Colloids and Surfaces A: Physicochem. Eng.

Aspects 366 (2010) 197202

Contents lists available at ScienceDirect

Colloids and Surfaces A: Physicochemical and

Engineering Aspects
journal homepage: www.elsevier.com/locate/colsurfa

Size-controlled preparation of silver nanoparticles by a modied polyol method

Tao Zhao a , Rong Sun a, , Shuhui Yu a , Zhijun Zhang b , Limin Zhou c , Haitao Huang d, , Ruxu Du e
a

Shenzhen Institutes of Advanced Technology, Chinese Academy of Sciences, 1068 Xueyuan Avenue, Shenzhen University Town, Shenzhen 518055, PR China
Key Lab for Special Functional Materials, Ministry of Education, Henan University, Kaifeng 475001, PR China
c
Department of Mechanical Engineering, the Hong Kong Polytechnic University, Hon Hum, Kow Loon, Hong Kong, PR China
d
Department of Applied Physics, the Hong Kong Polytechnic University, Hon Hum, Kow Loon, Hong Kong, PR China
e
Institute of Precision Engineering, the Chinese University of Hong Kong, Shatin, NT, Hong Kong, PR China
b

a r t i c l e

i n f o

Article history:
Received 3 February 2010
Received in revised form 17 May 2010
Accepted 2 June 2010
Available online 11 June 2010
Keywords:
Size-controlled preparation
Ag nanoparticles
Polyol method

a b s t r a c t
In this work, size-controlled silver nanoparticles were prepared with liquid phase chemical method in
the ethylene glycol/polyvinylpyrrolidone media. Crystal structure, size, thermal properties and surface
chemistry state of the silver nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), thermal analysis (TA) and X-ray
photoelectron spectroscopy (XPS). The particle size can be conveniently adjusted to 80 nm, 50 nm, 30 nm
and 10 nm by controlling the experimental parameters such as the ratio of PVP to AgNO3 , and the amount
of ammonia added as complexing agent. The as-obtained silver nanoparticles can be dispersed in water,
ethanol and other polar solvents, which has attractive applications in electrical and biological elds.
Crown Copyright 2010 Published by Elsevier B.V. All rights reserved.

1. Introduction
Silver nanoparticles have a wide range of applications in
many elds, such as surface-enhanced Raman spectroscopy [1],
catalysts [2,3], anti-bacterial materials [4,5] and lubricating materials [6]. Recently, it was reported that Ag nanoparticles exhibit
promising cytoprotective activities towards HIV-infected T-cells
[7,8] and HBV [9]. Ag/polymer composite [10,11] is approach
towards high-k materials for embedded capacitor application. The
dielectric behavior of such composites is strongly dependent on
the size, shape and distribution of the lling particles [12,13].
Nanoparticles with controlled particle size are of key importance
because the optical, and magnetic properties of these nanoparticles
depend strongly on their size [14,15]. Therefore, the synthesis
of size-controlled nanoparticles is of great importance for both
fundamental research and technical applications. Especially,
nanoparticles that can be dispersed in a specic media, such as the
polar or non-polar solvents, are most desirable in order to meet
different application requirements.
Up to now, various methods have been employed to prepare Ag
nanoparticles with different size and shape, such as UV irradiation
[16], electron irradiation [17], photochemical method [18], sonoelectrochemical method [19], microwave irradiation [20], chemical
reduction [2125], atom beam sputtering [26]. However, most of

the reported methods involve more than one steps and sometimes
produce unsafe chemicals. Besides, the derived Ag nanoparticles
with the above methods are hard to be dissolved in polar solvents,
which limits their applications. For example, use Ag nanoparticles
as llers in dielectric composites with polar polymers as the matrix,
or as the anti-bacterial and antiviral agents in aqueous media.
The purpose of this study is to synthesize size-controlled Ag
nanoparticles that can be dispersed in polar solvents using a
method that is simple and environmental friendly. As one of the
liquid phase chemical methods, polyol method is simple and environmentally friendly, without need for inert gas protection. It has
been proven that the polyol method is a convenient and versatile
method for the preparation of Ag [27], Pd [28], Te [29] BiIn [30],
FePt [31], metal oxides [32,33] and chalcogenide [34] nanoparticles.
The polyol involved in the reaction can act as a solvent, stabilizer, and reducing agent which limits particles growth and prevent
agglomeration. In previous studies, our research group [30,33] has
prepared ZnO nanotubes and BiIn alloy nanoparticles in polyols.
Preparations of Ag nanoparticles in polyols have been reported
before. However, almost all the studies focused on the morphology control [27,35], while the control of particle size using the
polyol process is rarely reported. In this paper, a simple and efcient
polyol process was explored to synthesize the size-controlled Ag
nanoparticles that can be dispersed in polar solvents. The formation
mechanism of Ag nanoparticles has been investigated in details.
2. Experimental

Corresponding authors.
E-mail addresses: rong.sun@siat.ac.cn (R. Sun), aphhuang@polyu.edu.hk
(H. Huang).

Silver nitrate (AgNO3 ) (impurity >99%, Kermel Chemical Co.,

Tianjin, China), polyvinylpyrrolidone (PVP-K30, MW 40,000)

0927-7757/$ see front matter. Crown Copyright 2010 Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.colsurfa.2010.06.005

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T. Zhao et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 366 (2010) 197202

Fig. 1. XRD pattern of PVP capped Ag nanoparticles.

(Kermel Chemical Co., Tianjin, China), ethylene glycol (impurity

>98%, Kermel Chemical Co., Tianjin, China) and ammonia (28%,
Kermel Chemical Co., Tianjin, China) were used as raw materials.
In a typical procedure, an appropriate amount of PVP
(0.171.7 g) was dissolved in 10 ml ethylene glycol and heated up
to 160 C in an oil bath, until it turned from colorless to light yellow. Then, 0.170 g of AgNO3 in another 10 ml ethylene glycol was
added dropwise into the above solution. and the reaction allowed
to proceed for 4 h at this temperature., A brown colloidal dispersion
was formed which indicated the formation of silver nanoparticles.
The colloidal dispersion was cooled down to room temperature and
mixed with a certain amount of acetone to allow for the generation
of brown precipitate The precipitate was collected after centrifugation (8000 rpm for 30 min) and washed with acetone for three
times, followed by drying at 40 C for 5 h in a vacuum dryer.
X-ray diffraction (XRD) patterns were recorded with Philips
XPert Pro X-ray powder diffraction instrument (the Netherlands,

Fig. 2. TEM images of PVP capped Ag nanoparticles prepared with different mass ratios of PVP to AgNO3 , (a) 8:1, (b) 10:1, (c) 15:1, (d) 20:1, (e) 8:1 (with ammonia) and (f)
10:1 (with ammonia).

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199

Philips Company). The operation voltage and current were 40 kV

and 40 mA, respectively, with a scanning rate of 10 /min. The
morphology of the as-synthesized Ag nanoparticles was examined on a JEOL JEM 100CX-II transmission electron microscope
(TEM) at an acceleration voltage of 100 kV. The prepared particles were dispersed in ethanol with ultrasonic agitation for 2 min,
and then deposited on a copper grid covered with a perforated
carbon lm. They were then subject to TEM observation. Nicolet
Avatar 360-type Fourier transform infrared spectroscopy (FT-IR,
the United States Nicolet Corporation) was used to characterize
the surface structure of Ag nanoparticles in the wavelength range
of 4000400 cm1 . The prepared Ag nanoparticles were mixed with
KBr powder and pressed into a pellet for measurement. Background
correction was made on the basis of the spectrum from a reference
pure KBr pellet. Thermogravimetry analysis (TGA) and differential thermal analysis (DTA) were conducted in nitrogen on a Seiko
EXSTAR 6000 thermal analysis system (TG & DTA, Japans Seiko Corporation) at a scanning rate of 10 C/min. The surface chemical state
of the Ag nanoparticles was also investigated by X-ray photoelectron spectroscopy (XPS, AXIS Ultra Kratos Analytical Ltd.), using
monochromatised Al K radiation with an anode voltage of 15 kV
and emission current of 3 mA. All the XPS spectra were calibrated
using the main component of the C1s signal, attributed to aromatic
carbons, at 284.8 eV.
3. Results and discussion
3.1. Crystal structure analysis
The XRD spectrum of the as-synthesized PVP capped Ag
nanoparticles of a typical size (30 nm) is shown in Fig. 1. Five
main characteristic diffraction peaks for silver were observed at
2 = 38.2 , 44.5 , 64.7 , 77.5 , and 81.8 , which correspond to the
(1 1 1), (2 0 0), (2 2 0), (3 1 1), and (2 2 2) crystallographic planes
of face-centered cubic (fcc) Ag crystals, respectively (JCPDS No.
870720). The result conrms that the samples were metallic silver nanoparticles with cubic crystal structure. No diffraction peaks
of Ag2 O were detected in Fig. 1, which suggests that the PVP capped
layer on Ag nanoparticles prevents Ag nanocores from oxidation.
3.2. Size-controlled Ag nanoparticles
With the aim of preparing monodispersed silver nanoparticles
with different sizes, several AgNO3 to PVP ratios were tried in order
to determine the optimum conditions. The AgNO3 concentration
was xed, while the amount of PVP added was varied in the range
of 0.171.7 g. Fig. 2a and b shows TEM images of PVP capped Ag
nanoparticles prepared with various PVP to AgNO3 ratios. When
the mass ratio of PVP to AgNO3 were slightly increased from 8:1
to 10:1, the size of Ag nanoparticles decrease drastically from 80
to 50 nm. However, if we further increase the mass ratio of PVP to
AgNO3 to 15:1 or 20:1, it found that the size of the nanoparticles
changed not obviously, as shown in Fig. 2c and d. The reason may
be as: when the mass ratio of PVP to AgNO3 was above 10:1, it was
found that the viscosity of the reaction system increased dramatically. The increased viscosity makes it difcult for the Ag atoms to
diffuse in the system and results in an almost constant particle size
that is independent of the PVP concentration. Therefore, it is difcult to prepare nanoparticles with size less than 50 nm by merely
increasing PVP concentration.
To overcome the problem, an appropriate amount of ammonia
was added to the AgNO3 solutions during the reaction process. The
pH of the AgNO3 solutions was adjusted to be 10 using ammonia
solution. As a result, well dispersed Ag nanoparticles with smaller
sizes of 30 and 10 nm were obtained, as shown in Fig. 2e and f,

Fig. 3. FT-IR spectra of (a) PVP and (b) PVP capped Ag nanoparticles.

respectively. In this reaction, NH3 and Ag+ form Ag (NH3 )2 + , which

is more difcult to be reduced than Ag+ does. From the potential
point of view, Ag+ /Ag0 electrical potential is 0.7991 V, while [Ag
(NH3 )2 ]+ /Ag0 electric potential is 0.3719 V at standard temperature
and pressure, so the reduction of Ag+ to silver metal is easier than
[Ag (NH3 )2 ]+ . Therefore, when the redox reaction took place, the
silver grain growth was suppressed and the grains were coated with
PVP, leading to smaller sizes of silver nanoparticles.
A typical reduction reaction of a silver cations. First, the ethylene
glycol lost water and changed into acetaldehyde. Then, Ag+ or [Ag
(NH3 )2 ]+ were reduced by acetaldehyde to Ag0 . The reaction could
be expressed as
HO(CH2 )2 OH CH3 CHO + H2 O
+

Ag + CH3 CHO Ag

[Ag (NH3 )2 ]+ + CH3 CHO Ag0

(1)
(2)
(3)

3.3. FT-IR analysis

Fig. 3 shows the IR spectra of PVP and PVP coated Ag nanoparticles. For PVP spectrum shown in Fig. 3a, the bands at 2920

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T. Zhao et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 366 (2010) 197202

and 2885 cm1 are attributed to the asymmetric and symmetric

stretching vibrations of CH2 , respectively. The bands at 722 cm1
are attributed to the bending vibrations in plane of the long chain
(CH2 )n (n > 4). 1095 cm1 and 1075 cm1 are the CN asymmetric and symmetric stretching vibrations, respectively. The bands
between 1400 and 1500 cm1 are three groups bond absorption
peaks of NC. The bands at 1661 cm1 is attributed to the stretching vibration of the C O. All the absorption peaks are related to
the characteristic absorption of PVP. The bands at 3430 cm1 are
attributed to the stretching vibration absorption of OH of adsorbed
water, as PVP has a strong hygroscopicity.
The IR spectrum of PVP capped Ag nanoparticles with an average diameter of 30 nm is shown in Fig. 3b. The CH2 vibration
bands are detected, but the asymmetric and symmetric stretching
vibration peaks of CN shift from 1095 and 1075 cm1 to 1118 and
1080 cm1 , respectively. The stretching vibration peak of C O also
moves from 1661 to 1668 cm1 . These shifted peaks indicate that
the N or O atoms of the PVP molecules interact with the surface of
Ag nanoparticles by chemical absorption.
3.4. Thermal behavior
Fig. 4 shows the TGA and DTA curves of PVP capped Ag nanoparticles. The mass loss before 100 C in the TGA curve is due to the
evaporation of adsorbed water. The weight loss from 100 to 200 C
is attributed to the decomposition of a small amount of organic
molecules in the sample. An obvious mass loss is observed from
404 to 457 C, which corresponds to the decomposition of the capping layer of the sample. Above 457 C, the TGA curve tends to
be smooth and at, and the sample reaches a constant weight.
The total mass loss of PVP coated Ag nanoparticles is about 86%.
There is an endothermic peak in the vicinity of 146 C in the DTA
curve which corresponds to the melting of the organic molecules in
the sample. The endothermic peak near 450 C is attributed to the

Fig. 4. TGDTA curves of PVP capped Ag nanoparticles.

decomposition of PVP. The thermal analysis results conrm that

the Ag nanoparticles are coated with PVP.
3.5. XPS analysis
Fig. 5 shows the XPS spectra of PVP. It can be seen that the
occurrence of carbon, oxygen, and nitrogen signals conrms the
presence of the typical PVP. Through curve tting it can be found
that the C1s spectrum is composed of four peaks with binding energies of 284.8, 285.6, 286.1, and 287.6 eV, which are attributed to the
C1 (and C4 ), C3 (and C5 ), C2 , and C6 of the PVP molecule, respectively. O1s electronic binding energy at 531.3 eV is attributed to the
carboxyl (C O) oxygen atom, and that at 533.4 eV corresponds to
the binding energy of the adsorbed water. N1s electronic binding
energy is at 399.6 eV.

Fig. 5. Molecular formula of PVP repeated unit, with carbon atom numbering and XPS spectra of PVP.

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201

Fig. 6. XPS spectra of PVP capped Ag nanoparticles.

Fig. 6 shows the XPS spectra of the PVP capped Ag nanoparticles,

where the C1s electronic binding energies at 284.8, 285.6, 286.1, and
287.6 eV are the same as those of PVP. Curve tting in the O1s region
leads to two peaks at 531.2 and 532.8 eV, originated from carboxyl
(C O) oxygen atoms of PVP and hydroxyl (COH) oxygen atoms
of ethylene glycol, respectively. Compared with PVP, the N1s electron binding energy increases to 400.3 eV, which implies that the
lone pair electrons of N atoms are transferred to the Ag nanoparticles, leading to the decrease of the electron cloud densities around
the N atoms. Ag3d electronic binding energy at 368.1 eV of the Ag
nanoparticles is the same as that of the metallic Ag. The oxygen
signals from Ag2 O (O1s electron binding energy at 529.2 eV) and
AgO (O1s electron binding energy at 528.5 eV) are not found. Due
to the interaction between the N atoms of PVP and the Ag nanoparticles, the N Ag coordination bond could form on the surface of
the Ag nanoparticles, which corresponds to the blue shift of the CN
stretching vibration, as indicated in Fig. 3b. Therefore, both the XRD
and XPS analysis indicate that PVP prevents Ag nanoparticles from
being oxidized.

4. Conclusion
In summary, an optimal condition for the synthesis of size controlled, well dispersed Ag nanoparticles in ethylene glycol/PVP
system has been developed by controlling the mass ratios of PVP
to AgNO3 , and by adding a certain amount of ammonia as the
complexing agent. The average particle size can be varied from
10 to 80 nm with a narrow size distribution by controlling the
amount of PVP and ammonia added. The particles size decreases
with increasing PVP concentration in a certain range and the addition of ammonia to the precursor solution can further decrease the
Ag particle size. FT-IR and XPS analysis results show that the N

atoms in PVP coordinates to the Ag core surface and form a coordination bond between a N atom and a silver at the surface of the core.
The size-controlled, well dispersed Ag nanoparticles prepared are
capable of being dispersed in water, ethanol, and other polar solvents which have potential applications in dielectric and biological
elds.
Acknowledgements
This work was supported by the National Natural Science Foundation of China (No. 20971089, No. 50807038) and the research
funding from National S&T Major Project with the contact No.
2009ZX02038 is greatly acknowledged.
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