NANO

LETTERS

Synthesis of Platinum Multipods: An xxxx

Vol. 0, No. 0
Induced Anisotropic Growth A-G

Xiaowei Teng† and Hong Yang*,†,‡

Department of Chemical Engineering and Laboratory for Laser Energetics, UniVersity

of Rochester, Rochester, New York 14627

Received February 17, 2005; Revised Manuscript Received March 25, 2005

ABSTRACT
This paper reports a highly effective synthesis of platinum multipods from platinum 2,4-pentanedionate in organic solvents. A trace amount
of silver acetylacetonate is used to trigger the nucleation and the anisotropic growth of Pt nanocrystals. The morphologies of Pt multipods
made include I- and V-shaped bipods, various types of tripods, and planar and three-dimensional (3D) tetrapods. The 3D Pt tetrapods can be
well-defined, resembling those observed for II−VI semiconducting materials, such as CdS and CdSe. Control of morphology and the multipod-
to-sphere transitions under various conditions have been systematically studied. A mode of formation based on the induced kinetically controlled
growth has been discussed.

Introduction. Development of nanometer scale branched
nanocrystals of metal,1-4 metal oxide,5-8 and semiconducting
materials9-14 is an important research subject that has
attracted a great deal of attention in recent years. In addition
to their intrinsic electronic, magnetic, photonic, and catalytic
properties, these branched nanomaterials have been proposed
to be used as building blocks for making complex nano-
structures through self-assembly processes.15 Such structures
are directly relevant to the fabrication of multiple-terminal
nanodevices and as active components in new photovoltaic
devices.16,17 Multipods such as 3D tetrapod nanocrystals can
also have advantages in the generation of hierarchical
nanostructured network over their counterparts of nanorods,
nanowires, nanocubes, and nanoprisms.
Although well-defined tetrapods of CdSe and CdS have
been developed for several years,18,19 the metal multipod and
hyper-branched nanostructures have only recently been
explored intensively.1-4 So far the level of control in the
anisotropic growth of branched metal nanocrystals cannot
match that for the growth of well-defined tetrapods of
cadmium chalcogenides (Se and S).10,11 This phenomenon
may be due to the fact that most metals typically do not
have polymorphism. The condition for branched growth
based on the lattice match at the surfaces of two crystal types
(such as zinc blende and wurtzite) in nanocrystals of
cadmium chalcogenides can be hard to create for metal
nanocrystals through a homogeneous nucleation and growth
process, though it is possible. Only gold, platinum, and
rhodium have been shown to form branched metal nano-
* Corresponding author: E-mail: hongyang@che.rochester.edu, Tele-
phone: (585) 275-2110; Fax: (585) 273-1348.
† Department of Chemical Engineering.
‡ Laboratory for Laser Energetics.
10.1021/nl0503072 CCC: $30.25 © xxxx American Chemical Society
Published on Web 00/00/0000
crystals. Although the formation mechanism is not com-
pletely clear, it appears that use of proper capping reagents
such as cetyltrimethylammonium bromide (CTAB) and poly-
(vinylpyrrolidone) (PVP) is very important, but it is only
one of the prerequisites. The kinetic control of growth process
is also critically important. The tested strategies for promot-
ing the formation of metal multipods include homogeneous
seeded growth4 and heterogeneous growth on metal
plates.3 Xia and co-workers have also demonstrated that the
addition of NaNO3 could promote the formation of Pt
octapods and tetrapods in a polyol process.1 We noted that
the length of the branches was rather short in these cases.
The branches were either not well defined or in a cone shape
rather than straight rods, which could be related to the growth
direction.
In this report, we present a synthetic method for making
Pt multipods through an induced anisotropic growth process
at temperatures below that for the homogeneous nucleation
and growth of Pt nanoparticles from platinum 2,4-pentanedi-
onate (Pt(acac)2). A small amount of silver acetylacetonate
(Ag(acac)) was used to trigger the formation of branched Pt
nanocrystal, as this silver precursor could readily decompose
and be reduced to form colloidal metal clusters at < 200
°C.
Experimental Section. In a typical synthesis, a mixture
of 1, 2-hexadecanediol (Aldrich, 90%, 800 mg), Pt(acac)2
(Gelest Inc., 200 mg), diphenyl ether (Aldrich, 99%, 2 mL),
hexadecylamine (HDA, Aldrich, 90%, 4 g), and 1,2-
adamantanecarboxylic acid (ACA, Aldrich, 99%, 180 mg)
was added into a 25 mL, three-neck, round-bottom flask
under argon protection. The reaction mixture was heated and
held at the designed temperature using a glycerol bath. The
PAGE EST: 6.2
temperature of this oil bath was monitored by Chemglass
ETC temperature controller. A small amount of Ag(acac)
(Aldrich, 99%, 3 mg) was then quickly added into the flask,
which resulted in a rapid formation of gray suspension,
indicating the formation of nanoparticles or multipods. The
color of the reaction mixture quickly turned into black. The
temperature could be maintained within ( 1 °C for the entire
reaction time period of 60 min. Aliquots of samples (∼200
µL) were taken every minute during the first 10 min to
monitor the growth kinetics. The concentrations of reagents
were fixed for all the synthesis, while the reaction temper-
atures were varied from 160 °C to 210 °C; unless indicated
otherwise. For those secondary injection experiments, a total
amount of 2.5 mL of reactant mixture (100 mg of HDA,
100 mg of Pt(acac)2, 100 mg of ACA, and 100 mg of 1,2-
hexadecanediol in 1 mL of diphenyl ether) was preheated
to 170 °C. Three equal aliquots (∼0.83 mL) of this mixture
were injected into the reaction flask at 7, 9, and 12 min after
the addition of Ag(acac).
After the reaction, the nanoparticles were washed and
separated using chloroform and ethanol. In a typical proce-
dure, a designed amount of the product (200 µL) was
dispersed in 800 µL chloroform in a small vial (2 mL),
followed by the addition of 1 mL ethanol to induce the
precipitation of nanoparticles. The precipitates were separated
from the solvent mixtures by centrifuge at 5000 rpm for 5
min. Yellow-brownish supernatant was decanted and the
black products were recovered by dispersing in 1 mL of
chloroform. This process was followed by a second wash
and separation using 1 mL of ethanol. The final products
were stored in chloroform.
Transmission electron microscopy (TEM) specimens were
prepared by dispersing the samples of nanocrystal in
chloroform (∼1 mg/mL) and drop-cast onto carbon-coated
copper grids. An ultrahigh vacuum scanning transmission
electron microscope (UHV-STEM, Cornell VG HB501) and
a regular TEM (JEOL 2000 EX) were used to examine the
size and shape of the nanoparticles. The UHV-STEM was
also used to conduct the energy-dispersive X-ray (EDX)
analysis and nanoelectron diffraction (ED) of individual
nanoparticles. The electronic gun of this STEM system could
be focused into a spot with a diameter of less than 1 nm.
The lattice fringes of Pt multipods were examined on a
Hitachi HD-2000 STEM operating in ultra-high resolution
mode at 200 kV and 30 mA. Powder X-ray diffraction
(PXRD) spectra were recorded on a Philips MPD diffrac-
tometer with a Cu KR X-ray source (λ ) 1.5405 Å) at a
scan rate of 0.015 2θ/s. Details of the characterization
methods could be found elsewhere.20, 21
Results and Discussion. The temperature for the forma-
tion of Pt nanoparticles from Pt(acac)2 via a homogeneous
nucleation and growth process was g ∼210 °C using the
reaction mixture described above. This reaction temperature
was similar to those reported for such systems.22 It is known
that various silver salts can be reduced to silver metal readily
through different pathways. We chose silver salt as the
reagent to induce nucleation and growth of Pt nanocrystals
from Pt(acac)2 at temperatures below 210 °C. Ag(acac) was
B Nano Lett.
used in this work because of its good solubility in organic
solvents, such as diphenyl ether. The evolution of Pt
multipods and nanoparticles was followed by TEM.
Figure 1 shows a series of TEM images of Pt nanoparticles
obtained at 180 °C for reaction times ranging from 4.5 to
60 min after a tiny amount of Ag(acac) was added into the
flask. At the initial stage, largely faceted rather than spherical
nanocrystals began to appear at 4.5 min after adding the silver
precursor, Figure 1a. Although some morphologies resembled
those that were previously observed for Pt nanoparticles,23
the embryonic forms of various multipods began to develop.
The population of multipods nevertheless was rather low at
this stage. These nanocrystals grew rapidly into multipods
within the next minute, which was indicated by the rapid
change of color from brown to black. A large area of
multipods with several different shapes was observed, Figure
1b. The various morphologies included triangular nano-
prisms; I- and V-shaped bipods; regular, T- and Y-shaped
tripods; and planar and 3D tetrapods. As the reaction
continued, the growth along the branch directions became
obvious, Figure 1c and 1d. The overall length-to-width aspect
ratio of the branches in Figure 1c and 1d was visibly higher
than those in Figure 1b, while the diameter of branches was
relatively constant. There were no obvious spherical Pt
nanoparticles. This observation was very different from the
Au multipods formed on Ag plates, which contained ∼40%
spherical nanoparticles.2 The rod-like shape of the branches
was also different from those Pt tetrapods and octapods made
in the polyol process through the addition of NaNO3 in that
these tetrapods were fully developed.1 After reaction for ∼10
min, no distinct growth along the branch direction was
observed; while the width of each branch began to increase,
Figure 1e, followed by a continuous disappearance of
multipods. The multipods turned into rice-shaped particles
with the dissolution and growth process, Figure 1f and 1g.
Upon 40 min after adding the silver precursor, multipods
evolved into spherical nanoparticles, Figure 1h. The size
distribution of nanoparticles became relatively monodisperse
at the reaction time of 60 min and no further morphology
change was observed, Figure 1i. This shape evolution
suggested that the formation of multipods should be a
kinetically controlled growth and the thermodynamically
stable shape of nanocrystals should be spherical.
Figure 2 showed PXRD and EDX spectra of Pt multipods.
All the X-ray diffraction peaks could be assigned to face-
centered cubic (fcc) platinum (space group: Fm3m). No
diffraction signal from silver could be observed. EDX was
used to analyze the chemical composition of individual
multipods. The observed EDX peaks at 2.1, 9.4, and 11.1
keV could be assigned to Pt M, LR, and Lβ lines, respectively.
The peaks at 8.0 and 8.9 keV could be assigned to the copper
KR and Kβ lines, respectively, which were from the substrate.
No silver signal could be detected. These data indicated that
the multipods were made of metallic platinum.
The structure details of multipods were analyzed by
nanoelectron diffraction using the UHV-STEM. Figure 3
shows the dark and bright field TEM images of a V-shaped
bipod, a regular 120° tripod, and a 3D tetrapod. As discussed
Figure 1. TEM images of Pt particles synthesized at 180 °C for (a) 4.5, (b) 5.5, (c) 7.5, (d) 9.0, (e) 12, (f) 15, (g) 20, (h) 40, and (i) 60
min after Ag(acac) was added. All scale bars are 20 nm.

above, there were variations of bipods, tripods, and tetrapods.

The two-branched structures could exist at different angles
and subsequently lead to diverse forms, ranging from
V-shaped bipods, Figure 2b, to almost straight I-shaped rods.
For the tripods, different branches tended to have similar
length but could also have a different aspect ratio for each
branch in the same tripod. The angles between neighboring
branches could also change from close to 180° in a T-shaped
tripod to 120° or less. The ED images taken at the tip region
of each branch of the tetrapod were shown as insets of Figure
3d. By calculating the length ratio from the center spots to
the adjacent spots, we obtained the zone axes of the
branches,24 which were [111] axes. The high-resolution TEM
image shows the V-shaped Pt bipod is single crystalline,
Figure 4. The measured d spacing corresponded to 2.2 Å
(or 2.2 nm for 10 consecutive lattice fringes), which could
be assigned to the (111) plane. These results indicated that
the growth of the branches was along 〈110〉 directions.
It has been reported that the formation of metallic
multipods and controlled platonic shapes could be associated
with the competitive growth between (111) and (100)
planes.1,2,25 In the case of formation of gold tripods and planar
tetrapods in aqueous solution using pre-synthesized silver Figure 2. PXRD (top) and EDX (bottom) spectra of Pt multipods.
plates as seeds,2 the growth was preferentially inhibited on The samples used were synthesized at 180 °C for 9 min after the
(111) planes, and the particles ended up with cube shapes addition of Ag(acac).
Nano Lett. C
Figure 3. (a) Dark and (b-d) bright field UHV-STEM images of Pt multipods synthesized at 180 °C. The insets show the nanodiffraction
patterns used to determine the crystallographic direction (zone axis) of each branch. The 10 nm scale bars apply to all images.

Pt nanocrystals triggered by the trace amount of silver could

Figure 4. High-resolution TEM image of a V-shaped Pt bipod
showing the (111) lattice fringes. The labeled length is for 10
repeating fringes.
showing the (100) planes. On the other hand, when growth
on (100) planes was inhibited, the resultant particles termi-
nated by the (111) faces. When growth on both (111) and
(100) planes was inhibited, (110) planes were dominant,
which led to the formation of tripods. Under our synthetic
conditions, the formation mechanism of Pt multipods ap-
peared to agree with those for Au multipods.
In the presence of surfactants, differences in the adsorption
of surfactants on the various crystal planes led to the
competitive growth. In our case, It seems that the branches
grew preferentially along 〈110〉 directions. This could not
be explained entirely by the steric hindrance in the case for
typical Au and Pt nanoparticles.1-3,23,26-28 The formation of
play an important role in directing the preferential growth
along a particular crystallographic direction. Although no
silver could be detected in the Pt multipods, we noted no
multipod formation without using silver precursors. In
addition, the Ag seeds have been used in the synthesis of
different metal particles.2,28-30 Addition of Ag(acac) into hot
organic solvent led to the formation of silver clusters that
promoted the Pt precursors decomposition and growth of Pt
on the low-index planes. These Ag clusters could contain as
few as four atoms.30 This seeded growth process allowed
the Pt nanocrystal to form below the nucleation and growth
temperature in the absence of silver species, which was
experimentally determined to be about 210 °C in our reaction
system. The growth kinetics could differ among the various
low-index planes.
Reaction temperature was another important parameter for
the kinetically controlled process, thus one would expected
it could affect the shape evolution of Pt nanocrystals. Figure
5 shows the typical TEM images of Pt nanoparticles obtained
at various times between 3.5 and 20 min after Ag(acac) was
added for the reactions conducted at 190 and 200 °C,
respectively. The TEM data showed that the shape evolution
from Pt multipods to spheres had a trend similar to those
reactions conducted at 180 °C. The optimal reaction times
for the formation of high population and well-defined
multipods were different from those formed at 180 °C. Large
populations of multipods appeared as early as 3.5 min after
the silver precursor added at 190 °C. The multipods began
to turn into spheres at ∼12 min. For those formed at 200

Figure 5. TEM images of Pt multipods and nanoparticles synthesized at (a-e) 190 and (f-j) 200 °C after the addition of Ag(acac) for
given periods of times: (a, f) 3.5, (b, g) 5.5, (c, h) 7.5, (d, i) 12, and (e, j) 20 min. All scale bars are 20 nm.
D Nano Lett.

Figure 6. Effect of temperature on the shape of Pt nanoparticles
and multipods. No Ag(acac) was added for reaction conducted at
210 °C, as particles formed spontaneously at this temperature.
°C, Pt multipods began to change their shapes as early as
∼7.5 min after the silver precursor was added. These results
indicated that anisotropic growth disappeared at an earlier
time with the increase of reaction temperature.
A wide range of reaction times and temperatures was
examined, and the results are summarized in Figure 6. The
classification of shapes for each data point shown in this
figure was based on a series of TEM studies. Three distinct
regimes were observed for these reaction systems at the
different temperatures, i.e., no particles, multipods, and
spheres. No Pt particles formed for the entire reaction period
up to 60 min, when the reaction temperatures were between
160 and 175 °C. Multipods were formed at 2.5 to 4.5 min
after the addition of Ag(acac) for the reactions conducted
between 180 and 200 °C. The multipods disappeared and
turned into spheres after reacting for additional 10 to 15 min.
The higher the reaction temperatures were, the earlier the Pt
multipods formed and the sooner they evolved into spheres.
We noted that the temperatures used to synthesize Pt particles
were lower than that for the decomposition of Pt(acac)2 in
the presence of HDA and ACA, which began at 210-220
Figure 7. TEM images showing the shape evolution of Pt multipods and nanoparticles after multiple secondary injections of reaction
mixtures at 180 °C. The TEM images were taken at (a) 7.0, (b) 8.5, (c) 11, (d) 15, (e) 20, (f) 30, (g) 40, and (h) 60 min, respectively. A
mixture of HDA (100 mg), Pt(acac)2 (100 mg), ACA (100 mg), 1,2-hexadecanediol (100 mg), and diphenyl ether (1 mL) was preheated to
170 °C and injected into the reaction flask in three equal aliquots at 7, 9, and 12 min after the reaction, respectively. All scale bars are 20
nm.
Nano Lett.
°C.22 It was plausible that silver might work not only to
induce the formation of nucleation seeds2,28-30 but also to
function as catalysts to facilitate the formation of Pt particles
below the decomposition temperature of Pt(acac)2. Recently,
Song et al. reported the synthesis of platonic shapes of Pt
nanoparticles with the addition of Ag precursors.28 Silver
species such as Ag42+ could adsorb on (100) planes of Pt
particles and promote the reduction of Pt salts preferentially
on (100) planes that adsorbed these Ag species continuously.
Further experiments are needed to determine if this mode
of formation is reasonable in our system.
The transitions from multipods to spherical nanoparticles
could be interpreted by the Ostwald ripening.31 In these cases,
there was a critical size at the equilibrium state.10,22,31 Particles
that were smaller than the critical size dissolved while the
large ones continued to grow. At the early stages after
nucleation, the kinetic growth governed the shapes of Pt
particles, resulting in multipod structures. When the monomer
depleted, the ripening process became dominant. The branches
of multipods began to dissolve, subsequently resulting in the
formation of spherical particles at relatively large diameters.
A thermodynamically controlled process should be favored
when thermal energy is sufficiently high. Particles tend to
minimize the surface energy through the transformation from
the highly faceted multipods to spheres that possess lower
specific surface area than multipods. The temperature-
dependent transitions observed in our results could be
interpreted by this formation mechanism.
We further investigated if the addition of Pt(acac)2 at the
various stages of the reaction could prolong the growth of
multipods. A reaction mixture with total amount of 100 mg
of Pt(acac)2 was injected into the reaction flask in three equal
aliquots at 7, 9, and 12 min, respectively, after the addition
of Ag(acac). To minimize the formation of new nuclei during
the secondary injections, less than 40% of the existing
reaction precursor was suggested in each addition.32 In our
case, each aliquot was equal to ∼17% of the total amount
E
Figure 8. TEM images showing the effect of Pt(acac)2 amount on the formation of Pt multipods. The amounts of Pt(acac)2 used were (a)
50, (b) 100, and (c) 200 mg, respectively. All scale bars are 20 nm.
of Pt(acac)2 in the reaction flask prior to the secondary
injection. Figure 7 shows the TEM images of Pt nanocrystals
synthesized at 180 °C for the reaction time periods of 7 (prior
to the first time of secondary injection), 8.5, 11, 15, 20, 30,
40, and 60 min, respectively. Our results indicated that the
growth process of multipods could be extended using the
multiple injection approach, and the transition time from
multipods to spherical particles changed to 30 min after the
initial addition of Ag(acac). Some multipods could still be
observed, even when the reaction time reached 60 min. In
comparison, without the multiple injection, the multipod-
to-sphere transition happened at ∼20 min after the initial
addition of Ag(acac).
The effect of the amount of Pt(acac)2 used on the shape
evolution of particles was also investigated. Pt(acac)2 precur-
sor at 50-, 100-, and 200-mg levels was chosen in these
experiments. Reactions were conducted at 190 °C for 5 min
after the addition of Ag(acac). Our TEM study shows that
at the low precursor concentration, spherical Pt particles were
predominant, Figure 8. At the intermediate precursor con-
centration, elongated nanoparticles and multipods with low-
aspect ratio branches formed. We noted that the Pt nano-
crystals formed using 100 mg Pt(acac)2 contained multipods
that resembled some of the morphologies previously ob-
served,1 suggesting that full growth of rod-like branched
multipods may be achievable in the polyol process with
the proper control of reactant molar ratio and reaction
condition.
Conclusion. Addition of a trace amount of Ag(acac) can
trigger the nucleation and growth of Pt nanoparticles at
temperatures below that for the homogeneous reaction. The
relatively low reaction temperatures also favor the kinetically
controlled anisotropic growth of platinum in the presence
of surfactants. This induced growth leads to the formation
of a high-population of Pt multipods. Unlike the cases
reported previously, the Pt tetrapods made in this work are
well-defined, resembling those observed for II-VI quantum
dots of CdS and CdSe. We believe the approach developed
in this work can be an effective method to make multipods
of different metals under appropriate conditions. These Pt
multipods may be used as new nanoscale building blocks
for making complex functional nanostructures through self-
assembly.15
Acknowledgment. This work is supported in part by U.S.
NSF (CAREER Award, DMR-0449849 and SGER Grant,
F Nano Lett.
CTS-041722), the DOE through LLE (DE-FC03-92SF19460),
and the subcontract of a MURI Grant from DoD (FA9550-
04-1-0430). This work made use of the Shared Experimental
Facilities at the Cornell Center for Materials research
(CCMR) supported by NSF and the Hitachi HD-2000 STEM
at the Centre for Nanostructure Imaging, University of
Toronto, funded by Canada Foundation of Innovation and
Ontario Innovation Trust. We are grateful to LLE for a
Horton Fellowship (X.T.). We thank Drs. Mick Thomas
(Cornell University) and Marc Mamak (University of Tor-
onto) for running the high resolution TEM. The support of
DOE does not constitute an endorsement by DOE of the
views expressed in this article.
Note Added after ASAP Publication. Text phrase II-IV
was corrected to II-VI in the Abstract and Conclusions. This
paper was published ASAP on 4/9/05. The corrected version
was reposted on 4/13/05.
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