Silver nanoparticles from the thermal decomposition of a two-dimensional nano-coordination polymer

Article abstract of DOI:10.1016/j.poly.2010.09.011

Nanostructures of the two-dimensional coordination polymer [Ag(μ₃-Hma)]_n (1) [H₂ma = maleic acid] have been synthesized by the reaction of KHma and AgNO₃ by a sonochemical process and with oleic acid treatment at 453 K. The single-crystal X-ray data of compound 1 shows the formation of a hemi paddlewheel structure. The coordination number of the Ag^I ions in compound 1 is three and there is an argentophillic interaction. Silver nanostructures and silver nanoparticles were synthesized by calcination and thermal decomposition of the compound 1 nanostructures, respectively. These nanostructures and nanoparticles were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The thermal stability of compound 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA).

Full text of DOI:10.1016/j.poly.2010.09.011

Polyhedron 29 (2010) 3304–3309
Contents lists available at ScienceDirect
Polyhedron
journal homepage: www.elsevier.com/locate/poly
Silver nanoparticles from the thermal decomposition of a two-dimensional
nano-coordination polymer
Kamran Akhbari , Ali Morsali , Pascal Retailleau b
a
a,
⇑
a
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-4838, Tehran, Islamic Republic of Iran
Service de Cristallochimie, Institut de Chimie des Substances Naturelles-CNRS, Bât 27, 1 Avenue de la Terrasse, 91190 Gif sur Yvette, France
b
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 4 April 2010
Accepted 7 September 2010
Available online 21 September 2010
Nanostructures of the two-dimensional coordination polymer [Ag(l3-Hma)]n (1) [H ma = maleic acid]
have been synthesized by the reaction of KHma and AgNO by a sonochemical process and with oleic acid
3
2
treatment at 453 K. The single-crystal X-ray data of compound 1 shows the formation of a hemi paddle-
I
wheel structure. The coordination number of the Ag ions in compound 1 is three and there is an argen-
tophillic interaction. Silver nanostructures and silver nanoparticles were synthesized by calcination and
thermal decomposition of the compound 1 nanostructures, respectively. These nanostructures and nano-
particles were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM).
The thermal stability of compound 1 was studied by thermal gravimetric (TG) and differential thermal
analyses (DTA).
Keywords:
Nano-coordination polymer
Silver nanoparticle
Sonochemical
Surfactant
Oleic acid
Ó 2010 Elsevier Ltd. All rights reserved.
1
. Introduction
Recently nanosized coordination polymers (NCPs) with finite
nanoparticles with well-defined shapes but the use of silver CPs
or silver NCPs to prepare silver nano structures is scarce [17].
Among the coordination polymers, structures with a two-dimen-
sional organization are of particular interest because of their po-
tential for offering optimized optical or electrical functions [18].
Continuing our previous work on silver(I) CPs [19–22] and studies
on the relation between the silver(I) coordination polymer dimen-
sion and the dimension of the resulting silver nano-structure
repeating units have aroused a growing interest due to their spe-
cial properties, distinctive from conventional bulk coordination
polymers (CPs) [1]. For this reason, such nano-sized materials are
interesting candidates for applications in many fields, including
electronics, catalysis, separation, biology, medical imagery and
others [2]. Recently, we and others have shown how such struc-
tures can be transformed into nano- and microparticle materials
through controlled precipitation methods [3–7]. For example, at-
tempts to reduce the crystal size of metal coordination polymers
to the nanometer scale have appeared using the reverse micelles
technique, the Langmuir–Blodgett method, template synthesis,
film formation and the simple mixing of starting complexes in
the presence of an organic stabilizer [8], but examples of the for-
mation NCPs by the sonochemical process are scarce [5–7].
I
[17,23], the synthesis of a two-dimensional Ag NCP of maleic acid
by the sonochemical process and oleic acid as a surfactant is re-
ported. Also silver nano-structures have been fabricated from this
silver(I) NCP by the calcination method and by a thermal decompo-
sition process.
2
. Experimental
2.1. Materials and physical techniques
Among polymeric coinage d10 metal complexes, silver(I) coordi-
nation polymers have received much attention because silver(I)
shows a tendency to form coordination polymers with unique me-
tal–carbon [9–13] and metal–metal [14,15] interactions. Silver has
been extensively used in a variety of applications such as catalysis,
electronics, photonics, photography, biology and medicine-science
due to its unique properties. For example, silver has the highest
electrical conductivity, thermal conductivity and reflectivity of all
metals [16]. Several methods can be applied to synthesize silver
All reagents for the synthesis and analysis were commercially
available and used as received. Double distilled water was used to
prepare the aqueous solutions. A multiwave ultrasonic generator
(
Sonicator_3000; Misonix, Inc., Farmingdale, NY, USA), equipped
with a converter/transducer and a titanium oscillator (horn),
2.5 mm in diameter, operating at 20 kHz with a maximum power
output of 600 W and an ultrasonic bath (Tecna 6; 50–60 Hz and
.138 KW) were used for the ultrasonic irradiation. Microanalyses
1
0
were carried out using a Heraeus CHN–O– Rapid analyzer. Melting
points were measured on an Electrothermal 9100 apparatus and are
uncorrected. IR spectra were recorded using Perkin–Elmer 597 and
⇑
Corresponding author. Tel.: +98 21 8011001; fax: +98 21 8009730.
E-mail address: morsali_a@yahoo.com (A. Morsali).
0
277-5387/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.poly.2010.09.011

K. Akhbari et al. / Polyhedron 29 (2010) 3304–3309
3305
Nicolet 510P spectrophotometers. The thermal behavior was mea-
sured with a PL-STA 1500 apparatus between 35 and 600 °C in a sta-
tic atmosphere of nitrogen. Crystallographic measurements were
made using a Bruker APEX area-detector diffractometer. The inten-
solutions, and the SEM images of three samples with higher con-
centrations were not acceptable. In order to obtain silver nano-
structures, precipitates of compound 1 nanostructures, which
were obtained from 0.1 to 0.5 M solutions of the initial reagents
with the sonicator unit, were calcinated at 673 K in a furnace under
a static atmosphere of air for 5 h.
sity data were collected using graphite monochromated Mo K
a
radiation. The structure was solved by direct methods and refined
2
by full-matrix least-squares techniques on F . Structure solution
and refinement was accomplished using SHELXL-97 program pack-
ages [24]. The molecular structure plot and simulated XRD powder
pattern based on single crystal data were prepared using MERCURY
software [25]. X-ray powder diffraction (XRD) measurements were
performed using a Philips X’pert diffractometer with monochroma-
2.4. Synthesis of [Ag(l3-Hma)] (1) nanoparticles by surfactant
n
To prepare compound 1 nanostructures by surfactant, precipi-
tates of compound 1 nanostructures (223 mg, 1 mmol) were dis-
persed in 16 mL (50 mmol) oleic acid (OA). This solution was
heated to 453 K for 1 h under an air atmosphere in an electric fur-
nace. At the end of the reaction, a black precipitate was formed. A
small amount of toluene and a large excess of EtOH were added to
the reaction solution, and compound 1 precipitate was separated
tized Cu Ka radiation. The samples were characterized with a scan-
ning electron microscope with a gold coating.
2.2. Synthesis of [Ag(
3 n
l -Hma)] (1) and preparation of its single
by centrifugation. The solid was washed with EtOH and dried,
crystals
À1
(
Found C, 21.40; H, 1.36%). IR (selected bands; in cm ): 553w,
6
1
50w, 706s, 875s, 991s, 1085w, 1196s, 1268w, 1353vs, 1397vs,
495vs, 1576vs, 1615s, 1704s, 3045w, 3447w.
In 20 ml CH
stirred with a solution of 0.057 g (1 mmol) KOH in 3 ml H
form a clear solution. Addition of 0.170 g (1 mmol) AgNO
ml CH CN still maintained a clear solution. The resulting solution
3
CN, 0.116 g (1 mmol) maleic acid were mixed and
O to
in
2
3
5
3
2.5. Synthesis of silver nanoparticles by surfactant
was stirred and then allowed to stand in darkness at room temper-
ature to evaporate for several days to obtain suitable crystals. The
crystals were washed with acetone and air dried. D.p. = 150 °C.
Yield: 0.167 g (75% based on final product). IR (selected bands; in
To prepare silver nanoparticles by surfactant [26], precipitates
of compound 1 nanostructures (446 mg, 2.0 mmol), obtained from
the sonochemical process, were dispersed in oleic acid (OA),
(16 mL, 50 mmol) to form an homogenous emulsion solution. This
solution was degassed for 15 min and then heated to 523 K for 1 h
under an air atmosphere in an electric furnace. At the end of the
reaction, a black precipitate was formed. A small amount of tolu-
ene and a large excess of EtOH were added to the reaction solution,
finally metallic silver was separated by centrifugation. The solid
was washed with EtOH and dried, neither d.p. nor IR bands were
observed.
À1
cm ): 553w, 649w, 705s, 871s, 992s, 1080w, 1192s, 1267w,
1
350vs, 1391vs, 1491vs, 1578vs, 1618s, 1700s, 3045w, 3445w.
Anal. Calc. for C AgO : C, 21.53; H, 1.34. Found: C, 20.65; H,
.40%.
4
H
3
4
1
2.3. Synthesis of [Ag(
3 n
l -Hma)] (1) nanostructures by the
sonochemical process
3 n
To prepare nanostructures of [Ag(l -Hma)] by the sonochem-
ical method, a high-density ultrasonic probe was immersed di-
3. Results and discussion
rectly into a solution of KHma (50 ml, 0.1 M) in MeOH, then into
this solution a proper volume of AgNO
3
aqueous solution (10 ml,
3.1. Structure description
0
.5 M) was added in a dropwise manner. The solution was ultra-
sonically irradiated with a power of 27 W for 1 h. The obtained pre-
cipitates were filtered, subsequently washed with MeOH and then
dried, (found C, 21.20; H, 1.29%). IR (selected bands; in cm ):
The Scheme 1 shows the reaction between silver(I) nitrate and
KHma by two different methods.
À1
The reaction between maleic acid (H
crystalline material of the general formula [Ag(
2
ma) and AgNO
3
provided a
(1).
5
1
55w, 650w, 708s, 878s, 994s, 1085w, 1191s, 1267w, 1351vs,
392vs, 1498vs, 1577vs, 1618s, 1701s, 3046, 3449w. Before the
l
3
-Hma)]
n
Determination of the structure of 1 by X-ray crystallography (Ta-
bles 1 and 2), showed the complex to be a novel two-dimensional
polymer (Fig. 1). The silver atoms can be considered to be three-
coordinate. As a result of the reaction conditions, partial deproto-
usage of the sonicator unit, we used an ultrasonic bath for the
ultrasonic irradiation with different concentrations of metal and li-
gand solutions (0.025, 0.05, 0.1, 0.2, 0.4 and 0.8 M) and a power of
0
.138 KW for 1 h, but we could not obtain a precipitate of com-
nation of the H
2
ma ligand occurs. The carboxylate and carboxylic
À
pound 1 with the three initial concentrations of metal and ligand
acid groups of the Hma ligand do not act as bridging groups.
Evaporation in MeCN solvent
Single crystal of [Ag(Hma)]n (1)
By sonochemical process
AgNO3 + KHma
Nanstructure of [Ag(Hma)]n (1)
Calcinations at 673 K
Silver nanostructure
In OA at 453 K
Nanstructure of [Ag(Hma)]n (1)
Silver nanoparticles
Thermal decomposition in OA at 523 K
Scheme 1. The produced materials from the reaction of the KHma ligand with silver(I) nitrate by two different methods and fabrication of silver nanostructures from
compound 1 nano-coordination polymer.

3
306
K. Akhbari et al. / Polyhedron 29 (2010) 3304–3309
Table 1
3 n
Crystal data and structure refinement for compound [Ag(l -Hma)] (1).
Empirical formula
Formula weight
T (K)
4 3 4
C H AgO
222.93
298(2)
0.71073
k (Å)
Crystal system
Space group
Unit cell dimensions
a (Å)
b (Å)
c (Å)
monoclinic
P2 /c
1
10.5896(16)
3.7140(6)
16.5617(18)
90.00
128.618(6)
90.00
508.93(13)
4
2.910
a
(°)
b (°)
(°)
c
3
V (Å )
Z
D
À3
calc (g cm
)
À1
Absorption coefficient (mm
)
3.881
F(0 0 0)
Crystal size (mm )
h range for data collection (°)
424
3
0.23 Â 0.21 Â 0.15
2.46–25.10
Index ranges
À8 6 h 6 12, À4 6 k 6 4,
À19 6 l 6 14
Reflections collected
2336
Independent reflections (Rint
)
916 (0.1180)
Absorption correction
Maximum and minimum transmission
Refinement method
semi-empirical from equivalents
0.5537 and 0.4289
Full-matrix least-squares on F2
916/0/84
Data/restraints/parameters
Goodness-of-fit (GOF) on F2
1.136
Final R indices [I > 2
R Indices (all data)
r
(I)]
R
R
1
= 0.0455, wR
= 0.0466, wR
2
2
= 0.1100
= 0.1112
1
Largest difference in peak and hole
1.496 and À1.678
À3
(
e Å
)
Table 2
Selected bond lengths (Å) and angles (°) for compound [Ag(
l
3
-Hma)]
n
(1).
Ag1–O4i
2.226(3)
2.276(2)
2.418(2)
2.9915(8)
2.276(2)
2.226(3)
O4 –Ag1–O3
i
ii
158.15(9)
106.85(9)
94.88(8)
80.38(6)
79.33(5)
163.10(7)
ii
i
Ag1–O3
Ag1–O1
Ag1–Ag1
O4 –Ag1–O1
ii
O3 –Ag1–O1
iii
i
iii
O4 –Ag1–Ag1
Fig. 1. A fragment of the two-dimensional network in 1; (a) along crystallographic c
axis, showing hemi paddlewheel structure, (b) along crystallographic axis,
iv
ii
iii
O3–Ag1
O3 –Ag1–Ag1
a
O4–Ag1v
O1–Ag1–Ag1
iii
showing parallel one-dimensional corrugated tape polymers which are connected
to each other to form a two-dimensional network, H atoms have been omitted for
clarity (Ag = violet, O = red, C = gray). (For interpretation of the references to colour
in this figure legend, the reader is referred to the web version of this article.)
Symmetry transformations used to generate equivalent atoms; i: x + 1, Ày À 1/2,
z + 1/2, ii: Àx + 2, y + 1/2, Àz + 3/2, iii: Àx + 3, Ày, Àz + 2, iv: Àx + 2, y À 1/2, Àz + 3/2,
v: x À 1, Ày À 1/2, z À 1/2.
À
The two carboxylate groups of two Hma ligands coordinate to two
+
Ag ions and form a hemi paddlewheel structure (Figs. 1a and 2).
The oxygen atom of the carboxylic acid C@O group occupies the
axial position of another hemi paddlewheel structure. Another fea-
ture of this hemi paddlewheel structure is the formation of Ag–Ag
bonds between two Ag atoms of this structure (Figs. 1a and 2). The
Ag–Ag interactions in compound 1, Ag1–Ag1 = 2.997 Å, are longer
than the Ag–Ag distances in similar dinuclear complexes (i.e.,
2
.704(2), 2.669(1) and 2.726(1) Å) [27–31] and slightly shorter
than those in the polymeric structure [32–35]. The relatively short
Ag–Ag bonds found here may thus be considered to be only
1
0
10
d
Á Á Ád non-covalent interactions [27–35]. Thus compound 1
can be considered to contain silver atoms with three-fold coordina-
tion and an O
3
AgÁ Á ÁAgO
3
coordination environment. The structure
Fig. 2. A fragment of the two-dimensional network in 1, along the crystallographic
b-axis, showing hydrogen bonding interactions as dashed lines and the hemi
paddlewheel structure, (Ag = purple, O = red, C = gray, H = white). (For interpreta-
tion of the references to colour in this figure legend, the reader is referred to the
web version of this article.)
of compound 1 could be considered as a parallel one-dimensional
corrugated tape polymers along the a-axis, which are connected to
each other and form a two-dimensional network (Fig. 1b). Hydro-
gen bonding interactions are present between the –OH and –COO
groups of the Hma ligand in compound 1 (Fig. 2).
Fig. 3a shows the simulated XRD pattern from single crystal X-
ray data of the above compound and Fig. 3b shows the XRD pattern
3 n
of typical samples of [Ag(l -Hma)] (1) prepared by the sonochem-
À
À
ical process and treatment with oleic acid at 453 K. Acceptable
matches, with slight differences in 2h, were observed between
the simulated patterns from single-crystal X-ray data (Fig. 3a)
and the experimental powder X-ray diffraction patterns for a nano-

K. Akhbari et al. / Polyhedron 29 (2010) 3304–3309
3307
Fig. 4. SEM images of compound 1 nanostructures prepared by the sonochemical
process (top) and treatment with oleic acid at 453 K (bottom).
Fig. 3. XRD patterns; (a) simulated pattern based on single crystal data of
compound 1, (b) nanostructures of compound 1 prepared by the sonochemical
process and treatment with oleic acid, (c) silver nanostructures and silver
nanoparticles prepared by calcination and thermal decomposition of compound 1
nanostructures.
1
20
00
200
150
TG
DTA
1
structure crystalline sample as obtained from the synthesis by the
sonochemical process and treatment with oleic acid at 453 K
8
6
4
2
0
0
0
0
0
(
Fig. 3b). The results of the XRD powder patterns indicate that
1
5
0
00
the experimental data are in good agreement with the simulated
XRD powder patterns based on single crystal data, hence this com-
pound is obtained as a mono-phase. The morphology, structure
and size of the five samples which were prepared by the sono-
chemical process and treatment with oleic acid were investigated
by scanning electron microscopy (SEM). Fig. S1a–c shows the
SEM images of compound 1, for three samples obtained by the
sonochemical process in an ultrasonic bath. As could be observed
from this figure, acceptable results were not obtained from this
process and the power of ultrasonic bath was not appropriate to
fabricate compound 1 nanostructures. On the other hand, with
lower concentrations of ligand and metal solutions, no precipitate
of compound 1 was formed. In order to obtain compound 1 nano-
structures using the sonochemical process, we used a multiwave
ultrasonic generator. Fig. 4(top) and Fig. S2 show the SEM images
of compound 1 nanostructures with an average diameter of
0
-50
700
0
100
200
300
400
500
600
Temperature(°C)
Fig. 5. Thermal behavior of compound 1 single crystals.
is stable up to 156 °C (Fig. 5), at which temperature decomposition
and pyrolysis of compound 1 starts in two steps with endothermic
and exothermic effects at 217 and 307 °C, respectively. In these
À
3
50 nm, obtained by the sonochemical process with a multiwave
two steps, removal of Hma occurs between 156 and 362 °C with
ultrasonic generator. Treatment of compound 1 nanostructures
with oleic acid as a surfactant at 453 K results in the formation
of compound 1 nanostructure aggregates from nanoparticles of
this compound, with a diameter of about 30–90 nm and average
diameter of 50 nm, which can be observed in Fig. 4(bottom).
Thermal gravimetric (TG) and differential thermal analyses
a mass loss of 48.7% (calc. 51.6%). Mass loss calculations show that
the final decomposition product is metallic silver.
Fig. 3c shows the XRD pattern of the residue obtained from cal-
cinations of compound 1 nanostructures at 673 K. The obtained
patterns match with the standard patterns of cubic silver with lat-
tice parameters (a = 4.0862 Å and z = 4) which are close to the re-
ported values, (JCPDS card number 04-0783). SEM images (Fig. 6,
(
DTA) of compound 1 single crystals show that the crystalline form

3
308
K. Akhbari et al. / Polyhedron 29 (2010) 3304–3309
ous work, silver nanoparticles were also obtained from silver(I)
nano-coordination polymers (NCPs) [17,23,36] and in this work,
we obtained similar results from a 2D coordination polymer with
argentophilic interactions.
4
. Conclusions
Nanostructures of a 2D silver(I) coordination polymer with a
hemi paddlewheel structure were synthesized by a sonochemical
process and with oleic acid at 453 K. Treatment of the sonochem-
ically synthesized nanostructures of compound 1 with oleic acid
led to the formation of agglomerated nanostructures of 1 from
nanoparticles. The silver nanostructures were fabricated by two
methods; (i) calcination of compound 1 nanostructures, obtained
from the sonochemical process, which led to silver nanostructure
agglomerates from silver nanoparticles and (ii) thermal decompo-
sition of compound 1 nanostructures in oleic acid at 523 K to fab-
ricate silver nanoparticles with an average diameter of 50 nm.
Acknowledgement
Support of this investigation by Tarbiat Modares University is
gratefully acknowledged.
Appendix A. Supplementary data
Supplementary data CCDC 639612 contains the supplementary
crystallographic data for compound 1. These data can be
obtained free of charge via http://www.ccdc.cam.ac.uk/conts/
retrieving.html, or from the Cambridge Crystallographic Data Cen-
tre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-336-
0
33 or e-mail: deposit@ccdc.cam.ac.uk. Supplementary data associ-
ated with this article can be found, in the online version, at
doi:10.1016/j.poly.2010.09.011.
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