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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 hoursat 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

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-

chemical reaction tends to the formation of anisotropic

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 amore 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

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

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

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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 onlyex-

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-

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

326 J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010 Lee et al.

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nm red shifted slightly and increased in intensity at the

early stage under light irradiation is because the smaller

nanoparticles converted into larger ones,23

which have a

longer plasmon wavelength and larger extinction coeffi-

cients originating from the non-linear volume-dependent

light scattering efficiencies of nanoparticles.25

The rising

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.

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).

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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.

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

328 J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010 Lee et al.

Fig. 3. Extinction spectra of the final products of silver

nanostructures at 15 (A), 40 (B), 60 (C), and 80

C (D).

Fig. 4. TEM images of the products synthesized at 15

(a), 40 (b), 60 (c) and 80 C (d).

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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 12nm) at 60Cf or 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-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 sodiumlamp 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.

Temperature Effect on Ag Nanoparticle Growth J. Chin. Chem. Soc., Vol. 57, No. 3A, 2010 329

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.

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.

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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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