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This Review is focused on the recent progresses in the synthetic approaches to the precise control
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of structure, size, shape, composition and multi-functionality of metal and metal alloy
nanoparticles. Many of these strategies have been developed based on colloidal methods, and to
limited extent, the galvanic and other methods. The shape, size and composition often govern
the chemical and catalytic properties that are important for electrochemical energy applications.
The structure–property relationship and the design in controllable structures and morphologies
for specific reactions such as oxygen reduction reaction (ORR) are emphasized.
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composition and thus, physical and chemical properties.10,11 pristine faces. In addition, by introducing the twin defects
For instance, heterostructures of Pt–M (M = Au, Pd, Ru) during the nucleation and growth stages, the total free energy
bimetallic NPs show much improved catalytic performance can be reduced to a level lower than that of the Wulff
toward oxygen reduction,12–18 formic acid oxidation,19,20 and polyhedron.8 Decahedron and icosahedron are two kinds of
methanol oxygen,21–25 compared with Pt catalysts. such morphologies.
Generally, metallic NPs with specific morphologies are The colloidal metal and metal alloy NPs, especially platinum
prepared by controlling the anisotropic growth using surfactants, and platinum-based alloys have been the choice of catalysts
or based on the intrinsic growth habits of crystals. The lattice in many important chemical and electrochemical reactions
defects existing in crystal seeds are helpful for making symmetry- including oxygen reduction reaction (ORR) and direct methanol
reduced morphologies, such as one-dimensional (1-D) rod and oxidation reaction (MOR). It is well known that catalytic
two-dimensional (2-D) plate. Surfactants typically play the roles reactions are sensitive to the electronic structure and surface
in tuning surface energy and particle dispersity through the atomic arrangement or coordination, which can be controlled by
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interaction between the organic groups of surfactants and solvent tuning the composition and shape of NP catalysts.18,25,37 Thus,
molecules. Through surfactant and metal surface interaction, engineering the structures of colloidal alloy NPs is a rational
certain crystal plane of a given NP is often preferentially stabilized approach to improve the properties or to obtain desirable
by surfactants through strong binding in comparison with other functions.38,39
crystal planes.11 The growth based on crystal habits is
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Fig. 2 TEM images showing the effect of molar ratios between HDA
and DDD on the formation of Pt multipods: (a) 2.5 : 1, (b) 1.6 : 1,
(c) 1.1 : 1, (d) 0.83 : 1, (e) 0.55 : 1 and (f) 0.27 : 1, respectively.
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lowest energy positions, but also constrain the routes for the
diffusion on surfaces.52–54 Depended on the initial position,
the atom may diffuse on terraces, along edges, or at corners of
the surface. The diffusion rate can be described as the
following:55
Vt = V0exp(Et/kT) (1)
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the kinetics, such as atomic diffusion, leading to anisotropic the particle-mediated growth, but also shows that besides the
growth. For example, when temperature decreases, atomic OA growth, an Ostwald ripening (OR)/coarsening process is
diffusion becomes weak and the growth of Pt crystals becomes occurring simultaneously (Fig. 6c and d). In the OR process,
anisotropic and the morphology transforms from fractal to atoms diffuse on the surface to decrease the surface area and
dendrite and eventually trigonal or hexagonal shape thus the overall surface energy. When the sizes of NPs are
(Fig. 4c).63 This process can be simulated by DLA method, as similar, the atoms diffuse toward each other to fill the pit area
shown in Fig. 4d and e.55 With the decrease of the diffusion between the two NPs. If the size is very different, the atoms in
energy barrier, the atomic diffusion becomes easy accordingly, the small NP diffuse to the large one, as shown in Fig. 6d. This
thus the morphology changes from fractal to dendrite and result matches very well with molecular dynamics (MD)
eventually the predicted polyhedral shapes, matching very well simulations for Ag–Pt alloy NP-mediated growth.42
with experimental data. In the synthesis of colloid metal nano- Many factors can have important effects on the particle-
crystals, most of the precursors are metal ions in solution, so the mediated growth process. By controlling these factors, various
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concentration gradient,64 reduction rate65 and diffusion57 all mesocrystals with new structures and morphologies are
have important effects on the growth. obtainable by using NPs as the building blocks. Uniform
apple-shaped and spherical core–shell ZnO mesocrystals
2.3 Particle-mediated growth were made from nanoplates, driven by the intrinsic dipole
interaction.79,80 Similarly, sea urchin-, flower- and meatball-like
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f = kTr2/3/3pZR (2)
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Fig. 6 (a) Illustration of the window for the cell used for in situ TEM study of nanocrystal growth in solution. (b) A series of video frames
captured at 12.1, 12.1, 24.2, and 77.0 s in the liquid cell for (A, B, and C) a particle growing by coalescence with a smaller particle and (D, E, and F)
a particle growing through steady accretion of atoms. (Adapted with permission from ref. 77. Copyright 2009 American Association for the
Advancement of Science.) (c) Illustration of encapsulated solution between graphene sheets and (d) in situ TEM images showing the two types of
growth modes. (Adapted with permission from ref. 78. Copyright 20012 American Association for the Advancement of Science.)
Theoretical calculation and experimental observation both conditions. It has been used as a powerful approach to the
show that these factors have important effects on the particle- crystal engineering of complicated nanostructures.92 Yang and
mediated AgPt nanowire growth, as shown in Fig. 9c.42 coworkers developed a simple etchant system for silver NPs.93
By carefully tuning the amount and composition of etchant,
2.4 Defects in seed-induced anisotropic growth they successively controlled the transformation of octahedral
silver NPs into truncated structures with etched edges and then
Control of shape can also be achieved through the seed-
back to cubic structures with slightly rough features.28 In
mediated growth. Since metals and metal alloys are often
addition, at a high concentration of NH4OH/H2O2 the selective
cubic phase, defects, especially twinning, need to be created
etching of {100} surfaces becomes pronounced, resulting in
in the initial seed crystals in order to generate symmetry-
concave features that eventually form octapods, which have
reduced morphology in a colloidal synthesis. In other words,
the same symmetry as that for the starting silver octahedral
the stacking faults break the symmetry in face-centered cubic
nanocrystals (Fig. 11a). Tilley et al. has found that the high-
metals and metal alloys, and enable the formation of anisotropic
concentration acetylacetonate species from the reaction
nanocrystals with 1-D, 2-D and 3-D morphologies. The final
precursor may also act as the etchant.94 It is preferred to etch
shapes depend on both the type and number of defects. The
and dissolve the platinum from the {100} facets rather than
functions of defects in seeds have been recently
{111} facets due to the high surface energy bound by {100}
reviewed.8,9,30,82–87 Therefore, only several examples are selected
facets. This process led to a morphological transformation of Pt
and discussed here. Fig. 10 shows that the shapes of Pt
NPs from initially formed nanocubes to octapod-like nano-
nanocrystals formed depending on the type and number of twin
crystals (Fig. 11b). Yang et al. reported that the core–shell
planes in seed crystals. The seeds with cuboctahedral structure
Au@Ag nanorods can be etched by FeCl3 to produce a number
lead to the formation of anisotropic needles of multipods, while
of dumbbell-like Ag-tipped Au nanorods.92 The selective
the single- and penta-twined seeds lead to the formation
etching from the side of the core–shell nanorods was attributed
of tripod-,29 pentapod- and rod-like49 structures. Seeds with
to the increased reactivity of these facets due to the low level of
two or more parallel twin planes or stacking faults form
surface passivation by surfactants (CTAB). Oxygen molecules
triangular or hexagonal nanoplates/prisms.49,88–90 The single
can selectively shorten the single-crystalline Au nanorods95 and
twinned seeds also grow to right bipyramid NPs by controlling
generate hollow structures from Pd nanocubes by mild oxidative
the growth environments.91
etching.96 Xiong97 and Xia98 demonstrated that the etching
process triggered by citric acid led to the transformation of
2.5 Chemical etching on colloidal NPs
Ag NPs from nanocubes to nanospheres, respectively. Jin and
Chemical etching of as-made NPs can be used to generate coworkers found that H2O2 can be used as a mild etchant to
complex architectures by using different etchants and reaction controllably dissolve Ag atoms from the Ag/Au bimetallic
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2.6 Others
Besides the above colloidal approaches, there are a few other
methods that have been developed. Electrochemical synthesis
and gas reducing agent using carbon monoxide (CO) are two
of the more powerful methods for controlling the shape of Fig. 12 (a) TEM and (b–c) HRTEM images of Pt hollow nanocubes
nanoparticles. prepared by the electrochemical methods. Inset of (a) shows the
corresponding potential cycling profile. Individual hollow cubes
2.6.1 Electrochemical methods. Sun and Wang’s group imaged under various tilting angles with respect to the direction of
used an electrochemical method to obtain Pt tetrahexahedral the imaging beam are shown in (c). (Reprinted with permission from
(THH) nanocrystals that are bounded by 24 high-index facets ref. 110. Copyright 2010 American Chemical Society.)
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Table 1 Colloidal metal and metal alloy NPs synthesized in the presence of foreign metallic additives
{111} + {110},
Au PDDA in glycol 164
{111}
Ag(I)
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a
PPDA = poly(diallyldimethylammonium chloride), CTAC = cetyltrimethylammonium chloride, DDAB = didodecyldimethylammonium
bromide, TEG = tetra(ethylene glycol), OTAC = octadecyl trimethyl ammonium chloride.
nanocrystals ultimately led to the formation of different morphol- of tetrahexahedra (convex cubes) when all the other conditions
ogies. Recently, Zheng et al. found that Fe(III) ions etched the Pd were kept the same.35,36,162 When NaCl were used as addi-
seeds at the early stage of the reaction to induce the formation of tional additives, trisoctahedral Au NPs with a single twin
branched mesocrystalline Pd nanocorolla.181 plane and high-indexed facets were produced in the presence
CTAB and CTAC are the common used surfactants for the of CTAC.182 Interestingly, Br was found to promote the
synthesis of noble metal NPs. In recent years, various kinds of formation of concave nanocubes rather than a convex form of
noble metal NPs with high-indexed surfaces have been pre- Pt or Pt alloys from their initial cubic morphology. Although
pared using CTAB and CTAC as capping agents. However, it the mechanism for Cl and Br mediated growth is still largely
is interesting that CTAB and CTAC always show an opposite unclear, a generally acceptable explanation is that both
effect configuration as capping agents for the preparation of Br and Cl are able to slow down the reduction of
NPs, although these two capping agents contain the same precursors,183,184 which is a prerequisite for the formation of
cation surfactant group. CTAC was found to facilitate the noble metal concave or convex nanocubes by combining with
formation of concave cubes, while CTAB led to the formation other additives, such as Ag+,33 Na2H2P2O7,185 and Cu2+.166
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Fig. 16 SEM images of (A) octahedra, (B) rhombic dodecahedra, 5.2 Core–shell based bimetallic nanocrystals
(C) truncated ditetragonal prisms, and (D) concave cubes synthesized
from solutions at Ag+/Au3+ molar ratios of 1 : 500, 1 : 50, 1 : 12.5, and In principle, the formation of multimetallic core–shell NPs or
1 : 5, respectively (reprinted with permission from ref. 163. Copyright 2011 core–shell like heterogeneous nanostructures including
American Chemical Society). Scale bars: 200 nm. dendrite, particle-on-particle, raspberry, or flower is usually
thermodynamically favored.30 A lower critical energy barrier
Besides Br and Cl, introducing methylamine allows concave for the heterogeneous nucleation of second metal on the
Pt nanocrystals having {411} high-index facets to be prepared in preformed NP or core than that of homogenous nucleation
presence of PVP.186 Huang et al. have demonstrated a Mn3O4 provides the driving force for the synthesis of core–shell
NP-induced synthesis of polycrystalline twinned Pt NPs and structured NPs. The formation process can be roughly divided
length-controlled Pt NRs with high index facets.187 into three major types: layer-by-layer, island-on-wetting layer,
and island growth modes, depending on the overall excess
energy of the system, which is related to the surface and
5. Further understanding the formation of alloy interfacial energy terms, and the strain energy because of
and bi-metallic nanocrystals lattice mismatch at the interface. In a colloidal synthesis
process, the heterogeneous deposition of a metal or metal
5.1 Alloying through atomic diffusion
alloy on the core occurs through one of the above three growth
Control of atomic diffusion in bimetallics is an effective way to modes to form core–shell or core–shell like nanostructures in
synthesize alloy NPs with designed sizes and compositions. the presence of capping ligands (Fig. 18a), while the metallic
One such process involves mixing independently prepared cores can exist in either ordered or disordered form.210
colloidal particles of pure metal A and B, and then heating Recently, electrochemical dealloying methods, chemical-
or sonicating in the presence of capping agents.198–202 As reaction-driven reconstruction approaches and UPD have
shown in Fig. 17, after mixing the two colloidal suspensions, been developed for controlling bi- or multimetallic core–shell
NPs aggregate to form heterogeneous structures in order to like NPs, as shown in Fig. 18b and c.211–213 In a typical UPD
reduce the global Gibbs free energy.203 Coarsening of NPs process for making Pt monolayer shell on selected metals, Cu
with small particles results in the formation of core–shell NPs. is used as the sacrificial layer (Fig. 18b).214,217 A Pt monolayer
Finally, the alloy NPs were formed because of the atomic can be deposited on different metallic NPs through the
diffusion under favored reaction conditions (such as high galvanic reaction.211,214 The core–shell NPs prepared through
temperatures).199 Both the size and composition could be electrochemical dealloying can be due to the redox potential
fine-tuned based on the NP precursors.202 For example, difference between the two metal elements. The atom with the
monodisperse AgAu alloy NPs were made through interfacial low redox potential can be oxidized and dissolved into
diffusion of core/shell structured Ag/Au NPs using a solution by electrochemical treatment. For instance in AgPt
solvothermal synthesis method.198 In this case, Ag NPs were alloy NPs, after electrochemical removal of the more reactive
first made by thermal reduction of AgNO3 in oleylamine. metal, such as Ag, core–shell like NPs surface rich in Pt could
These Ag NPs were used as seeds for the deposition of Au be generated (Fig. 18c).212 Besides the electrochemical
NP through the reduction of HAuCl4 with oleylamine at 50 1C. approach, reacting gases, such as CO, NO, O2, and H2 can
The AgAu alloy NPs formed after the core/shell structured selectively cause certain metal elements enriched on the outer
Ag/Au NPs were heated at 100 1C in oleylamine to facilitate surface of alloy NPs (Fig. 18d).215 When Pd/Rh alloy NPs
Ag and Au counter diffusion in the core/shell structure. were exposed to an oxidizing gas atmosphere of NO, the
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Table 2 Colloidal metal and metal alloy NPs synthesized in the presence of inorganic ion and neutral molecule additives
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Table 2 (continued )
{110} + {100} +
SCN (KSCN) Pd CTAB in H2O 195
{111}
a
DMF = dimethylformamide, TBAB = NBu4Br.
core–shell NPs with Rh enriched surface were obtained. Rh DGmix,NPs(r) = DGV,AB (XADGV,A + XBDGV,B)
atoms were ‘‘pushed’’ back to the core, if the NP was exposed = DHmix TDSmix–Dgmix(r) (4)
to a reducing gas of CO.
where XA and XB are the molar fractions of atom A and B
over the total atoms, respectively. This change results in the
5.3 Effects of particle size on alloy phase formation
increase of surface energy (Dgmix(r)). Qualitatively speaking,
With NP size decreases, the ratio of surface to total atoms when the NP size decreases, the corresponding surface energy
increases, and many size-related properties such as catalytic and term increases and the mixture Gibbs free energy term
electronic properties change accordngly.216–219 At the same time, decreases. Thus, the bimetallic alloy phase may form more
the increasing ratio of surface energy to total free energy facilitates easily in nanometer scale than in bulk. For immiscible
the formation of alloy phases between two metals.30 Alloy phases bimetallic materials, when the NP size decreases below a
were readily detected with two immiscible metals in bulk, such as certain value, stable alloy phases may form. As illustrated
Ag–Pt,220 Au–Pt,221 Au–Fe,222 Pt–Ru223 and Pb–Sn,224 when in Fig. 19, NPs composed of metal A and B (which
they are made into crystals with diameters of a few nanometers. are immiscible in bulk) are able to mix with each other to
For example, Ag–Pt binary alloys do not form stable alloy for form alloy NPs when the size is below a critical value (rc).
compositions between BAg2Pt98 and Ag95Pt5 at oB400 1C in For quantitative analysis, the enthalpy part of Gibbs free
the bulk through high-temperature processing methods. energy should have major effect on the formation of alloy
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Fig. 18 Schematic illustrations of (a) synthesis of bimetallic core–shell or core–shell-like NPs from metal precursors and (b–d) methods for the
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synthesis and structural control of core–shell multimetallic NPs: (b) Underpotential deposition (UPD) and replacement, (c) electrochemical
de-alloying, and (d) reaction-driven process (adapted with permission from ref. 210. Copyright 2011 Wiley-VCH).
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catalysts is another major problem due to the ripening and truncated octahedron populations of 70%, 90% and 100%
grain growth of the metal particles and the corrosion of carbon were obtained, with the remaining particles being cubes
supports during operation.254 Various nanostructures, such as enclosed by {100} facets (Fig. 24). The Pt3Ni catalyst with
nanowires/nanotubes,128,140,255–261 nanosheets,157,262–265 and 100% truncated octahedra, i.e., the sample with the highest
multipods29,84,130,266–270 have been examined to address the portion of (111) surface among the three, shows the highest
durability and activity issues. ORR catalytic activity, which was about 4-times higher in area
In addition, research efforts have been devoted to the specific activity than the Pt/C catalysts.
development of high-index facet Pt and Pd catalysts since Recently, both cubic and octahedral Pt–M (M = Co, Fe,
the report of high performance for ORR by Pt tetrahexahedral Ni, Pd) alloy catalysts (on carbon supports) were prepared
nanocrystals.105–107,185,186,191,271,272,31 The high-index facets from nanocrystals synthesized using the GRAILS method and
are shown to have a high percentage of low-coordinated through surface activation using a short-chain amine.116 As
atoms, steps, edges, and kinks on the surface of these shown in Fig. 25, the Pt3Ni octahedral NP catalysts were
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structures, all of which are potentially active sites.273–275 A bounded by {111} facets and the Pt3Ni cubic NPs bounded by
cubic Pt concave nanocrystal, which is composed of 24 {100} facets. The Pt3Ni octahedral NP has a higher activity
identical kite-shaped {411} faces, is a good example than that of cubes towards the ORR. A five-time improvement
(Fig. 23).186 The exposed high-index {411} facets in the in ORR specific activity over the Pt/C catalysts was found for
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concave Pt nanocrystals were attributed to the excellent the octahedral Pt3Ni nanocrystals.
electrocatalytic activity in the oxidation of both formic acid
and ethanol.186 6.3 Bimetallic heterostructures with three-dimensional
nanostructures
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