NaOH using an ac voltage of –10 to +10 V as described in
Part 1 [2]. From the lattice spacing in the TEM images, as
well as from the energy dispersive x-ray (EDX) analysis in
Fig. 1(b), we conclude that the particles consist of a pure
metal. Hence, we conclude that cathodic corrosion has
transformed the metallic wires into metallic nanoparticles.
Focussing on platinum, we have studied the particle
size distribution by TEM. Figure 2 shows the distribution,
whose maximum correlates well with the estimate for the
average particle size of 12 nm obtained by fitting the
widths of the XRD diffraction lines with the Scherrer for-
mula. The latter correlates the broadening of an XRD peak
to the size of nanoparticles [3].
As one can see, the distribution is rather narrow and in-
vites the question whether size controlled synthesis of nano-
particles is possible via this cathodic corrosion method. Fi-
gure 3(a) demonstrates that this is indeed the case. We have
obtained XRD patterns of platinum nanoparticles synthe-
sized at various current densities, and used Scherrer equation
to determine the average particle size. The resulting semi-
linear dependence shows that simply by varying the ac cur-
rent during cathodic corrosion one can directly influence the
size of the resulting nanoparticles between 6 and 12 nm.
An important measurement supporting the validity of
this method of size determination via XRD is presented in
Fig. 3(b). It is well-known that while the nanoparticles
become smaller, their lattice constant decreases. By fitting
the x-ray diffraction peaks we can determine their exact
positions, and hence the lattice constant. The monotonous
Fig. 1. (a) TEM image of Pt nanoparticles synthesized by cathodic corrosion. The corresponding EDX analysis graph is shown in (b).
The EDX results show that the nanoparticles consist of pure metal. The weak signal of Al in the EDX spectrum comes from the TEM
sample holder.
Fig. 2. Size distribution of platinum nanoparticles obtained by the
ac cathodic corrosion in 10 M NaOH, as measured by the high-
resolution TEM.
Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion
Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3 401
contraction of the lattice constant for smaller nanoparticles,
shown in Fig. 3(b), is in line with the reported values for
particles of such sizes [4,5] indicating that our size deter-
mination is correct and that we have indeed achieved size-
controlled synthesis with this method.
The dependence in Fig. 3(a) can be understood if we
consider the model of cathodic corrosion presented in
Part 1 of this article [2]. By increasing the current density
we increase the corrosion rate and thus the concentration of
the precursor for nanoparticle growth in the electrolyte
adjacent to the electrode. In the nucleation-and-growth
mechanism, such increase would lead directly to the for-
mation of larger nanoparticles under the assumption that
the nucleation density remains constant. This is indeed
what we observe.
Many properties of nanoparticles are governed by the
fact that a significant fraction of the atoms are on the sur-
face. As the surface tension of such high curvature objects
is rather high, the system usually tries to minimize the sur-
face area by adopting a quasi-spherical shape. However,
many interesting properties arise if one can coerce the na-
noparticles into some peculiar, nonequilibrium shapes [6].
A distinct plasmon resonance in gold nanorods is perhaps
the most prominent example of the usefulness of these
properties [7]. Here we show that using our synthesis
method we can influence the surface properties of nanopar-
ticles, creating particles with a large fraction of (100) fa-
cets at the surface. Such particles with relatively open sur-
faces are very promising nanocatalysts [8]. In Fig. 4 we
present a TEM image of such nonspherical particles and a
set of the so-called “blank” cyclic voltammograms, which
show the hydrogen desorption region on platinum nanopar-
ticles prepared in different concentrations of NaOH. A
clear tendency of the increase of the peak at 0.27 V and the
Fig. 3. (a) Nanoparticle size determined from the (111) XRD
peak, using the Scherrer formula, as a function of the ac current
employed during synthesis at –10 to 10 V in a 5 M NaOH solu-
tion. (b) Average lattice constant determined from the position of
the first five XRD lines for each nanoparticle sample using
Bragg’s law (bulk Pt value 3.92 Å).
Fig. 4. (a) TEM images of nonspherical platinum nanoparticles
prepared by ac corrosion in 10 M NaOH. (b) Cyclic voltammo-
grams (CVs) of 5 μg of platinum nanoparticles synthesized in
various concentrations of NaOH electrolyte at –10 to +10 V ac
(black) and at –10 V dc (grey). Particles were drop-cast on a gold
support and the CVs were measured in hanging meniscus confi-
guration in a three-electrode electrochemical cell. The cell was
filled with 100 ml of 0.5 M H2SO4 solution, de-aerated with ar-
gon of 5N purity. Curves were recorded at 50 mV/s scan rate
and normalized by the electrochemical surface area using the
210 μC/cm2 coefficient from Ref. 13.
A.I. Yanson and Yu.I. Yanson
402 Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3
formation of a shoulder at 0.36 V with increasing concen-
tration can be seen. Comparing with the reference voltam-
mograms for platinum single crystals [9] we conclude that
our nanoparticles develop more and more (100) step and
terrace sites at their surface. Following the analysis of
Ref. 10 we see that for the nanoparticles prepared in most
concentrated electrolytes, the amount of (100) sites at the
surface exceeds 50%.
The fact that the preferential orientation of the surface
of the nanoparticles can be influenced just by the concen-
tration of the solution, in which the nanoparticles are syn-
thesized, is rather unique. In general, to change the shape
of nanoparticles that are produced by conventional chemi-
cal reduction methods, additional substances that adsorb
preferentially on certain crystallographic planes are added
to the solution. The growth of these planes can be either
inhibited or promoted by the adsorption, leading to either
stronger or weaker expression of these planes on the sur-
face of the particles, correspondingly. However, these ad-
sorbed additives also act as “contaminants”, inhibiting the
useful properties of such nanoparticles during catalysis.
These additives adsorb so strongly that they are difficult to
remove from the particle surface [11]. In order to explain
our shape-selective synthesis without additives, we suggest
that the cations (Na+) that are present in the solution are
preferentially adsorbed on the (100) crystallographic planes,
thus leading to a stronger expression of these planes on the
nanoparticles. In fact, recent DFT calculations have con-
firmed that adsorption of Na+ is energetically much more
favorable on the (100) planes of platinum [12]. The advan-
tage of this method to control the preferred orientation of the
surface of the particles is that the surface remains clean, i.e.,
free of adsorbed organics.
The mechanism of cathodic corrosion that we have pro-
posed in the first part of this paper does not rely on the
particular type of cationic species present in solution, as
long as the cation remains irreducible at the electrode sur-
face. We have confirmed experimentally that cathodic syn-
thesis of nanoparticles proceeds in solutions containing
Li+, K+, Cs+, Ca2+, as well as ammonium and tetraalkyl-
ammonium cations. Moreover, nanoparticles are formed
during cathodic corrosion in solutions rather independent
of the type of the anions [14]. The generic nature of this
phenomenon suggests applicability to metals other than
platinum. Indeed, we have observed cathodic corrosion and
nanoparticle formation for Pt, Rh, Pd, Au, Cu, Re, Fe, Ni,
Nb, Ti, Si and Al. While for some the particles remain me-
tallic, for others, due to the aqueous alkaline environment
in which they are formed, they quickly oxidize. This de-
monstrates that the cathodic corrosion method can be used
to produce nanoparticles of virtually any metal. Characteri-
zation of some metallic particles is shown in Fig. 5.
Fig. 5. (a) X-ray diffraction patterns of Au, Ag, Pt, Cu and Rh nanoparticles produced by ac corrosion in NaOH. The positions of the
peaks coincide with those expected for the crystal structure of a corresponding metal (in the case of Cu and perhaps Ag some oxide is
also visible). Using Scherrer formula, which correlates the width of a diffraction line to the crystallite size in the sample, we obtain the
rough indication for the average crystallite size to be 15, 58, 12, 57 and 6 nm, respectively*. (b), (c) TEM images of Au and Rh nanopar-
ticles, respectively. (d), (e) Size distributions of Au and Rh nanoparticles, obtained from the analysis of the TEM images.
* The value for Au was recently revised through better fitting and comprehensive data analysis.
Cathodic corrosion: Part 2. Properties of nanoparticles synthesized by cathodic corrosion
Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3 403
The data presented above convincingly shows that ca-
thodic corrosion is not an exclusive property of platinum,
and that other metals also readily form nanoparticles under
these electrochemical conditions. It is now tempting to see
what would happen if the starting electrode wire is made of
an alloy. In the following we show that in this case the
nanoparticles retain the alloy’s composition. Our XRD
results for a series of platinum–rhodium alloys, presented
in Fig. 6(a), reveal a surprisingly good agreement with the
Vegard rule [15]: the lattice constant, determined from the
position of the diffraction lines, changes linearly between
the limiting values of two pure metals proportionally to
their concentration in the alloy, see Fig. 6(b). An inde-
pendent EDX analysis reveals a very similar composition
of the nanoparticles, see Fig. 6(c). This is a rather im-
portant result, as it not only shows that the composition of
the alloy is retained in the nanoparticles, but also that the
constituent metals in the nanoparticles do not segregate but
remain properly alloyed.
The PtRh alloy example is not unique — other alloys
also exhibit similar behavior, see Fig. 7 [16]. This shows
that the cathodic corrosion method provides an easy way to
synthesize alloy nanoparticles.
To summarize, the cathodic corrosion method of nano-
particle synthesis allows one to produce clean particles of
Fig. 6. (a) XRD patterns of the nanoparticles obtained from PtxRh1–x alloys of different composition. Dashed lines indicate positions of
pure Pt (black) and Rh (grey) diffraction maxima. (b) Position of the diffraction lines vs. the composition of the alloy. Grey, dashed line
shows the resulting average particle size per alloy. (c) Energy dispersive x-ray (EDX) analysis of the composition of the PtxRh1–x nano-
particles. Reproduced from Ref. 16.
Fig. 7. XRD patterns of nanoparticles of some platinum alloys.
The shift of the diffraction lines from the pure Pt positions
(dashed lines) is the consequence of alloying.
A.I. Yanson and Yu.I. Yanson
404 Low Temperature Physics/Fizika Nizkikh Temperatur, 2013, v. 39, No. 3
virtually any metal. The nanoparticles have a narrow size
distribution and the average particle size can be easily con-
trolled. Furthermore, if the starting electrode is an alloy,
the method yields alloyed nanoparticles. Finally, there ap-
pear to be further possibilities towards controlling the sur-
face termination and thus the shape of the nanoparticles.
Catalytic properties
All these properties are particularly attractive for appli-
cations in heterogeneous catalysis. Platinum, being one of
the most scarce and expensive metals, is also one of the
best industrial catalysts. As the reactions take place only
on the surface of platinum, it is extremely advantageous to
maximize its surface area by converting platinum into na-
noparticles. Additionally, catalytic activity of small nano-
particles may be enhanced due to size-effects [1]. We have
shown that platinum nanoparticles synthesized by the ca-
thodic corrosion method show higher catalytic activity per
gram of platinum than the state-of-the-art commercial cata-
lysts. This is due to the fact that the surface of our nanopar-
ticles is extremely clean and, since they are formed in
highly non-equilibrium conditions, has many irregularities
known as “active sites” [14]. The latter are especially ad-
vantageous for the oxidation reactions of small alcohols,
relevant for fuel cells [1].
Another catalytic process that is very relevant for
wastewater treatment is the reduction of nitrite (or nitrate)
to nitrogen. While most processes reduce nitrite to ammo-
nia, recently an electrochemical process has been discov-
ered which can very selectively convert nitrite into
dinitrogen [17]. Unfortunately, the selectivity can only be
obtained on Pt(100) single crystal electrodes, which is
clearly an impractical solution for removing nitrite contam-
ination from wastewater. By synthesizing platinum nano-
particles with high amount of (100) sites on the surface as
described above, we have managed to obtain the required
selectivity also on the practical nanocatalyst.
In industrial catalysis it is long established that alloys
often have superior catalytic properties compared to pure
metals. For example PtRu alloy is much more resistant to
carbon monoxide poisoning in an alcohol fuel cell com-
pared to pure Pt [18]. The combination of Pt and Rh in an
alloy should be advantageous for nitrate reduction. With
the cathodic corrosion method we have synthesized both
the PtRu and PtRh nanoparticles and showed their en-
hanced activity for methanol oxidation and nitrate reduc-
tion, respectively [16]. In the future it would be most inter-
esting to apply this method to the synthesis of the
automotive three-way exhaust catalyst, which consists of
Pt, Rh and Pd.
Conclusions
In this article we have presented a new, simple yet ver-
satile method for the electrochemical synthesis of nanopar-
ticles. We have also shown that this new method allows for
great control of their properties, namely the size, the shape
and the composition. As these are the very first results, we
envisage many more possibilities for making practical
quantities of nanoparticles with pre-defined properties us-
ing this method of cathodic corrosion.
One attractive possibility, briefly mentioned in the text,
is the synthesis of bimetallic nanoparticles where one met-
al will oxidize, providing an oxidic support for a catalytic
nanoparticle of the second metal. This will provide great
flexibility towards synthesizing novel catalysts for numer-
ous reactions. Another yet unexplored possibility lies in
using this method for the synthesis of semiconductor
nanocrystals, also known as quantum dots. Further, one
can think of exploiting the universality of the method for
the synthesis of, e.g., superconducting (alloy) nanoparti-
cles, etc. It is clear that both the fundamental aspects of
novel chemistry of cathodic corrosion and the broad hori-
zon of potential applications should be explored further.
Acknowledgments
A.I.Y. and Yu.I.Y. acknowledge the Dutch NWO vidi
grant and STW Valorization grant (project 12572), respec-
tively. We thank P. Rodriguez for his pioneering contribu-
tion to the (100)-terminated nanoparticle studies, F. Tiche-
laar and P. Kooyman (TU Delft) for TEM analysis, E. Bouw-
man for providing generous access to the XRD facility.
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