A water-based synthesis of octahedral, decahedral, and icosahedral Pd nanocrystals

DOI: 10.1002/anie.200703755

Source and publish data:

Angewandte Chemie - International Edition p. 9279 - 9282 (2007)

Update date:2022-08-29

Topics:

Authors:

Lim, Byungkwon

Xiong, Yujie

Xia, Younan

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Article abstract of DOI:10.1002/anie.200703755

Shapes from water: Pd nanocrystals with controllable shapes are synthesized by reducing a Pd salt with citric acid in aqueous solution. Citric acid favors the formation of octahedra, icosahedra, or decahedra (see picture) owing to its strong binding to the {111} facets of Pd. Shape control of these nanocrystals is readily accomplished by adjusting the amounts of Na₂PdCl₄ precursor and citric acid added to the reaction mixture. (Figure Presented)

Full text of DOI:10.1002/anie.200703755

Angewandte

Chemie

DOI: 10.1002/anie.200703755

Shape-Controlled Nanoparticles

A Water-Based Synthesis of Octahedral, Decahedral, and Icosahedral

Pd Nanocrystals**

Byungkwon Lim, Yujie Xiong, and Younan Xia*

Noble-metal nanocrystals have attracted increasing attention

owing to their potential use in catalysis, electronics, and

biology.^[1]The physicochemical properties of these nano-

crystals are highly sensitive to their shape and size. For

example, the number, location, and intensity of surface

plasmon resonance (SPR) bands of Au and Ag nanocrystals

display a strong correlation with the shape of the particle.^[2]

Furthermore, the reactivity and selectivity of metal nano-

catalysts depend strongly on the crystallographic planes

exposed on the surface of the particles and can therefore be

tuned by controlling the morphology of these particles.^[3]An

exquisite shape control of noble metal nanocrystals is there-

fore highly desirable for tailoring their properties and is also

required for high performance in many applications.

Palladium nanocrystals are widely used as primary

catalysts for the low-temperature reduction of automobile

pollutants, hydrogenation reactions, and organic reactions

such as Suzuki, Heck, and Stille coupling.^[4]Pd is also well-

known for its remarkable capacity in hydrogen absorption.^[5]

Most of these applications are related to the adsorption of

hydrogen onto the surface of Pd nanocrystals. Recent studies

have revealed that the hydrogen-absorption capacity and

surface-enhanced Raman scattering (SERS) activity of Pd

nanocrystals are dependent on their shape.^[6,7]A wide variety

of Pd nanocrystals, including cuboctahedra, cubes, rods, and

bars, have been prepared to date, mostly by the polyol

method, in which ethylene glycol (EG) serves as both a

reductant and a solvent.^[8]However, the major products of a

polyol synthesis are often restricted to shapes such as

truncated cubes or cuboctahedra, owing to the fast reduction

and growth rate associated with the polyol process.

an octahedron and a decahedron are two particle shapes that

face-centered cubic (fcc) noble metals can potentially take,

although high-yield syntheses of these two types of nano-

structures are yet to be realized for Pd.^[11]

The formation of a particular shape in the synthesis of

metal nanocrystals is often explained in terms of the presence

of surfactants or capping agents,^[8,10]which can change the

order of free energies of different facets through their

interactions with the metal surface in a solution-phase

synthesis.^[12]This alteration may significantly affect the

relative growth rates of different facets and thus lead to

different morphologies for the final products. To achieve

shape control of a nanocrystal, however, not only the

thermodynamics or physical restrictions imposed by the

surface stabilizing agent must be considered, but also

nucleation and kinetics. Herein, we report on a water-based

system for the facile synthesis of Pd nanocrystals with various

shapes by reducing a Pd precursor with citric acid. Citric acid

or citrate ion can also serve as a capping agent in this system

thanks to their strong binding to the {111} facets of Pd.^[10,13]

More specifically, we demonstrate that citric acid favors the

formation of a structure such as an octahedron, icosahedron,

or decahedron whose surface is covered by {111} planes. We

also demonstrate that the shape of the Pd nanocrystals can be

controlled by varying the concentrations of the Pd precursor

and citric acid. We have been able to selectively produce Pd

octahedra, icosahedra, and decahedra in high yields using this

simple approach.

The synthesis was conducted in an aqueous solution

containing Na₂PdCl₄, PVP, and citric acid at 908C for 26 h.

Na₂PdCl₄and PVP are used as a Pd precursor and a stabilizer,

respectively. Citric acid serves as a mild reductant and a

capping agent in a manner similar to the mechanism of a

conventional citrate-based synthesis of gold or other noble-

metal nanoparticles.^[14]Several hours into the reaction, the

color of the solution changed from light yellow to deep brown,

thereby indicating the formation of Pd nanocrystals. We

explored a range of concentrations for both Na₂PdCl₄(5.8–

17.4 mm) and citric acid (0.13–0.39m) to determine the

optimal conditions for the preparation of Pd nanocrystals

with different shapes.

An alternative water-based system could provide a more

convenient and environmentally benign route to the synthesis

of noble-metal nanocrystals, because it does not involve toxic

organic solvents or reagents. Recently, our group reported the

syntheses of Pd thin plates and icosahedra in aqueous solution

using poly(vinyl pyrrolidone) (PVP) and citric acid as the

reducing agent, respectively.^[9,10]It is worth pointing out that

[*] Dr. B. Lim, Dr. Y. Xiong, Prof. Y. Xia

Department of Chemistry, University of Washington

Seattle, Washington 98195 (USA)

Figure 1 shows scanning electron microscopy (SEM) and

transmission electron microscopy (TEM) images of Pd

octahedra synthesized in the presence of 7.3 mm Na₂PdCl₄

and 0.13m citric acid with a molar ratio of the repeating unit

of PVP to the Pd precursor of 5:1. The sample contains

approximately 90% octahedra with edge lengths of approx-

imately 20 nm and around 10% other shapes, including

triangular plates and decahedra (see also Figure S1 in the

Supporting Information). Although an octahedral shape has

E-mail: xia@chem.washington.edu

[**] This work was supported in part by grants from the ACS (PRF-

44353-AC10) and the NSF (DMR-0451788), and a subcontract from

GEMSEC, an MRSEC program on the UW campus sponsored by

NSF. Y.X. is a Camille Dreyfus Teacher Scholar (2002–2007). B.L.

was partially supported by the Postdoctoral Fellowship Program of

the Korea Research Foundation (KRF).

Supporting information for this article is available on the WWW

under http://www.angewandte.org or from the author.

Angew. Chem. Int. Ed. 2007, 46, 9279 –9282

ꢀ 2007 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

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Communications

Figure 1. a, b) SEM and c, d) TEM images of Pd octahedra synthesized

Figure 2. a–c) TEM images of three samples prepared under the same

conditions as those in Figure 1 except that the reaction time was

shortened to 1, 3, and 20 h, respectively. d) TEM image of Pd

icosahedra synthesized under the same conditions as in Figure 1

except that the concentration of Na₂PdCl₄was reduced to 5.8 mm. The

insetin (d) shows an SEM image of the Pd icosahedra.

at90 8C for 26 h in the presence of 7.3 mm Na₂PdCl₄and 0.13m citric

acid. The molar ratio of the repeating unit of PVP to the Pd precursor

is 5:1. The SEM image in (b) was taken by tilting the substrate by 308.

The insetin (b) shows an SEM image of Pd octahedra whose C₃axes

are oriented perpendicular to the substrate. The inset in (d) shows a

schematic illustration of the octahedron.

been previously reported for Au, Ag, and Pt nanoparticles,^[15]

this is the first synthesis of Pd octahedra as a majority product.

The SEM images (Figure 1a,b) clearly show the octahedral

shape bound by {111} planes. The Pd octahedra exhibit sharp

edges and corners as well as smooth surfaces. Figure 1c,d

shows typical TEM images of the Pd octahedra. These

octahedra exhibit two differently projected shapes, namely a

rhombus and a hexagon, depending on their orientation

relative to the electron beam. An octahedral particle lying on

a flat surface against one of its faces rather than a corner or

edge has a projected hexagonal shape, as shown in Figure 1d.

Both SEM and TEM images show the absence of octahedra

with truncated corners.

We monitored the evolution of the particle shape by

removing samples at various reaction times and then viewing

them by TEM. Figure 2a–c shows TEM images of Pd

nanoparticles sampled at 1, 3, and 20 h, respectively. At t =

1 h, the sample mainly contains small particles with a nearly

spherical profile, which could be either cuboctahedral or

twinned seeds. At t = 3 h, particles with an octahedral shape

and sizes of less than 10 nm are observed. These results

indicate that the octahedra probably evolve from cuboctahe-

dral seeds. After t = 20 h all the small nanocrystals below a

certain size have disappeared while the larger octahedra have

become bigger, thereby suggesting the involvement of

Ostwald ripening in the growth process. We also found that

the shape of the Pd nanocrystals is highly sensitive to the

concentration of the Pd precursor. For instance, reducing the

concentration of Na₂PdCl₄by 20% and maintaining the

concentration of citric acid and the molar ratio of PVP to Pd

precursor at 0.13m and 5:1, respectively, gives icosahedra as

the major (> 80%) species in the product (Figure 2d),

whereas increasing the concentration of Na₂PdCl₄by 20%

gives octahedra (see Figure S2 in the Supporting

Information). These results indicate that formation of

single-crystal Pd octahedra is more favorable than that of

icosahedra at a relatively high initial concentration of Pd

precursor.

A fivefold twinned decahedron, which can be described as

an ensemble of five tetrahedral single crystals with twin-

related adjoining faces, is one of the shapes that are enclosed

by {111} facets.^[16]To achieve further shape control of Pd

nanocrystals, we searched for reaction conditions that lead to

decahedral nanoparticles and found that increasing the

concentrations of the Pd precursor and citric acid above

those that lead to octahedra and icosahedra allowed us to

obtain Pd decahedra in high yields. Figure 3 shows SEM and

TEM images of Pd decahedra synthesized in the presence of

17.4 mm Na₂PdCl₄and 0.39m citric acid. Both types of images

reveal that decahedral nanoparticles (> 80%) with a regular

pentagonal symmetry and sizes of 25–40 nm are produced in

addition to a small amount of triangular plates. The presence

of fivefold twinning from the center of the decahedral particle

can be seen in the magnified TEM image (Figure 3d).

To elucidate the formation mechanism of Pd decahedra,

we conducted the reactions at different concentrations of

citric acid whilst maintaining the concentration of Na₂PdCl₄at

17.4 mm. Figure 4 shows TEM images of four samples that

illustrate the strong dependence of the yield of Pd decahedra

on the concentration of citric acid. At a relatively low

concentration of citric acid (0.13m), the sample contains

mainly Pd octahedra (Figure 4a). However, the yield of

decahedra increases drastically up to 90% as the concen-

tration of citric acid is increased from 0.20m to 0.39m

(Figures 4b–d). This result indicates that the capping effect

of citric acid favors the formation of decahedra.

9280 www.angewandte.org

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Angew. Chem. Int. Ed. 2007, 46, 9279 –9282

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Angewandte

Chemie

atoms N less than 309), while decahedral and cuboctahedral

seeds predominate at larger sizes (N > 309).^[18]When the

concentration of Pd precursor is low the icosahedral seeds

remain small for a long period of time due to the slow addition

of Pd atoms, which means that icosahedra are formed in high

yields in a slow reduction process (Figure 5). When the

Figure 3. a, b) SEM and c, d) TEM images of Pd decahedra synthesized

in the presence of 17.4 mm Na₂PdCl₄and 0.39m citric acid. The molar

ratio of the repeating unit of PVP to the Pd precursor is 5:1. The inset

of (b) shows a schematic illustration of the decahedron.

Figure 5. Reaction pathways that lead to Pd nanocrystals with different

shapes.

concentration of Pd precursor is increased, however, the

generation of Pd atoms becomes faster, and most seeds will

take a decahedral or cuboctahedral shape because of their

increased size. The formation of decahedra with sizes larger

than 20 nm is not favorable because of the internal strain in

the lattice caused by twin defects.^[19,20]Moreover, these

defects make decahedral seeds much more susceptible to

oxidative etching by the O₂/Cl^Àpair than single-crystal seeds,

which results in their dissolution.^[20,21]This means that single-

crystal octahedra are more likely to remain in the final

product, as can be seen in Figure 1. The yield of decahedra

can be improved by increasing the concentration of the

capping agent (citric acid or citrate ion in this case), as

demonstrated in Figure 4. Citric acid or citrate ion can reduce

the surface energies of the {111} facets of a decahedron by

binding strongly to them and thus compensate for the extra

strain energy caused by twinning. In addition, these species

can block the oxidative etching by competing with oxygen

adsorption on the surface of the Pd decahedra or exhausting

the adsorbed oxygen atoms. Accordingly, the decahedra are

preserved and thus accumulate throughout the reaction. We

expect that the methodology established for this Pd system

might be extendible to other fcc noble metals such as Au, Ag,

and Pt, although some modifications to the experimental

conditions might be required.

Figure 4. TEM images of samples prepared under the same conditions

as those in Figure 3 except that the citric acid was added to the

reaction mixture at different concentrations: a) 0.13, b) 0.20, c) 0.26,

and d) 0.39m. The decahedra in (d) are similar to those shown in

Figure 3.

As we and others have demonstrated for the silver system,

the crystallinity of a seed plays a key role in determining the

shape of a particle.^[2c,17]The Pd nanocrystallite or seed can

take a single-crystal, single-twinned, or multiple-twinned

structure (including both decahedral and icosahedral struc-

tures) in the solution phase. As we have shown in a previous

study, the use of a mild reducing agent such as citric acid

(rather than EG) can promote the formation of twinned

seeds.^[10]It has also been shown by simulation that icosahedral

seeds are favored for Pd at small sizes (with the number of

In summary, Pd nanocrystals with controllable shapes

have been synthesized by reducing a Pd salt with citric acid in

aqueous solution. The distribution of single-crystal and

multiple-twinned seeds can be altered at the nucleation

stage by adjusting the amounts of Na₂PdCl₄and citric acid

added to the reaction mixture. A number of polyhedra

covered by {111} facets (octahedron, icosahedron, and

Angew. Chem. Int. Ed. 2007, 46, 9279 –9282

ꢀ 2007 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

www.angewandte.org

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Communications

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Experimental Section

In a typical synthesis of Pd nanocrystals, poly(vinyl pyrrolidone)

(PVP; MW= 55000, Aldrich) and citric acid (Fisher) were dissolved

in water (8.0 mL) in a 25-mL, three-necked flask equipped with a

refluxcondenser and a teflon-coated magnetic stir bar and heated to

908C in air with stirring. Sodium tetrachloropalladate(II) (Aldrich)

was dissolved in water (3.0 mL) at room temperature, and this

aqueous solution of Na₂PdCl₄was then rapidly added to the flask with

a pipette. The molar ratio of Na₂PdCl₄to the repeating unit of PVP

was kept at 1:5 in all experiments. The reaction mixture was heated at

908C in air for 26 h and then the product was collected by

centrifugation, washed once with acetone, and finally washed twice

with ethanol to remove excess PVP.

TEM images were recorded with a Phillips 420 transmission

electron microscope operating at 120 kV. SEM images were recorded

with an FEI field-emission scanning electron microscope (Sirion XL)

operating at an accelerating voltage of 10 kV. Samples for TEM and

SEM studies were prepared according to a reported method.^[10]The

yield of each type of nanocrystal was calculated from 200–300

nanoparticles.

Received: August 15, 2007

Published online: October 30, 2007

Keywords: nanostructures · palladium · polyhedra ·

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9282 www.angewandte.org

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Angew. Chem. Int. Ed. 2007, 46, 9279 –9282

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Article Doi

A water-based synthesis of octahedral, decahedral, and icosahedral Pd nanocrystals

DOI: 10.1002/anie.200703755

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