ARTICLE IN PRESS

Journal of Crystal Growth 285 (2005) 681–

691
www.elsevier.com/locate/jcrysgro

Beyond Archimedean solids: Star polyhedral gold nanocrystals

Justin L. Burta, Jose L. Elechiguerraa, Jose Reyes-Gasgaa,b, J.
Martin Montejano-Carrizalesc, Miguel Jose-Yacamana,
a

Department of Chemical Engineering, Texas Materials Institute, Center for Nano- and Molecular Science and Technology,
The University of Texas at Austin, Austin, TX, 78712-1062, USA
b
On sabbatical from: Instituto de Fisica, Universidad Nacional Autonoma de Mexico. Apartado Postal 20-364,
01000 Mexico D.F., Mexico
c

Instituto de Fisica, Universidad Autonoma de San Luis Potosi, 78000 San Luis Potosi, S.L.P., Mexico
Received 31 August 2005; accepted 8 September 2005

Communicated by K. Nakajima

Abstract

We report star polyhedral gold nanocrystals synthesized by colloidal reduction with ascorbic acid in water at ambient
conditions. We identify two distinct classes of star nanocrystals: multiple-twinned crystals with fivefold symmetry, and
monocrystals. These respective classes correspond to icosahedra and cuboctahedra, two Archimedian solids, with preferential
growth of their {111} surfaces. Due to this preferential growth, the {111} faces of the original Archimedean solids grow to
become tetrahedral pyramids, the base of each pyramid being the original polyhedral face. By assuming a star morphology,
gold nanocrystals increase their proportion of exposed {111} surfaces, which possess the lowest surface energy among low-
index crystallographic planes for FCC crystals. Thus, we propose that the driving force for star nanocrystal formation could be
the reduction in surface energy that the crystals experience. Interestingly, icosahedrally derived star nanocrystals possess a
geometric morphology closely resembling the great stellated dodecahedron, a Kepler-Poinsot solid. r 2005 Elsevier B.V. All
rights reserved.

PACS: 61.46.+w; 81.07.Bc; 68.37.Lp; 68.37.Hk

Keywords: A1. Nanocrystal morphology; A1. Nanostructures; B1. Star nanocrystals

1. Introduction
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682 J.L. Burt et al. / Journal of Crystal Growth 285 (2005) 681–691
Corresponding author. Tel.: +15122329111; fax:
+15124717060.
E-mail address: yacaman@che.utexas.edu (M.
Jose-Yacaman).
0022-0248/$-see front matter r 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.jcrysgro.2005.09.060
the academician and layman alike. The classical
Greeks deduced the existence of five regular convex
polyhedra (the Platonic solids), but the discovery of
regular star polyhedra (the KeplerPoinsot solids)
dates from the Renaissance. Interestingly, regular star
polyhedra were first envisioned by artists who
embellished their renderings of the Platonic solids by
replacing their surfaces with pyramids. For example,
a marble inlay of the small stellated dodecahedron is
found in the floor of St. Mark’s Basilica in Venice,
and is attributed to Paolo Uccello, a fifteenth-century
artisan. The German artist Wentzel Jamnitzer
produced a conceptual drawing of the great stellated
dodecahedron in his Perspectiva Corporum
Regularium, published in 1568. It was more than 50
years later when the small and great stellated
dodecahedra were recognized as regular concave
polyhedra from a mathematical standpoint, when
Johannes Kepler described them in his landmark work
Harmonices Mundi, published in 1619. The dual
structures of the small and great stellated dodecahedra
were subsequently described by Louis Poinsot in
1810 [1].
Polyhedral crystals are a prized pursuit in the world
of nanoscience, both from an intellectual and a
practical standpoint. Metallic nanostructures exhibit
unique properties and are of interest in a wide range
of applications including catalysis, electronics, and
sensors [2,3]. The morphology of a nanocrystal
strongly influences its electromagnetic, optical, and
physicochemical properties [4], and new strategies for
growing nanocrystals of various shapes are
continually being developed. Branched
nanostructures are also highly desired, and great
progress has been made in the synthesis of branched
semiconductor nanocrystals [5–7].
Recently, the first branched gold nanostructures
were reported [8,9]. The synthesis methods employed
were derived from the seed-mediated growth
technique that has been used extensively for the
production of gold nanorods [10–12]. Briefly, gold
Philosophers, mathematicians, and artists have long
been fascinated by regular polyhedra, and their
aesthetically pleasing symmetry appeals to
ionic salt is reduced with a weak reducing agent
(typically ascorbic acid) in the presence of seed
crystals, and of surfactant molecules that promote
growth in a specific crystallographic direction. The
morphology of the resulting crystals depends on the
size, shape, and type (i.e. gold or silver) of seed
crystals used, on the relative concentrations of seed
crystals, ionic salt, and surfactant molecules, and on
the number and duration of incubation steps
employed.
We have found that branched gold nanocrystals can
also be obtained without the use of seed crystals,
surfactant molecules, or successive incubation steps.
Herein we report the structural features of star
polyhedral gold nanocrystals, synthesized by colloidal
reduction with ascorbic acid. We have identified two
distinct types of star polyhedral nanocrystals,
corresponding to icosahedra and cuboctahedra with
preferential growth of their exposed {111} surfaces.
Specifically, the {111} faces of the original
Archimedean solids grow into tetrahedral pyramids,
with the base of each pyramid being the original
polyhedral face. In the case of icosahedrally derived
star nanocrystals, the crystal shape closely resembles a
great stellated dodecahedron, one of the Kepler-Poinsot
solids. Our results suggest that the role of ascorbic acid
in promoting the formation of branched gold
nanocrystals is more significant than has been
appreciated to date.
2. Experimental procedure
2.1. Nanocrystal synthesis
Star polyhedral gold nanocrystals were synthesized
by colloidal reduction in aqueous solution at ambient
conditions. Hydrogen tetrachloroaurate trihydrate
(HAuCl43H2O, 99.9+%), and ascorbic acid were
purchased from Sigma-Aldrich. Briefly, a 32-fold
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molar excess of ascorbic acid dissolved in 10mL water
was added rapidly, under vigorous stirring, to a round
bottom flask containing an aqueous solution of 510 –
5
mol HAuCl4, bringing the total volume to 30mL. Upon
addition of ascorbic acid, the solution rapidly changed
color, becoming an opaque orange-red. Although the
reaction appeared nearly instantaneous, the solution
was left under vigorous stirring for fifteen minutes to
ensure completion of the reaction.
2.2. Electron microscopy
Transmission electron microscopy (TEM), selected
area electron diffraction (SAED), and weak beam dark
field (WBDF) analysis were performed using a JEOL
2010F TEM equipped with Schottky-type field
emission gun, ultra-high resolution pole piece (Cs ¼
0.5mm), and a scanning transmission electron
microscope (STEM) unit with high angle annular dark
field (HAADF) detector operating at 200kV. Scanning
electron microscopy (SEM) was initially performed
with an FEI Strata DB235 dual beam SEM/FIB, and
subsequently with a JEOL 7401F SEM.
3. Results
3.1. Overview of the as-synthesized product
Fig. 1(a) is a representative image of the
assynthesized product. On average, 20% consists of
rounded, multiple-twinned nanoparticles with
indefinite shapes. Most of these particles are smaller
than 50nm, whereas the branched crystals range from
100 to 200nm. When the branched crystals are
allowed to precipitate, the smaller rounded particles
remain in solution and are thus easily removed.
Another 20% of the as-synthesized product consists
of nanocrystals with one or more

Fig. 1. Star polyhedral gold nanocrystals. (a) Low-magnification TEM image of the as-synthesized product. (b) SEM image of a multiple-
twinned star nanocrystal, revealing pyramids emerging around the perimeter of the crystal and from its upper surface. (c, d) SEM images of
monocrystalline stars demonstrating the presence of eight pyramids, each oriented 901 from its nearest neighbors.
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enlarged pyramids, but lacking a uniform dispersion
of pyramids over the entire crystal surface. The
appearance of these crystals often resembles an
arrowhead. The remaining 60% of the assynthesized
product consists of star polyhedral gold nanocrystals,
with 20% being multipletwinned crystals with
fivefold symmetry, and 40% being monocrystalline
star polyhedra. As mentioned previously, the size of
these crystals is on the order of 100–200nm, but
despite this broad variation, the geometric proportions
of a given type of star nanocrystal are remarkably
consistent from one crystal to another, regardless of
size.
Fig. 1(b) is an SEM image of a multiple-twinned
star nanocrystal. Pyramids are observed emerging in
projection from the upper surface of the crystal, which
confirms that the pyramids are threedimensional
features. Figs. 1(c) and (d) are SEM images of
monocrystalline star polyhedra. In Fig. 1(c), four in-
plane pyramids oriented 901 from each other are
observed. Additionally, two pyramids 901 from each
other emerge from the upper surface of the crystal, in
a plane orthogonal to that containing the other four
visible pyramids. Fig. 1(d) presents another
monocrystalline star in an orientation which reveals a
pyramid emerging from the lower surface of the
crystal, also at 901 from its nearest neighbors. From
these observations, and in combination with tilting
sequences from TEM images, we conclude that
monocrystalline stars possess eight pyramids, two
groups of four in-plane pyramids oriented 901 from
each other, in two orthogonal planes.
3.2. Multiple-twinned star polyhedra
Fig. 2(a) is a representative TEM image of the first
specific type of star polyhedral nanocrystal we have
characterized. Tilting sequences of TEM images, as
in Figs. 3(a)–(d), were performed, and by tracking the
emergence and disappearance of pyramids at various
tilting angles, three-dimensional reconstructions were
obtained. Twenty distinct pyramids were observed,
and their spatial arrangement indicates that they
emanate from an icosahedral core. Based on the
observed global symmetry, we propose a structural
model for this class of nanocrystal, seen in Fig. 2(b),
corresponding to an icosahedron with tetrahedral
pyramids extending from each of its 20 {111} faces.
The structure of these icosahedrally derived star
nanocrystals resembles the great stellated
dodecahedron, a Kepler-Poinsot solid. However, a
great stellated dodecahedron possesses elongated
pyramids, the edge length of each pyramid being
related to the edge length of the icosahedral base by the
golden ratio [13]. In contrast, our model was
constructed by growing tetrahedral pyramids on
icosahedral faces, both to satisfy FCC stacking and to
match the experimentally observed shape of the
pyramids. Properly speaking, our proposed model is a
60-faced deltahedron [14]. The peaks of the
nanocrystalline pyramids have a rounded appearance.
Since the corners of faceted nanocrystals generally
terminate in terraced steps [15,16], we expect surface
steps to give a rounded appearance to the peak of a
tetrahedral pyramid.
Figs. 4(a)–(c) present a multiple-twinned
nanocrystal, both in bright field (Fig. 4(a)) and WBDF
(Figs. 4(b) and (c)). From the bright field image, ten
pyramids are observed around the perimeter of the
crystal, while WBDF allows us to visualize the
pentagonal array of pyramids emerging from the upper
and lower surfaces of the crystal. For WBDF, a
diffraction-contrast image is formed by tilting the
sample out of the Bragg condition to increase inelastic
scattering. Thickness fringes are produced due to
interference between scattered and transmitted beams,
and the width and separation of thickness fringes is
directly related to the angle of incidence between the
electron beam and the sample. Thus, WBDF illustrates
how thickness changes within the crystal [17]. In the
vicinity of a defect, lattice distortions cause planes to
be locally tilted back to the Bragg condition, so twin
boundaries are clearly delineated.
By selecting diffraction spots corresponding to the
upper or lower surfaces in WBDF, we observe
pyramids extending above or below the plane of the
page. In Fig. 4(b) there is an upward-facing pentagonal
arrangement of pyramids, while in Fig. 4(c) the
pyramids form a downward-facing pentagon. This
agrees with the geometric arrangement of pyramids in
our proposed model (Fig. 2(b)). WBDF also reveals the
fivefold symmetry of the
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Fig. 2. The two classes of star polyhedral gold nanocrystals. (a) TEM image of a multiple-twinned star nanocrystal, and (b) proposed model,
an icosahedron with each of its 20 {111} surfaces replaced by a tetrahedral pyramid. (c) TEM image of a monocrystalline star, and (d) proposed
model, a cuboctahedron with each of its eight {111} truncations replaced by a tetrahedral pyramid.
twin boundaries, as required for an icosahedrally generally have brighter contrast. On the other hand, in
derived nanocrystal from purely geometric the vicinity of crystal defects, Huang-scattering
considerations. contrast results from inelastic dispersion that occurs
Figs. 4(d)–(f) present another icosahedrally derived when the electron beam encounters atoms that deviate
multiple-twinned nanocrystal. The bright field image from their ideal lattice positions [19,20].
(Fig. 4(d)) reveals 10 pyramids in-plane surrounding Huang-scattering contrast illuminates the fivefold
the center of the crystal (the tenth pyramid is slightly symmetric twin boundaries in Fig. 4(e). The brighter
hidden due to sample tilt). In the corresponding HAADF contrast in the center of the crystal is due to
HAADF image (Fig. 4(e)), the fivefold symmetry of increased thickness, which is expected since
the twin boundaries between pyramids on the upper pentagonal arrays of pyramids project from the upper
face of the crystal is clearly visible. HAADF images and lower surfaces of the crystal. In the electron
are formed by electrons that have undergone high angle diffraction pattern (Fig. 4(f)), the inner ring represents
scattering [18]. The two primary factors that determine {111}, and the outer ring {311} spots. An aperiodic
HAADF image contrast for our gold nanocrystals are sequence of
specimen thickness and structural defects. As electrons
travel through thicker regions of the specimen and
interfere with more atoms, the probability for high
angle scattering increases. Therefore, thicker regions
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Fig. 3. TEM tilt sequence for a multiple-twinned star nanocrystal, with [x1, y1] tilting angles (a) [0, –15]; (b) [0, 15]; (c) [0, 0]; and (d) [15,0].
(e, f) WBDF images illustrating some of the individual monocrystalline domains present within the crystal.
diffraction spots occurs along the axis running tions at one point [21], such as the pentagonal array of
vertically through the {220} spots. This aperiodicity pyramids at the center of Fig. 4(e).
is characteristic of crystals with fivefold symmetry,
and occurs when the electron beam encounters five
distinct crystallographic orienta-
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The multiple-twinned structure of these nanocrystals combined with the SEM analysis discussed previously
is a direct result of their fivefold symmetry. It is not (Figs. 1(c) and (d)), we propose a structural model, seen

Fig. 4. (a) TEM image of a multiple-twinned star nanocrystal. (b, c) Corresponding WBDF images, demonstrating the fivefold symmetric
twinned structure. (d) TEM image of another multiple-twinned gold nanocrystal. Corresponding (e) HAADF image and (f) SAED pattern. For
clarity, black lines outline the fivefold symmetry at the center of (e).
possible to fill space by joining five perfect tetrahedra in Fig. 2(d), corresponding to a cuboctahedron with
to form a center with fivefold rotational symmetry, tetrahedral pyramids extending from each of its eight
because a gap of 7.51 remains between the final two {111} faces. Figs. 5(a)–(c) present three orientations
tetrahedral units [22]. When crystals possessing for the cuboctahedrally derived star nanocrystals, and
fivefold symmetry are formed, such as the decahedron the corresponding SAED patterns (Figs. 5(d)–(f))
or icosahedron, defects must be introduced at the demonstrate the monocrystallinity of the structures.
tetrahedral boundaries to accommodate the structure Figs. 5(g) and (h) are HAADF images of the
[23]. Hence, the icosahedrally derived nanocrystals are orientations in Figs. 5(a) and (b), respectively. The
multipletwinned, with 20 distinct monocrystalline HAADF contrast in Fig. 5(h) reveals the presence of
domains (such as those visible in Figs. 3(e) and (f)). two pyramids in the central region of the crystal, in
addition to the six pyramids visible at the perimeter of
3.3. Monocrystalline star polyhedra the crystal.
The orientation of the star nanocrystal in Fig. 5(a)
Fig. 2(c) is representative of the second type of star is such that the four pyramids at the upper surface of
polyhedral nanocrystal we have characterized. Based the crystal are aligned directly above the four
on 3D reconstructions from TEM tilting sequences, and
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pyramids at the lower crystal surface. In the the center of the crystal, the electron beam travels
corresponding HAADF image (Fig. 5(g), the through one continuous monocrystalline region. On

Fig. 5. Monocrystalline star polyhedral gold nanocrystal. (a) TEM image, (d) SAED, and (g) HAADF image for the [001] zone axis. (b) TEM
image, (e) SAED, and (h) HAADF image for the ½11¯ 4¯ zone axis. (c) TEM image and (f) SAED for the ½11¯ 2¯ zone axis.
(i) Representative WBDF image. the other hand, at the corners the electron beam enters
one pyramid at the upper crystal surface, exits the
crystal, then reenters a pyramid at the lower crystal
contrast is brighter at the corners of the crystal than in surface with a different crystallographic orientation.
the center. This contrast inversion occurs because in This increases the local inelastic dispersion, resulting
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J.L. Burt et al. / Journal of Crystal Growth 285 (2005) 681–691
in brighter contrast at the corners even though the
crystal thickness is greatest in the center.
Fig. 5(i) is a WBDF image of a cuboctahedrally
derived star nanocrystal. The continuity of thickness
fringes over the entire crystal structure demonstrates its
monocrystallinity. In addition to illuminating the six
pyramids around the perimeter of the crystal, WBDF
contrast also reveals the two pyramids emerging in
projection from the upper and lower surfaces of the
crystal. These two pyramids are not visible in
conventional TEM images at this orientation, due to the
thickness of the central region of the crystal. The
thickness fringe contours also illustrate rounding of the
pyramid peaks, as noted previously. Thus, in both
monocrystalline and multiple-twinned star polyhedra,
local minimization of energy dictates rounded peaks
for the tetrahedral pyramids.
4. Discussion
4.1. Synthesis approach
The first reported branched gold nanocrystals were
synthesized using the seed-mediated growth technique
[8,9]. Because of the relative complexity of this system,
it has been difficult to discern which of the several
variables involved are critical for the growth of
branched gold nanocrystals. Our approach was to
develop a greatly simplified reaction in order to
determine the essential set of parameters required to
induce branching of gold nanocrystals. Our plan was to
minimize the number of variables, beginning simply by
reducing gold ionic salt with ascorbic acid in water.
Surprisingly, we found that adding a 32-fold molar
excess of ascorbic acid was sufficient to produce
branched gold nanocrystals at ambient conditions. At
lower molar excesses of ascorbic acid, less branching
and markedly increased aggregation was observed.
By foregoing the use of templating surfactant
molecules and seed crystals, we sacrifice a degree of
control over the size and shape distribution of the
products. However, with our simplified approach, we
know with certainty that it is exclusively ascorbic acid
molecules and their oxidized derivatives that promote
the preferential growth of {111} gold nanocrystal
surfaces in our reaction system. Our preliminary results
689
suggest that the role of ascorbic acid in the formation
of branched gold nanocrystals is more significant than
has been appreciated. Further research will be required
to gain a precise understanding of the role of ascorbic
acid in the branching of gold nanocrystals.
Subsequently, these insights could be combined with
more sophisticated synthesis techniques, such as seed-
mediated growth, to develop rational design criteria for
the controlled synthesis of a variety of branched gold
nanocrystals.
4.2. Preferential growth of {111} surfaces
Gold nanocrystals increase the proportion of their
exposed {111} surfaces by assuming star polyhedral
morphologies, since each exposed {111} surface of
the original Archimedean solid is replaced by a
tetrahedral pyramid presenting three exposed {111}
surfaces. For FCC crystals the relative surface
energies of the low-index crystallographic planes are
g111og100og110 [24]. Thus, assuming a star morphology
lowers the surface surface energy of a growing
crystal, and this could be the driving force for star
nanocrystal formation in our system.
The sizes of our icosahedrally derived star
nanocrystals are on the order of 100–200nm.
However, icosahedral gold nanocrystals of this size
are typically not observed. Recently, Yang and
coworkers demonstrated that by careful regulation of
the growth rate for each crystallographic direction,
icosahedral gold nanocrystals on the order of 100–
300nm can be synthesized [25]. For our reaction
conditions, in the presence of ascorbic acid and its
oxidized derivatives, icosahedral nanocrystals are
stabilized by preferential growth of their exposed
{111} surfaces, allowing for growth of icosahedrally
derived star polyhedral nanocrystals.
4.3. Characteristic defects
Although the vast majority of monocrystalline stars
are free from structural defects, a sizable number of
multiple-twinned stars contain defects and have an
imperfect shape. This is to be expected, since a
multiple-twinned structure inherently possesses more
lattice strain, and thus a higher potential for defects.
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However, characteristic defects were observed for 5. Conclusions

both classes of star polyhedral gold nanocrystals.
Fig. 6(a) is a TEM image of an imperfect multiple- In summary, we have synthesized star polyhedral
twinned star nanocrystal. In a defect-free multiple- gold nanocrystals by colloidal reduction with ascorbic
twinned star, each tetrahedral pyramid constitutes an acid. We have identified two distinct classes of star
individual monocrystalline domain, as seen in Fig. nanocrystals: multiple-twinned crystals with fivefold
6(b). However, a common defect for multiple- symmetry, and monocrystals, which correspond,
twinned stars is the presence of a twin boundary respectively, to icosahedra and cuboctahedra with
within a pyramid (Fig. 6(c)). Since each pyramid is a preferential growth of their
distinct crystalline domain, such defects typically
remain localized within one of the
20 pyramids. Fig. 6(d) is a TEM image of an
imperfect monocrystalline star. A stacking fault
extending through the entire crystal is evident in a
bright field image at higher-magnification (Fig. 6(e)).
The stacking fault is vividly illuminated in the
corresponding WBDF image (Fig. 6(f)).

Fig. 6. Characteristic defects for (a–c) multiple-twinned and (d–f) monocrystalline star polyhedral gold nanocrystals. (a) TEM image of an
imperfect multiple-twinned star. (b) HREM of a well-formed pyramid. (c) HREM of one of the two twin boundaries visible within the
neighboring pyramid. (d) TEM image of an imperfect monocrystalline star. (e) Bright field and (f) WBDF images clearly reveal a stacking
fault extending through the entire crystal.
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exposed {111} faces. In each case, the {111} faces of
the original Archimedean solid grow into tetrahedral
pyramids. By assuming a star morphology, gold
nanocrystals increase their proportion of exposed
{111} surfaces, and we propose that the accompanying
reduction in surface energy could be the driving force
behind star nanocrystal formation. In our synthesis, it
is exclusively ascorbic acid molecules and their
oxidized derivatives that stabilize and promote the
preferential growth of {111} surfaces, and our results
suggest that the role of ascorbic acid in promoting the
formation of branched gold nanocrystals is more
significant than has been appreciated to date.
Acknowledgments
This research is supported by Welch Foundation
Grant number F-1615. JLB thanks the
University of Texas at Austin College of Engineering
and Mr. Robert L. Mitchell for support through the
Thrust 2000 Robert L. and Jane G. Mitchell Endowed
Graduate Fellowship in Engineering. This material is
based upon work supported under a National Science
Foundation Graduate Research Fellowship (to JLB).
JLE acknowledges support received from CONACYT-
Me´ xico. We thank JEOL USA for facilitating SEM
analysis with the JSM 7401F, and undergraduate
researcher Luis Salazar for helping with the
nanocrystal synthesis.
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