Journal of the Chinese Chemical Society, 2010, 57, 325-331 325

Finding a Facile Method to Synthesize Decahedral Silver Nanoparticles

through a Systematic Study of Temperature Effect on Photomediated
Silver Nanostructure Growth

Yao-Chang Lee ( ), Sin-Jia Chen ( ) and Cheng-Liang Huang* ( )

Department of Applied Chemistry, National Chiayi University, Chiayi City, Taiwan, R.O.C.

To the best of our knowledge, few reports have been concerned with the effect of temperature on
photomediated silver nanostructure growth. In this work, the shape evolution from spherical silver
nanoparticles to silver nanoprisms and nanostructures in other shapes under the irradiation of a sodium
lamp (lmax = 589 nm, 0.66 W/cm2) at various temperatures (i.e., 15, 40, 60, and 80 °C) were studied by re-
cording the TEM images and time-course UV-vis-NIR spectra of the silver colloids. From TEM and spec-
tra analysis, it was found that the photomediated silver nanoparticle shape conversion process would be
faster at a higher temperature, i.e., ca. 2 hours at 80 °C, and slower at a lower temperature, i.e., ca. 17 hours
at 15 °C. The silver nanoplates synthesized at a higher temperature had a narrower size distribution and
were thicker than those synthesized at a lower temperature. Some decahedral silver nanoparticles, about
10% of the final irradiation products, were observed in the synthesis (with a sodium lamp) at 15 °C. In or-
der to produce a higher yield of decahedral silver nanoparticles, the sodium lamp was replaced with blue
LEDs (lmax = 450 nm), which have a wavelength closer to the SPR of decahedral silver NPs (ca. 490 nm).
The decahedral silver nanoparticles with a fairly narrow size distribution were obtained by irradiating the
spherical nanoparticle colloids with the blue LEDs at 2 °C in the absence of PVP or other large-molecu-
lar-mass surfactants.

Keywords: Temperature; Silver nanoprism colloid; Decahedral silver nanoparticles; SPR.

1. INTRODUCTION chemical reaction tends to the formation of anisotropic

In recent years, noble metal nanoparticles have at-
tracted extensive interest mainly because of their potential
application in catalyst, 1 optical devices, 2 biological and
chemical sensors,3 and surface enhanced Raman spectros-
copy (SERS). 4-6 It is well known that the physical and
chemical properties of the nanostructures are highly de-
pendent on their sizes and shapes.1a,7 Therefore, tremen-
dous efforts have been devoted in morphology control to
successfully synthesize noble metal nanostructures with
various shapes such as spheres, 8 rods,9 boxes,10 shells,11
tetrahedrons,12 cubes,3,13 disks,14 wires,15 hexagons,16 bi-
pyramids,17 stars,18 prisms,19,20 and decahedra.21
It was found in previous studies that the shapes of
nanoparticles can be controlled through altering the ratio of
growth rates along different facets by the addition of sur-
factants, ions and capping agents.22 It was also found that
the wavelength, time and intensity of the light irradiation
can also affect the morphologies and size distribution of the
final products.23 Mirkin et al. have reported that the photo-
nanoparticles because the dipole plasmon excitation in-
duces ultrafast charge separation on the nanoparticle sur-
face, 23 leading to face-selective silver cation reduction,
while the random thermal reaction tends to the formation of
isotropic nanoparticles.23 Therefore, if one wants to obtain
nanostructures with particular shapes, one should enhance
the photochemical process relative to the thermal reaction
process. However, the silver colloidal solutions under
higher light intensities would have higher temperatures due
to the heating effect of light absorption and hence have a
more rapid thermal reaction. In order to control the ratio of
photochemical reaction to thermal reaction, we put the col-
loidal solution and the light source in a temperature-con-
trolled water-filled tank. The TEM images and time-de-
pendent UV-vis-NIR extinction spectra of the silver col-
loids in each batch with the same light intensity and differ-
ent water temperatures were recorded to monitor the shape
evolution of the silver nanoparticles. We found that the sur-
face plasmon resonance (SPR) signals in the extinction

* Corresponding author. E-mail: clhuang@mail.ncyu.edu.tw

326 J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010
spectra of spherical nanoparticles disappeared more rap-
idly at a higher temperature than at a lower temperature. It
indicates that the thermal reaction could speed up the shape
conversion process. We also found that the silver nano-
plates synthesized at a higher temperature were larger,
thicker, and more homogeneously distributed in size than
those at a lower temperature. It was also found that the syn-
thesis at a very low temperature, such as 15 °C, not only ex-
hibited a very slow shape conversion rate but also produced
nanostructures with divergent morphologies. A portion of
the products, about 10%, synthesized at this low tempera-
ture were decahedral in shape. Since the decahedral silver
nanoparticles have a shorter SPR wavelength than the sil-
ver nanoprisms and tend to be formed at lower tempera-
tures, we replaced the sodium lamp (589 nm) with blue
LEDs (450 ± 12 nm) and placed the spherical nanoparticle
colloids in the tank at a lower temperature, i.e., 2 °C. After
irradiation for ca. 48 hours, we obtained the high-yield and
PVP-free decahedral silver nanoparticles with a fairly nar-
row size distribution of about 40-80 nm.
2. EXPERIMENTAL SECTION
2.1. Materials
Silver nitrate, sodium citrate, and sodium borohy-
dride were all purchased from Sigma-Aldrich. The as-re-
ceived chemicals were used without any further purifica-
tion. Milli-Q grade water (> 18 MW) was used for all solu-
tion preparation throughout all the experiments.
2.2. Instrumentation
Samples for transmission electron microscopy (TEM)
images were examined using a Hitachi H-7100 TEM oper-
ated at 75 KV. Samples for TEM measurement were pre-
pared by placing a drop of silver nanoparticle colloidsonto
carbon-coated copper grids and left to dry. All UV-vis-NIR
extinction spectra were recorded at 25 °C on a Hitachi
U-2800 spectrophotometer with a 1-cm quartz cuvette.
2.3. Preparation of Silver Nanoprisms and Decahe-
dral Silver Nanoparticles
Silver nanoprism colloids were prepared according to
literature methods.5j,19f-h A solution of sodium citrate (3.0 ´
10-2 M, 1 mL) and a solution of silver nitrate (1.0 ´ 10-2 M,
1 mL) were added to 97 mL pure water with rapid stirring.
Then the solution of sodium borohydride (5.0 ´ 10-3 M, 1
mL) was added drop-wise to the mixture, under vigorous
magnetic stirring. The solution immediately turned yellow,
which is the typical color for spherical nanoparticle silver
colloids. After being stirred for 30 min, the prepared solu-
Lee et al.
tions were irradiated with the sodium lamp (Philips 400-W
l = 589 nm) in the temperature-controlled water bath. The
typical power of the light on the colloid solution was about
0.66 W/cm2. The silver nanoplate colloids with a blue or
green color were obtained after 2 to 30 hours, which were
dependent on the bath temperature.
Decahedral silver nanoparticle colloids were pre-
pared by irradiating the spherical nanoparticle colloids
with the blue LEDs (450 ± 12 nm), about 3.5 mW/cm2, in a
water bath kept at 2 °C. The decahedral silver colloids, with
an orange-yellow color, were obtained after ca. 48 hours.
The colloids were then subjected to centrifugation at 8000
rpm for 15 min. The precipitates were highly-yielded deca-
hedral silver nanoparticles with a fairly narrow size distri-
bution.
2.4. Time Dependent UV-vis-NIR Extinction Spectra
and TEM of Silver Nanoplate Colloids
The shape evolution of the silver nanoparticles syn-
thesized at different temperatures was monitored by re-
cording their time-dependent UV-vis-NIR extinction spec-
tra and TEM images. Depending on the shape conversion
rate, 1 mL of colloidal solution was drawn out every 5-10
minutes for those synthesized at 60-90 °C, and every 20-40
minutes for those at 5-50 °C.
3. RESULTS AND DISCUSSION
Figs. 1a and 1b show the extinction spectra and TEM
image, respectively, of the spherical silver nanoparticles
corresponding to the yellow colloid before the light irradia-
tion. Since the intense light radiation from the sodium lamp
would increase the temperature of the silver colloids, we
controlled the temperature of the colloids by immersing the
lamp and reaction vials in a water tank, which was con-
nected to a circulator.
Figs. 2a-d show the time evolution of UV-vis-NIR ex-
tinction spectra of the silver colloids synthesized at 15, 40,
60, and 80 °C, respectively. According to the literature, the
peak position at ca. 392 nm was attributed to the surface
plasmon resonance of the silver spherical nanoparticle, and
the peaks at ca. 335 nm, 470 nm, 500 nm and 700 nm were
attributed to the out-of-plane quadrupole, dipole, in-plane
quadrupole and dipole surface plasmon resonance modes,
respectively.19a,24 These spectra show that the peaks at ca.
392 nm red shifted slightly to ca. 394 nm and their signals
increased by a factor of about 1.5 at the early stages (i.e.,
within 30 minutes) and decreased at the later stages of the
shape evolution reaction. The fact that the peaks at ca. 392
Temperature Effect on Ag Nanoparticle Growth J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010 327

Fig. 1. (a) Extinction spectra of spherical silver nanoparticle colloid. (b) TEM image of spherical silver nanoparticles.

nm red shifted slightly and increased in intensity at the longer plasmon wavelength and larger extinction coeffi-
early stage under light irradiation is because the smaller cients originating from the non-linear volume-dependent
nanoparticles converted into larger ones, 23 which have a light scattering efficiencies of nanoparticles.25 The rising

Fig. 2. Time evolution of UV-vis-NIR extinction spectra of the silver colloids synthesized at 15 °C (a), 40 °C (b), 60 °C (c),
and 80 °C (d).
328 J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010
times of the shape evolution reactions synthesized at differ-
ent temperatures were almost the same, ca. 30 minutes, and
almost independent of the temperature. This result is possi-
bly due to the fact that the conversion from smaller spheri-
cal nanoparticles into larger ones depends almost only on
the photochemical reaction but does not depend on the
thermal reaction. However, the rates of disappearance of
the peaks at ca. 394 nm increased a lot at higher tempera-
tures, e.g., ca. 2 hours for 80 °C and 17 hours for 15 °C.
This indicates that the conversion of large spherical nano-
particles into nanoplates or the nanostructures with other
shapes would strongly depend not only on the photochemi-
cal reaction but also on the thermal reaction.
Spectra A-D in Fig. 3 show the extinction spectra cor-
responding to the final products of silver nanostructures at
15, 40, 60, and 80 °C, respectively. The fact that the peak
widths of the in-plane dipole SPR modes in Fig. 3 de-
creased as the temperature increased implies that the nano-
structures synthesized at higher temperatures were more
homogeneous in size than those synthesized at lower tem-
peratures. Figs. 4a-d show the TEM images corresponding
to the products synthesized at 15, 40, 60 and 80 °C, respec-
tively. Fig. 4a, corresponding to the products synthesized at
15 °C, shows that most of the nanoparticles are triangular
in shape with very divergent sizes (i.e., some are smaller
than 40 nm, some are between 40-100 nm, and some are
larger than 120 nm). According to the reports by Mirkin et
al., the silver nanoprisms larger than 120 nm should come
from the photo-induced fusion of 4 small nanoprisms.19b
This is consistent with the observation that the peaks at ca.
Fig. 3. Extinction spectra of the final products of silver
nanostructures at 15 (A), 40 (B), 60 (C), and 80
°C (D).
Lee et al.
1050 nm, corresponding to the in-plane dipole SPR of very
large silver nanoprisms in Fig. 2a, appeared in the later
stage of the shape conversion reaction. Fig. 4d, corre-
sponding to the synthesis at 80 °C, shows that the nano-
structures are quite uniform in size of ca. 70-100 nm, of
which most are round triangular and the rest are circular in
shape. Few very large nanoprisms were observed at this
high temperature growth process. This observation implies
that the relatively sharp corners, which were found at lower
temperatures, might be very important for photo-induced
fusion of smaller nanoprisms into larger ones. The rounder
tips of the silver nanoprisms synthesized at a higher tem-
perature probably resulted from heat etching, photo etch-
ing, or the cooperation of photo and heat effects. Further
study is necessary to examine this observation. Figs. 4a-d
also show that the thicknesses of nanoplates synthesized at
a higher temperature were larger than that of those synthe-
sized at lower temperatures, i.e., 5-8 nm for 15 °C, 6-9 nm
for 40 °C, 7-9 nm for 60 °C and 12-14 nm for 80 °C. The
greater thickness of the nanoplates synthesized at a higher
temperature might have resulted from the fact that the ther-
mal reaction has less facet-selective growth than the photo-
reaction.23
Fig. 5 shows the TEM images of silver colloids syn-
thesized at 15 °C in a larger scale. Some of the products (the
ratio is ca. 1/10) synthesized at this low temperature were
decahedral in shape. According to this observation, it can
be concluded that the synthesis at lower temperatures, such
Fig. 4. TEM images of the products synthesized at 15
(a), 40 (b), 60 (c) and 80 °C (d).
Temperature Effect on Ag Nanoparticle Growth
as 15 °C, not only exhibits a very slow shape conversion
rate, but also tends to generate decahedral silver nanoparti-
cles. Since the decahedral silver nanoparticles have a shorter
SPR wavelength than silver nanoprisms, a light source with
a shorter wavelength should be more suitable for producing
decahedral silver nanoparticles. Fig. 6 shows the TEM im-
age of the silver nanostructures prepared by irradiating the
spherical nanoparticle colloids with the blue LEDs (450 ±
12 nm) at 2 °C for 48 hours. This TEM image shows that
the products are high-yield decahedral silver nanoparticles
with a fairly narrow size distribution of about 40-80 nm.
Fig. 7 shows the TEM image of the final products which
were prepared by irradiating the same spherical nanoparti-
cle colloids with the blue LEDs (450 ± 12 nm) at 60 °C for 6
hours. In Fig. 7, it is found that most of the products were
silver nanoplates with a thickness of about 9-11 nm. The
fact that few decahedral silver nanoparticles were synthe-
Fig. 5. TEM images of silver colloids synthesized at
15 °C in a larger scale.
Fig. 6. TEM image of decahedral silver nanoparticles,
which were prepared by irradiating the spheri-
cal nanoparticle colloids without adding any
surfactants nor PVP with the blue LEDs (450 ±
12 nm) at 2 °C for 48 hours.
J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010 329
Fig. 7. TEM image of decahedral silver nanoparticles,
which were prepared by irradiating the spheri-
cal nanoparticle colloids without adding any
surfactants nor PVP with the blue LEDs (450 ±
12 nm) at 60 °C for 6 hours.
sized at a high temperature and a lot of decahedral silver
nanoparticles can be formed at a very low temperature im-
plies that the thermal reaction helps to increase the forma-
tion rate of silver nanoplates. From these results, we can
conclude that thermal reaction is a key factor in synthesiz-
ing silver nanoparticles and that one can probably control
the morphology of nanoparticles by controlling the temper-
atures even without adding PVP or other large-molecu-
lar-mass surfactants.
4. CONCLUSION
The shape evolution from spherical silver nanoparti-
cles to silver nanoprisms and the nanostructures in other
shapes with a sodium lamp at various temperatures, i.e., 15,
40, 60, and 80 °C, were studied by recording the time
course UV-vis-NIR spectra and TEM images of the silver
colloids. From TEM and spectra analysis, we concluded
that the photomediated silver nanoparticle shape conver-
sion process would be faster at a higher temperature, and
slower at a lower temperature. The synthesis (with a so-
dium lamp) at low temperatures, such as 15 °C, not only has
a slower shape conversion rate but also produces decahe-
dra, with a yield ca. 10%. In order to produce a higher yield
of decahedral silver nanoparticles, the sodium lamp was re-
placed with blue LEDs, which have a wavelength closer to
the SPR of decahedral silver NPs. The decahedral silver
nanoparticles with a fairly narrow size distribution were
obtained by irradiating the spherical nanoparticle colloids
with the blue LEDs at 2 °C in the absence of PVP or other
large-molecular-mass surfactants.
330 J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010
ACKNOWLEDGMENT
This work was supported by the National Science
Foundation of Taiwan (NSC 96-2113-M-415-007-). We
would like to thank Ms. Pei-Hua Su and Prof. Ming-Jen
Lee for measuring the TEM images. We would also like to
thank Prof. Chia-Min Young for his helpful suggestions on
TEM studies. C.L. is grateful to Profs. Yuan T. Lee, Chi-
Kung Ni, Jon T. Hougen, I-Chia Chen, Jen-Ray Chang,
Chia-Min Young and Wenlung Chen and for their long time
support and encouragement.
Received February 26, 2010.
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