J. Phys. Chem.

B 2006, 110, 6543-6548 6543

Controlled Synthesis of High-Quality PbS Star-Shaped Dendrites, Multipods, Truncated

Nanocubes, and Nanocubes and Their Shape Evolution Process

Guangjun Zhou, Mengkai Lu1 ,* Zhiliang Xiu, Shufen Wang, Haiping Zhang,
Yuanyuan Zhou, and Shumei Wang
State Key Laboratory of Crystal Materials, Shandong UniVersity, Jinan 250100, P.R. China
ReceiVed: September 3, 2005; In Final Form: January 25, 2006

Well-defined single-crystalline PbS nano- and microstructures including dendrites, multipods, truncated
nanocubes, and nanocubes were synthesized in high yield by a simple solution route. Novel star-shaped PbS
dendrites with six symmetric arms along the 100 direction, each of which shows one trunk (long axis) and
four branches (short axes), have been achieved using Pb(AC)2 and thioacetamide (TAA) as precursors, under
the molar ratio Pb(AC)2/TAA ) 2/1, at initial reaction temperature 80 C, refluxing for 30 min at 100 C, in
the presence of cetyltrimethylammonium bromine (CTAB). The nanorods in each branch are parallel to
each other in the same plane and are perpendicular to the trunk. The truncated nanocubes mainly bounded by
the {100} plane were prepared under a different Pb(AC)2/TAA molar ratio, at initial reaction temperature 40
C, refluxing for 12 h at 100 C. Based on the systematic studies on their shape evolution, a possible growth
mechanism of these PbS nano- and microstructures was proposed. The shapes of PbS nanocrystals with face-
centered cubic (fcc) structure are mainly determined by the ratio (R) between the growth rates along the
100 and 111 directions. The Pb(AC)2/TAA molar ratio and the initial reaction temperature influence the
growth ratio R in the formation of PbS nuclei at an early stage, which results in the final morphology of PbS
nanocrystals. Under the current experimental conditions, we can control the PbS shape evolution by simply
tuning the molar ratio, the initial reaction temperature, and the period of reaction. Based on the systematic
studies on the shape evolution, this approach is expected to be employed for the control-shaped synthesis of
other fcc structural semiconductor nanomaterials. The photoluminescence properties were investigated and
the prepared nano- and microstructures displayed a very strong luminescence around 600-650 nm at room
temperature.

1. Introduction which means it should be useful on optical devices such as

Nanometer-scale materials have attracted considerable interest
in recent years due to their unique physical and chemical
properties and potential applications in nanoscale devices.1-6
It is well-known that the shape and size of nanocrystals have
much influence on their widely varying properties. The archi-
tectural control of nanosized materials with well-defined shape
is important for the success of bottom-up approaches toward
future nanodevices. In the past decades, there has been an
increasing number of excellent studies on novel nanostructural
materials with various shapes, such as nanorods,7-9,42 nano-
cubes,10-15 nanobelts,16-18 nanowires,19-22,43 nanofibers,23-26
nanotubes,27-30 and dendrites.31-34 The ability to understand and
predict the final architecture of nanoscale building blocks is
still limited. If we understand the growth mechanism and the
shape-guiding process, it will be possible to program the system
to yield the building blocks with desired shape and crystallinity.
Semiconductor nanostructures have outstanding electronic and
optical properties and are useful on nanodevices such as light-
emitting diodes,35 single-electron transistors,36 and infrared
detectors.37 As one of the semiconductor compounds, PbS is
an important - semiconductor material with a narrow band
gap energy and large excition Bohr radius.38 Moreover, quantum-
size PbS has exceptional third-order nonlinear optical properties,
* Corresponding author. Fax: +86-531-88565403. E-mail: mklu@
icm.sdu.edu.cn.
10.1021/jp0549881 CCC: $33.50 2006 American Chemical Society
Published on Web 02/18/2006
optical switches.39 PbS quantum dots with stable efficient
luminescence in the near-IR spectral range has potential
application in communication, biological imaging, and infrared
photodetector.40 PbS nanocrystals with various morphologies
has been achieved. For example, cubic-shaped PbS microcrystals
and nanocrystals have been produced by the decomposition of
a single-source precursor.41 Rodlike PbS nanocrystals have been
obtained using a combination of surfactant and polymer matrix
as a template.42 PbS nanowires as well as nanosheets have been
prepared by a polymer-assisted solvothermal method.43,44 Rod-
based PbS multipods were synthesized from the thermal
decomposition of a molecular precursor.45 Star-shaped PbS
microcrystals with eight symmetric arms along the 111
direction have been formed by an aqueous phase route.46,47
Dendrites have recently attracted much attention due to the
interesting morphology, properties, and potential applications.
Dendritic nanostructures of semiconductor compounds are one
type of attractive supramolecular structures.33,48,49 In this paper,
novel star-shaped PbS dendrites with six symmetric arms along
the 100 direction, multipods, truncated nanocubes, and
nanocubes were prepared in high yield via a simple surfactant-
assisted route in the presence of CTAB under different reaction
conditions, respectively. The shapes of PbS nanocrystals evolved
from metastable star-shaped multipods as a transient species to
stable truncated nanocubes. The growth mechanism of the PbS
nano- and microstructures was proposed. As a mode study for
6544 J. Phys. Chem. B, Vol. 110, No. 13, 2006 Zhou et al.

the shape-guiding strategy, we present a rational synthetic

scheme that yields novel architectures of semiconductor nano-
crystals. Simultaneously, we elucidated the specific role of
important growth parameters for shape determinations. These
results establish that it is possible to control the morphology of
semiconductor nanocrystals using solution chemistry, which has
important implications for both fundamental scientific studies
and future technological application.

2. Experimental Section
Preparation of PbS Dendrites. All the reagents were
purchased from Shanghai Chemistry Co. with analytical-grade
purity and were used without further purification. The synthesis
of PbS products was carried out by the thermal decomposition
of thioacetamide (TAA) in aqueous solution of lead acetate at
suitable initial reaction temperature and period of reflux in the
presence of surfactant. In a typical experiment, 6 mmol of
Pb(AC)2 and 3 g of CTAB were dissolved in 80 mL of deionized
water in a three-necked flask equipped with a condenser. The
mixtures were then heated to 80 C under continuous vigorous
stirring. Twenty milliliters of 3 mmol of thioacetamide (TAA)
solution was added dropwise to the above solution at 80 C
(initial reaction temperature), up to the final concentrations of
0.06 mol/L Pb(AC)2 and 0.03 mol/L TAA, and the mole ratio
of Pb(AC)2/TAA of 2/1. The color of the reaction mixture
changed to black slowly in the dropwise procedure. When the
addition of TAA was completed, the reaction mixture was heated
to 100 C and refluxed for 30 min. The resulting black products
were separated by centrifugation at 3500 rpm for 20 min, washed
several times with water and ethanol, and then dried at 60 C
for 5 h in a vacuum-dryer. Figure 1. (a) Low- and (b) high-magnification SEM images of star-
Characterization of Samples. The X-ray diffraction (XRD) shaped PbS dendrites with six arms along 100 directions synthesized
under the molar ratio Pb(AC)2/TAA ) 2/1, the concentrations of
patterns were recorded using a Rigaku D/Max 2200PC diffrac-
Pb(AC)2 and TAA of 0.06 and 0.03 mol/L, respectively, and initial
tometer with graphite monochromatized Cu KR irradiation reaction temperature 80 C, with refluxing for 30 min at 100 C, in
( ) 1.5418 ). Transmission electron microscopy (TEM) the presence of 3 g of CTAB/100 mL.
images were carried out using a JEM-100CX2 transmission
electron microscope. Scanning electron microscopy (SEM)
the higher magnification SEM image of mono-arm dendrites
images were measured on a JEOL JSM-6700f scanning electron
(Figure 2c), it can be clearly seen that the nanorods
microscope. Emission spectra were measured on an Hitachi 850
perpendicular to the trunk in the branches have complex delicate
fluorescence spectrophotometer. All the measurements were
structures with one smaller trunk and four smaller branches.
carried out at room temperature.
Influence of the Pb(AC)2/TAA Molar Ratio and the Initial
Reaction Temperature on the PbS Morphologies. The
3. Results and Discussion
morphology of the PbS nano- and microcrystals depends on
Morphology and Nanostructure of PbS Dendrites. The the concentrations of reagents, surfactant, molar ratio of
morphologies and structures of the products have been inves- precursor, synthesis temperature, and time. All the parameters
tigated by SEM and TEM. Well-defined, star-shaped PbS were found to be interdependent, thus resulting in PbS nano-
dendrites (Figure 1a and 1b) were synthesized as described in and microcrystals with various morphologies. Among the
the Experimental Section, using Pb(AC)2 and TAA as precur- various parameters, the Pb(AC)2/TAA molar ratio and the initial
sors, the molar ratio being controlled at Pb(AC)2/TAA ) 2/1 reaction temperature are particularly crucial for the control of
and the initial reaction temperature at 80 C, and refluxed for both the morphology and the size of PbS nano- and microc-
30 min at 100 C, in the presence of 3 g of CTAB/100 mL. rystals. To investigate the influence of the Pb(AC)2/TAA molar
Indeed, the yield of this structure is very high, and almost all ratio and the initial reaction temperature on the PbS morphology,
of the crystals are six-arm star-shaped dendritic nanostructures. a series of separate experiments were carried out by changing
The typical SEM of individual PbS dendrite (insert in Figure the molar ratio from 2/1 to 1/1 and 1/3 and the initial reaction
1b) shows a clear view of its three-dimensional (3D) structure temperature from 80 C to 35, 40, 50, 60, and 100 C,
with six symmetric arms that grow along 100 directions. Each respectively, under conditions of fixed refluxing time (30 min).
arm has one trunk (long axis) and four branches (short axes). The morphologies of PbS nano- and microcrystals prepared
The nanorods in each branch are parallel to each other and under various Pb(AC)2/TAA molar ratios at different initial
in the same plane and are perpendicular to the trunk. reaction temperatures are shown in Table 1. It can be seen from
Moreover, there is an interesting phenomenon that the Table 1 that all the products were dendrites when the molar
junction of the six symmetry arms is broken by a 20 min ratio was 2/1 at various initial reaction temperatures. When the
ultrasonic wave of irradiation (45 W). All the star-shaped Pb(AC)2/TAA molar ratio was changed to 1/1, the final products
structures disband and the dispersed mono-arm dendrites are were PbS dendrites only when the initial reaction temperature
then present in the products as shown in Figure 2a and 2b. From was above 60 C. When the Pb(AC)2/TAA molar ratio was
Controlled Synthesis of High-Quality PbS J. Phys. Chem. B, Vol. 110, No. 13, 2006 6545

Figure 2. (a) SEM and (b) TEM images of mono-arm dendrites prepared by 20 min ultrasonic wave of irradiation. (c) Higher magnification SEM
images of the mono-arm dendrites.

TABLE 1: Influence of the Pb(AC)2/TAA Molar Ratio and the Initial Reaction Temperature on the PbS Morphologies
molar ratio initial reaction temperature
Pb(AC)2/TAA 35 C 40 C 50 C 60 C 80 C 100 C
2/1a dendrites dendrites dendrites dendrites dendrites dendrites
1/1b multipods multipods nanoparticles dendrites dendrites dendrites
1/3c multipods multipods multipods nanoparticles dendrites dendrites
a-c
The final concentrations: a[Pb(AC)2] ) 0.06 mol/L, [TAA] ) 0.03 mol/L; b[Pb(AC)2] ) 0.03 mol/L, [TAA] ) 0.03 mol/L; c[Pb(AC)2] )
0.03 mol/L, [TAA] ) 0.09 mol/L; refluxed for 30 min at 100 C, in the presence of 3 g of CTAB/100 mL.

Figure 3. TEM images of the PbS nanostructures obtained under various initial reaction temperatures: (a) 35, (b) 40, (c) 50, (d) 60, (e) 80, and
(f) 100 C. The molar ratio of Pb(AC)2/TAA ) 1/1 and the concentrations of Pb(AC)2 and TAA are 0.03 and 0.03 mol/L, respectively, with
refluxing for 30 min at 100 C, in the presence of 3 g of CTAB/100 mL.

changed to 1/3, the PbS dendrites were obtained while the initial
reaction temperature was above 80 C. If the initial reaction
temperature was decreased to 60 C, only nearly spherically
nanoparticles could be achieved. If the initial reaction temper-
ature was decreased to 50, 40, and 35 C, respectively, only
star-shaped multipod nanocrystals could be obtained.
Figure 3 shows the TEM images of the PbS nanostructures
obtained under a different initial reaction temperature, the molar
ratio Pb(AC)2/TAA ) 1/1, and refluxed for 30 min at 100 C
in the presence of 3 g of CTAB/100 mL. When the initial
reaction temperature was fixed at 35 and 40 C, respectively,
the star-shaped PbS multipod nanocrystals were formed (Figure
3a and 3b). However, when the initial reaction temperature was
increased to 50 C, the nearly spherically PbS nanoparticles were
formed (Figure 3c). When the initial reaction temperature was
fixed at 60 C, the dendritic structures were achieved (Figure
3d). When the initial reaction temperature was increased to 80
and 100 C, respectively, the morphology and size of the PbS
dendrites did not show significant change (Figure 3e and 3f).
Morphological Evolution Process of the PbS Nanocrystals.
To investigate the morphological evolution process of the PbS
nanocrystals, the molar ratio of Pb(AC)2/TAA was fixed at 1/3
and the initial reaction temperature was fixed at 40 C under
the same other reaction conditions. Refluxed time was changed
from 10 min to 30 min, 2 h, 5 h, and 12 h; a variety of PbS
nanocrystals including star-shaped multipods (Figure 4a and 4b),
nanoparticles (Figure 4c), and truncated nanocubes (Figure 4d
and 4e) were obtained. Figure 4 indicated clearly the evolution
process of the PbS nanocrystals by varying the refluxed time.
Figure 5a shows the SEM images of the truncated nanocubes
(the same samples in Figure 4e). It is clearly seen that the large
quantity of nanocrystals have a smooth surface and almost all
corners and edges of these nanocubes were slightly truncated.
The edge length of these truncated nanocubes are about 70-80
nm. Figure 5b shows the SEM image of individual slightly
truncated nanocubes sitting on the silicon substrate against one
of its square/hexagon facets, indicating that the slightly truncated
nanocubes were bounded mainly by {100} facets. Figure 5c
6546 J. Phys. Chem. B, Vol. 110, No. 13, 2006
Figure 4. Morphological evolution process of the PbS nanocubes:
TEM images of the samples synthesized at initial reaction temperature
40 C, under different refluxing times of (a) 10 min, (b) 30 min, (c) 2
h, (d) 5 h, and (e) 12 h. The molar ratio of Pb(AC)2/TAA ) 1/3 and
the concentrations of Pb(AC)2 and TAA are 0.03 and 0.09 mol/L,
respectively, in the presence of 3 g of CTAB/100 mL.
shows the SEM image of individual truncated nanocubes sitting
on the silicon substrate against one of its triangular facets,
illustrating the high symmetry of these nanocubes. It is clearly
seen from Figures 5b and 5c that the truncated nanocube is a
single crystal, with its square/hexagon facets being indexed to
{100} planes and triangular ones to {111} plane.
Formation of PbS Nanocubes. To explore the influence of
the different sulfur ion sources and surfactant on the morphology
of PbS crystals under the same experimental conditions, the
following experiments were performed. First, we employed
thiourea instead of TAA as a sulfur ion source, at an initial
reaction temperature of 40 C and refluxing for 12 h at 100 C
in the presence of CTAB. PbS macrocrystals were obtained
(Figure S1a). Second, we employed 3 g of the polymer poly-
(vinylpyrrolidone) (MW ) 30000) (PVP) instead of 3 g of
Figure 5. (a) SEM images of truncated PbS nanocubes synthesized at initial reaction temperature 40 C, with refluxing for 12 h at 100 C and the
molar ratio of Pb(AC)2/TAA ) 1/3, in the presence of 3 g of CTAB/100 mL. (b) High-magnification SEM image of a slightly truncated PbS
nanocube sitting on the silicon substrate against one of its square/hexagon facets. (c) High-magnification SEM image of a truncated PbS nanocube
sitting on the silicon substrate against one of its triangular facets.
Zhou et al.
CTAB, using TAA as a sulfur source. Only irregular nanopar-
ticles were observed (Figure S1b in the Supporting Information).
However, when these two parameters were varied simulta-
neously, using an equal mole of thiourea instead of TAA as
precursor, and equal polymer PVP instead of surfactant CTAB
as capping regent and under the same reaction conditions, the
PbS nanocubes were exclusively formed as shown in Figure 6.
In addition, the concentration of CTAB is also an important
factor in the formation of PbS nanocrystals. When no surfactant
was introduced, only irregular nanoparticles were formed (Figure
S2a and S2c in the Supporting Information). When the
concentration of CTAB was decreased to 1 g/100 mL in the
reaction solution, the bigger cubes (Figure S2b in the Supporting
Information) with about 200 nm edge length were obtained at
the initial temperature 40 C and refluxed for 12 h at 100 C,
and no dendrites were formed (Figure S2d in the Supporting
Information) at the initial temperature 80 C and refluxing for
30 min at 100 C.
XRD Measurements and Photoluminescence Spectra. Both
the truncated nanocubes (the same samples in Figure 5a) and
star-shaped dendrites (the same samples in Figure 1a) were also
self-assembled on single-crystalline silicon wafers for powder
XRD characterization. Figure 7a,b presents the XRD patterns
recorded on these two samples, indicating that types of
nanocrystals present a well-defined fcc structure with the Fm3m
space group (a ) 5.936 ). For a comparison, the relative
intensities of the diffraction peaks from the standard card
(JCPDS file number 05-0592) were labeled on the bottom of
Figure 7 as well. In Figure 7a, it is worth noting that the ratio
between the intensities of (200) and (111) diffraction peaks is
higher than the conventional value (3.2 versus 1.2). This
indicates that the nanocubes abound in {100} facets, which are
consistent with the results from the SEM observation.
The room-temperature photoluminescence spectra of the
obtained PbS samples are shown in Figure 8. These spectra
exhibit different features depending on their morphological
variation. With the excitation wavelength of 495 nm, the
emission maximums of the photoluminescence spectra of the
obtained PbS samples are around 632 nm. The photolumines-
cence properties of nanocrystals are generally impacted by many
factors, such as nanoparticle shape, size, and size distribution.
In particular, the effect of lattice defect could not be ignored. It
is thought that the nanocubes with higher crystallinity have low
concentration of defects, which act as sites for nonradiative
recombination of electron-hole pairs.50 As a result, the emission
intensities of perfect nanocubes are stronger than those of
truncated nanocubes and star-shaped dendrites. The emission
Controlled Synthesis of High-Quality PbS
Figure 6. TEM images of PbS nanocubes synthesized using thiourea
as a precursor. The molar ratio of Pb(AC)2/thiourea ) 1/3 and the
concentrations of Pb(AC)2 and thiourea are 0.03 and 0.09 mol/L,
respectively, at initial reaction temperature 40 C, with refluxing for
12 h at 100 C, in the presence of 3 g of PVP/100 mL.
Figure 7. X-ray powder diffraction patterns of (a) truncated nanocubes
and (b) star-shaped dendrites.
Figure 8. Room-temperature photoluminescence spectra of PbS
samples with various morphologies: (a) irregular nanoparticles prepared
in the absence of surfactant, (b) star-shaped dendrites, (c) truncated
nanocubes, and (d) nanocubes prepared in the presence of surfactant.
intensities of the irregular nanocrystals obtained in the absence
of surfactant are weakest.
Mechanism of Fabrication. It is well-known that surface
energies associated with different crystallographic planes are
usually different, and a general sequence may hold, {111} <
{100} < {110}.51 The growth rates on different surface facets
are dominated by the surface energy. When a particle grows,
facets tend to the low-index planes to minimize the surface
energy. As illustrated by Z. L.Wang,51 the shape of an fcc
nanocrystal is mainly determined by the ratio (R) between the
growth rates along the 100 and 111 directions. Octahedra Y2003F08).
J. Phys. Chem. B, Vol. 110, No. 13, 2006 6547
bounded by the most stable {111} planes will be formed when
R ) 1.73, and perfect cubes bounded by the less stable {100}
planes will result if R is reduced to 0.58. For the truncated
nanocubes illustrated in Figure 5, the ratio R should have a value
close to 0.7-0.87. TAA was substituted by an equal mole of
thiourea as precursor, and CTAB was substituted by PVP as
capping regents. First, the growth of PbS crystals is weakened
when thiourea is used as a sulfur source. Second, PVP is a
nonionic surfactant and CTAB is a cation surfactant, so PVP is
a weak binding ligand to the PbS crystal. Since the formation
of the 2D nuclei on {111} faces has a low activation energy in
weakly binding capping molecules,52 growth on the {111} faces
is now favored and the R is reduced to about 0.58. Nanocubes
bound by the {100} plane were formed as shown in Figure 6.
When the initial reaction temperature was increased to 80 C,
the growth rates were accelerated. The difference between the
enhanced growth rates on the {100} and {111} planes induced
the ratio R to have a value of more than 1.73, which resulted in
the formation of the star-shaped dendrites as shown in Figure
1a and 1b.
Based on the systematic studies of varying growth parameter
and detailed structure, we have discovered the critical factor
for determining architectural features of the PbS nanocrystals.
The molar ratio of Pb(AC)2/TAA and the initial reaction
temperature have an influence on the growth ratio R in the
formation of PbS nuclei at an early stage, which results in the
final morphology of PbS nanocrystals. The molar ratio and the
initial reaction temperature play a key role in the formation of
PbS nanostructures. In other words, we can control the PbS
shape evolution by simply tuning the molar ratio and the initial
reaction temperature and the period of reaction. Not only can
the stable PbS nano- and microstructures such as truncated
nanocubes (Figure 4e and Figure 5) and six-arm star-shaped
dendrites (Figure 1) be obtained, but also the metastable
nanostructures such as star-shaped multipods nanocrystals
(Figure 3a, 3b and Figure 4a, 4b) and nearly spherically
nanoparticles (Figure 3c and Figure 4c) can be achieved under
the current experimental conditions. Although another type of
morphology of PbS nanocrystals, octahedron or truncated
octahedron, was not observed this time, we believe that it could
also be achieved under this experimental procedure by varying
the growth parameters. This work is currently in progress.
4. Conclusion
In summary, a simple solution process has been successfully
developed to prepare PbS nano- and microstructures with various
morphologies. Their shape evolution process and the influence
of the growth parameters on the growth ratio R have been
discussed. The desired architecture of building blocks such as
star-shaped dendrites and truncated nanocubes can be consis-
tently obtained by programming the growth parameters such
as the molar ratio, the initial reaction temperature, and period
of reaction. Based on the systematic studies on the shape
evolution, this approach is expected to be employed for the
control-shaped synthesis of other fcc structural semiconductor
nanomaterials. The photoluminescence properties were inves-
tigated and the prepared structures displayed a very strong
luminescence around 600-650 nm at room temperature. These
properties may be promising for applications in the fabrication
of photoelectric materials.
Acknowledgment. This work is supported by the awarded
funds of excellent state key laboratory (No. 50323006) and the
Natural Science Foundation of Shandong Province (No.
6548 J. Phys. Chem. B, Vol. 110, No. 13, 2006
Supporting Information Available: TEM images of the
PbS nano- and macrostructures synthesized under various initial
reaction temperature, precursor, and surfactant. This material
is available free of charge via the Internet at http://pubs.acs.org.
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