Colloids and Surfaces A: Physicochem. Eng.

Aspects 360 (2010) 612

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Colloids and Surfaces A: Physicochemical and

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

Microwave-assistant synthesis of inorganic particles from ionic liquid precursors

Jianmei Pang a , Yuxia Luan a, , Qingzhong Wang b , Jimin Du c , Xiaoqing Cai a , Zhonghao Li b
a
School of Pharmaceutical Science, Shandong University, Jinan, Shandong Province 250012, PR China
b
School of Materials Science and Engineering, Shandong University, Jinan, Shandong Province 250061, PR China
c
School of Chemistry and Chemical Engineering, Anyang Normal University, Henan Province, PR China

a r t i c l e i n f o a b s t r a c t

Article history: The structurally similar ionic liquid precursors are explored for synthesis of inorganic particles by the
Received 12 November 2009 microwave heating method. During the synthesis, the ionic liquid precursors have multi-functions such
Received in revised form 19 January 2010 as reactant, solvent and template. Specically it has good adsorbing property for microwave to result in a
Accepted 28 January 2010
fast synthesis. It demonstrates that a wide variety of metal oxide or hydroxide particles with uniform size,
Available online 4 February 2010
morphology could be synthesized from tetrabutylammonium hydroxide (TBAH) or tetraethylammonium
hydroxide (TEAH) ionic liquid precursors by the microwave heating method. The formation mechanism
Keywords:
of the synthesized particles is proposed based on the experimental results.
Ionic liquid precursor
Inorganic particles 2010 Elsevier B.V. All rights reserved.
Microwave

1. Introduction liquid crystal precursors (ILCPs) which serve as solvent, reactant

Metal oxide or hydroxide particles, especially transition metal
oxides or hydroxides with sizes in the low micrometer to
nanometer range, are important materials for many applica-
tions. Catalysis, magnetic storage, labels and contrast agents for
biomedicine, and battery technology are only a few examples
of nanoscale metal oxide or hydroxide applications [1]. Differ-
ent synthesis approaches for metal oxide or hydroxide particles
are developed in the last few years with respect to achiev-
ing control of crystallite size, shape, and assembly behavior [2].
However, in spite of all the progress, the preparation of nanocrys-
talline metal oxides or hydroxides remains rather time- and also
energy-consuming. One possibility to accelerate the synthesis
process is the use of microwave irradiation because the use of
microwave heating offers an immense reduction of the reaction
time in comparison to traditional heating in an oil bath or in an
autoclave. However, microwave-assisted preparation routes for
inorganic materials are not yet as popular as for organic com-
pounds.
Room-temperature ionic liquids (ILs) are attractive envi-
ronmentally benign solvents for organic chemical reactions,
separations, and electrochemical applications [35]. The advan-
tages of ILs in inorganic synthetic processes have been gradually
realized [616]. Particularly, ionic liquids can act as solvents, reac-
tants, and templates for the fabrication of inorganic materials [8,9].
The structurally related ionic liquid crystals are dened as ionic
Corresponding author. Tel.: +86 531 88382007; fax: +86 531 88382731.
E-mail address: yuxialuan@sdu.edu.cn (Y. Luan).
and template for the synthesis of inorganic materials. For exam-
ple, Taubert et al. have used ILCPs for the fabrication of CaF2
tubes, CuCl plates and Au plates [1721]. According to the origi-
nal ILCPs approach [17], the concept for fabrication of inorganics
from ionic liquid precursors (ILPs) is developed [22,23]. The ionic
liquid precursor is the ionic liquid which can act as solvent and
reactant precursor for the growth of the inorganic materials. We
have recently shown that the IL tetrabutylammonium hydroxide
(TBAH) is an efcient ILP for the fabrication of nanostructured ZnO
particles [2430].
There are large positive ions with high polarizability in ILs,
which makes ILs very good solvents for absorbing microwaves.
Therefore, the use of microwave heating in ILs for the synthesis of
inorganic nanomaterials has some advantages over other solvents
[10]. The current paper proposed a facile route for the synthe-
sis of inorganic materials from ionic liquid precursors with the
assistance of microwave heating. It demonstrates that a wide vari-
ety of metal oxides or hydroxides with uniform size, morphology
could be synthesized from tetrabutylammonium hydroxide (TBAH)
or tetraethylammonium hydroxide (TEAH) ionic liquid precursors
with the assistance of microwave heating. The advantage of our
approach is that there is no need for the synthesis of complex
metal organic precursors prior to the metal oxide or hydroxide
synthesis. Specically, interesting metal oxide or hydroxide par-
ticles could be synthesized with a fast and simple route without
any additional template agents like surfactants. This work is a con-
tribution on applying ionic liquid precursors with multi-functions
in the formation of the inorganic particles. That is, the ionic liq-
uid precursor has good property for adsorbing microwave to result
in a fast synthesis and the ionic liquid precursor can work as

0927-7757/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.colsurfa.2010.01.062
 J. Pang et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 360 (2010) 612
Fig. 1. XRD patterns of the samples prepared in TBAH ionic liquid precursor. (a) -
Ni(OH)2 , (b) CuO, (c) -Co(OH)2 , (d) Cd(OH)2 , (e) La(OH)3 , (f) -Fe2 O3 , (g) 3PbOH2 O
(*)and PbO (#), (h) hydrohausmannite (*) and Mn3 O4 (#).
Fig. 2. SEM and TEM images of the products synthesized in TBAH ionic liquid. (a) 3PbOH2 O and PbO, (b) Fe2 O3 , (c) hydrohausmannite and Mn3 O4 , (d) Co(OH)2 . Inset in (b)
is a ED pattern of Fe2 O3 .
7
reactant, solvent and template during the growth of inorganic
materials.
2. Materials and methods
2.1. Materials
Tetrabutylammonium hydroxide (TBAH, 50%, w/w aqueous
solution), tetraethylammonium hydroxide (TEAH, 25% ,w/w aque-
ous solution), Mn(NO3 )2 4H2 O, Fe(NO3 )3 9H2 O, Co(NO3 )2 6H2 O,
Ni(NO3 )2 6H2 O, Cu(NO3 )2 3H2 O, La(NO3 )3 6H2 O, Cd(NO3 )2 4H2 O,
Pb(NO3 )2 were used without further purication.
2.2. Synthesis in TBAH
In a typical synthesis, 0.456 mmol of the respective metal nitrate
was dissolved in 1 g of water to form a clear solution. Then the
above solution was injected to 0.5 g of TBAH solution (50%) in 10 ml
tube. Finally, the tube with the solution was heated in a microwave
oven (Galanze WD300) for 1 min. The products were recovered
by repeated centrifugation and washing with water and ethanol,
respectively, and dried at 60 C for 5 h.
2.3. Synthesis in TEAH
In order to make a comparison with the samples synthesized
from TBAH, we adjust the TEAH concentration as the same as the
TBAH solution. For the typical synthesis, 0.456 mmol of the respec-
tive metal acetate was dissolved in 0.935 g of water to form a clear
8 J. Pang et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 360 (2010) 612

Fig. 3. SEM and TEM images of the products synthesized in TBAH ionic liquid. (a) Cd(OH)2 , (b) CuO, (c) Ni(OH)2 , (d) La(OH)3 .

solution. Then the above solution was injected to 0.565 g of TEAH
solution (25%) in 10 ml tube. Finally, the tube with the solution
was heated in a microwave oven (Galanze WD300) for 1 min. The
products were recovered by repeated centrifugation and wash-
ing with water and ethanol, respectively, and dried at 60 C for
5 h.
2.4. Characterization
X-ray diffraction was done on a Rigaku Dmax-rc X-ray diffrac-
tometer with Ni ltered Cu K radiation. SEM was done on a Hitachi
SU-70 FESEM operated at 10 kV. TEM was done on a Hitachi H-
800 transmission electron microscope at an accelerating voltage of
150 kV.
3. Results and discussion
Fig. 1 shows the representative XRD patterns for the samples
obtained in TBAH ionic liquid. The XRD results indicate that the syn-
thesized metal oxide or hydroxide particles are well crystallized.
Also part of the samples exhibit broad reections which indicates
that small particles can be synthesized by the current microwave
heating method.
Fig. 2 shows scanning electron microscopy (SEM) and trans-
mission electron microscopy (TEM) data of some samples from
Pb, Fe, Mn, Co nitrate reaction in TBAH ionic liquid. Based on the
SEM and TEM images it is found that Pb, Fe and Co nitrate lead to
3PbOH2 O/PbO, Fe2 O3 and Co(OH)2 particles in plate shape with
the size of 1102 469, 153 46 and 220 36 nm, respectively. The
size is determined by measuring the length of the particles based

Table 1
Morphology and size of the products synthesized in TBAH ionic liquid by microwave heating approach.

Product Morphology Length or diameter (nm) Width (nm)

3PbOH2 O and PbO Plates 1102 469 696 399

-Fe2 O3 Plates 153 46
-Co(OH)2 Plates 220 36
Cd(OH)2 Plates 153 46
Aggregations 46 19a
CuO Plates 533 100 193 15
-Ni(OH)2 Networks 40 5 61
La(OH)3 Quasi-spheres 83
Hydrohausmannite and Mn3 O4 Plates 76 23
Quasi-spheres 25 6
a
Represents the size of the quasi-spheres which construct the aggregates.
 J. Pang et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 360 (2010) 612
Fig. 4. SEM and TEM images of the products synthesized in TEAH ionic liquid. (a) 3PbOH2 O/PbO, (b) Fe2 O3 , (c) hydrohausmannite/Mn3 O4 , (d) Co(OH)2 . Inset in (c) is a TEM
image.
on the calibration of the SEM/TEM images. Typical electron diffrac-
tion pattern of Fe2 O3 displays rings, which are usually assigned to
polycrystalline materials. However, in the current case, the rings
are not continuous, but rather consist of closely packed discrete
spots. Such spotted lines are characteristic of the diffraction of an
assembly of single crystalline particles with discrete orientations,
where the spots of each single crystal pattern superimpose. Fur-
ther evidence for the single crystalline nature of the particles can
also be found in the fact that the particles shown in Fig. 2b have a
well-dened habit.
For Mn nitrate, there are plates plus the quasi-sphere nanopar-
ticles, in which the size of the plate is 76 23 nm and the size of
the quasi-sphere nanoparticle is 25 6 nm. The XRD experiment
shows that hydrohausmannite and Mn3 O4 coexist in the synthe-
sized sample.
Fig. 3 shows SEM and TEM images of the samples from Cd, Cu,
Ni and La nitrate reaction in TBAH ionic liquid. From Fig. 3a it is
found that Cd nitrate leads to Cd(OH)2 particles with plates plus
the quasi-sphere nanoparticle aggregates, in which the size of the
plate is 153 46 nm and the size of the quasi-sphere nanoparti-
cle is 46 19 nm. The quasi-sphere particle represents the particle
which is not in well spherical shape. Fig. 3b shows that the Cu
nitrate results in CuO plates with the length of 533 100 nm
and the width of 193 15 nm. Fig. 3c shows Ni(OH)2 nanorod-
constrcuted dendrimers form with the Ni nitrate as the reactant,
and the rod diameter is 6 1 nm. For the La nitrate, the product is
La(OH)3 particles in quasi-sphere shape with the size of 8 3 nm
(Fig. 3d).
9
Table 1 summarizes the electron microscopy data for all the
samples synthesized in TBAH ionic liquid by the microwave heating
method. The iron oxide particles obtained here have a well-dened
plate which is different from other authors reports usually with
the formation of spherical particles. Our approach is a simple and
therefore technologically interesting alternative for the fabrica-
tion of well-dened Fe2 O3 nanoparticles. Examples of plate-like
nanocrystals, especially from CuO and Co(OH)2 have already been
reported. However, these platelets were synthesized by using dif-
ferent time-consuming methods and it is still a great challenge
to construct plate-like particles of all these materials using the
same procedure with a fast formation. As a result, our ILP-based
microwave heating approach provides a generic fast approach for
the controlled fabrication of a wide variety of metal oxide and
hydroxide nanoparticles with dened morphologies. Moreover,
the -Ni(OH)2 rod-constructed dendrimers reported here are a
new developed morphology. The plate-like or dendrimer parti-
cles obtained using our ILP microwave heating approach might
bring about new applications or improved performance in electro-
chemistry, magnetism, and catalysis. For example, our -Ni(OH)2
plates are candidates for magnetic materials or electrodes in high-
density batteries. The CuO, Co(OH)2 plates could nd applications
in magnetic materials, heterogeneous catalysis, gas sensors, elec-
trode materials, or in eld emitters. Overall, these results show that
the synthesis from ionic liquid precursor by the microwave heating
approach provides a exible and rapid approach for well-dened
metal oxide and hydroxide nanoparticles with uniform shapes and
relatively uniform sizes.
10 J. Pang et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 360 (2010) 612

Fig. 5. SEM and TEM images of the products synthesized in TEAH ionic liquid. (a and b) Cd(OH)2 , (c) CuO, (d) Ni(OH)2 . Inset in (b) is a ED pattern of the crystals shown in the
image. Inset in (d) is a TEM image of Ni(OH)2 .

For comparison, we also perform the synthesis in TEAH ionic
liquid which has a similar structure as that of TBAH using the same
procedure described above. Here the mole concentration of the
TEAH ionic liquid in aqueous solution is the same as the TBAH sys-
tem. The added metal nitrate amount is also same as the TBAH
system. Fig. 4 shows SEM and TEM images of some samples from
Pd, Fe, Mn and Co nitrate reaction in TEAH ionic liquid. From Fig. 4a
it is found that 3PbOH2 O/PbO thick plates form with the length of
6.5 3.5 m and the width of 3.7 1.3 m. The result is somehow
different from the TBAH system in which thin plates form. Also the
size of the plates are much larger than that from TBAH ionic liq-
uid. Fig. 4b shows that Fe2 O3 quasi-spheres form with the size of
10 2 nm. This is completely different from the TBAH ionic liquid
in which plate particles form. Fig. 4c shows the Mn nitrate leads to
hydrohausmannite/Mn3 O4 quasi-sphere particles with the diame-
ter of 6 1 nm. For the Co nitrate, like the products from TBAH ionic
liquid, Co(OH)2 plates form with the size of 833 326 nm (Fig. 4d).
Fig. 5 shows SEM and TEM images of the samples from Cd, Cu,
Ni nitrate reaction in TEAH ionic liquid. Fig. 5a and b shows the
SEM and TEM images of the products from Cd nitrate, demonstrat-
ing the formation of well-dened Cd(OH)2 plates with the size of
143 38 nm. The inset in Fig. 5b is a selected area showing electron
diffraction pattern of the crystals, which veries that the synthe-
sized plates are single crystals. It is found that the result is different
from the TBAH system in which only a few plates form. Therefore
the TEAH ionic liquid can control the Cd(OH)2 plate formation much
better than the TBAH ionic liquid. Fig. 5c shows that the CuO plate
particles with the length of 260 153 nm and width of 151 76 nm
are obtained for Cu nitrate reactant which is similar to the TBAH
system although the size is different. Fe nitrate results in Fe2 O3
quasi-spheres with the size of 10 2 nm. This is completely differ-
ent from the TBAH ionic liquid in which Fe2 O3 plate particles form.
Fig. 5d shows that Ni(OH)2 plates with the diameter of 25 5 nm
form for Ni nitrate reactant. The product is different from that
obtained in TBAH ionic liquid. Well-dened plates form in TEAH
while nanorod-constructed dendrimers form in TBAH ionic liquid.
For the La nitrate, La(OH)3 quasi-spheres with the size of 7 2 nm
are obtained, which is similar to that from the TBAH ionic liquid.

Table 2
Morphology and size of the products synthesized in TEAH ionic liquid by microwave heating approach.

Product Morphology Length or diameter Width

3PbOH2 O and PbO Plates 6.5 3.5 m 3.7 1.3 m

-Fe2 O3 Quasi-spheres 10 2 nm
-Co(OH)2 Plates 833 326 nm
Cd(OH)2 Plates 143 38 nm
CuO Plates 260 153 nm 151 76 nm
-Ni(OH)2 Plates 25 5 nm
La(OH)3 Quasi-spheres 7 2 nm
Hydrohausmannite and Mn3 O4 Quasi-spheres 40 5 nm
 J. Pang et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 360 (2010) 612
Scheme 1. Proposed formation process for the plate-like particles.
Table 2 summarizes the electron microscopy data for all the
samples synthesized in TEAH ionic liquid by the microwave heating
method. Comparing the results from the TBAH and TEAH ionic liq-
uids based on Tables 1 and 2, it is clear that there is difference for the
inorganic particles formed from the two structurally similar ionic
liquids. For example, we can nd that the size of most of the par-
ticles from the TEAH is smaller than those from TBAH ionic liquid.
Moreover, there are several completely different shapes between
several products from these two ionic liquids. For example, the
nickel hydroxide formed in TEAH is plates while rod-constructed
dendrimers form in TBAH. The TEAH can result in large-scale syn-
thesis of cadmium hydroxide plates while there are only a few
plates formed in TBAH ionic liquid. The hydrohausmannite/Mn3 O4
particles are in quasi-sphere shapes in TEAH while there are plate-
like particles formed plus the quasi-sphere particles in TBAH. For
the iron oxide, the result is completely different from each other
for the two used ionic liquids: Fe2 O3 quasi-sphere particles form in
TEAH while well-dened plates form in TBAH ionic liquid.
In principle, the crystal growth process consists of nucleation
and growth, which are inuenced by the intrinsic crystal structure
and the external conditions including the kinetic energy barrier,
temperature, time and capping molecules, and so forth [31]. The
crystal structures of most of the plate-like particles (Cd(OH)2 ,
Ni(OH)2 , Co(OH)2 ) synthesized in the work are hexagonal in nature.
In general, for the materials of hexagonal structure, the anisotropic
growth along the c-axis is available to form the 1D nanostructures.
However, herein the nanoplates have been fabricated from the ionic
liquid precursor route, indicating that ionic liquid precursor plays
the critical role in the formation of nanoplates. As for Cd(OH)2 ,
Ni(OH)2 and Co(OH)2 , the structure of the crystal is interpreted as
the following [32]. The hydrogen atoms are isolated between lay-
ers of MO6 octahedra along the c-axis, where M is a divalent cation
such as Cd, Ni and Co. The MO6 octahedra are compressed along
the c-axis, creating a distorted hexagonal close packing of oxygens.
Each oxygen is hydrogenated, and the OH groups lie along the c-
axis resulting in the negative charge of the surface on the primary
nucleus. The formation process for the plate-like particles can be
explained as the following (Scheme 1). First the seed crystal forms
due to the reaction of the metal salt with the ionic liquid. During the
crystal growth process, the positive cations with the carbon chain
from the ionic liquid precursor preferably adsorb on the (0 0 0 1)
plane of the seed crystal due to the Coulombic force, which slows
down crystal growth along the [0 0 0 1] orientation. Accordingly,
the intrinsically anisotropic growth of nucleus along the [0 0 0 1]
direction is substantially suppressed and the crystal growth then
proceeds sideways, leading to the formation of plate-like particles,
which is similar to the formation of the ZnO plate reported in our
previous work [28].
For some of the particles synthesized from TBAH and TEAH
ionic liquids, they have different morphologies. Although the dif-
ference in Coulombic force interaction between the cation of the
ionic liquid and the negative surface of the nucleus may result in
the difference in the synthesized particle, it cannot explain well for
the dendrimers formed in TBAH while plate-like particles formed in
TEAH. Therefore we deduce that the formation process might also
be inuenced by the different aggregates formed by these two ionic
11
represents the cation of the ionic liquid.
liquids in the solution. The structure of TBAH and TEAH ionic liquid
is similar although the length of the carbon chain is different. These
ionic liquids are with cation head and carbon chain group, there-
fore they have the aggregation behavior similar to the surfactant. It
is well-known that the length of carbon chain strongly inuences
the aggregation behavior of the surfactant [33]. The aggregates in
the solution might have the function like the soft template for the
growth of the inorganic crystals. That is the template function for
these two ionic liquids are different which might also inuence the
crystal growth of Ni(OH)2 . The primary results show that there is
no liquid crystal formed in these two ionic liquids, therefore the
template function might be attributed to the micelles formed by
these ionic liquids. The study of the detailed aggregation behavior
of these two ionic liquids is underway.
4. Conclusion
In conclusion, here we use the structurally similar ionic
liquid precursors for the synthesis of inorganic particles with
the assistance of microwave heating. The ionic liquid precur-
sors cannot only act as solvent, reactant and template for the
growth of inorganic crystals but also adsorb microwave ef-
ciently to result in a fast synthesis of interesting materials.
This microwave-assistant synthesis concept based on the ionic
liquid precursors could have potential application for the syn-
thesis of other kinds of materials including doped crystals and
could be an technically important contribution for the materials
area.
Acknowledgements
This work is supported by National Natural Science Foundation
of China (NSFC, No. 20803044, No. 20803043), the Excellent Young
Scientist Foundation of Shandong Province (BS2009CL002) and the
Scientic Research Foundation for the Returned Overseas Chinese
Scholars, State Education Ministry.
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