Geckeler K.E., Nishide H. (Eds.) Advanced Nanomaterials

7.5 CNT–AuNP Composites 285

Figure 7.27 Experimental procedure, in which

poly(ethyleneimine) possibly interacts with acid - functionalized

MWNTs through electrostatic interaction and a physisorption

process. Reprinted with permission from Ref. [89] .

introducing other reducing agents. More importantly, the dense package of AuNPs

on the surface of CNTs was tailored by simply changing the experimental param-

eters, such as the initial molar ratio of PEI to HAuCl

4

, the relative concentration

of PEI and HAuCl

4

to MWNTs, and both the temperature and duration of the heat

treatment. This approach is anticipated to become universal for preparing com-

posites of CNTs and other noble metals, as well as heterogeneous CNT – AuNP

composite nanowires, and also shows potential for applications such as electronic

nanodevices.

Fullam and coworkers have shown that CNTs can be used as templates for the

formation of Au nanowires – a new type of composite material which may have

the potential for a wide range of applications. The CNT - templated self - assembly

of gold nanocrystals and subsequent thermal processing of the nanocrystal assem-

blies to form continuous polycrystalline gold nanowires extending over many

micrometers were described [90] . The AuNPs were decorated on the surface of the

CNTs, when mixing the CNTs to a dispersion of tetraoctylammonium bromide -

stabilized gold nanocrystals ( ∼ 6 ± 1 nm) in chloroform. A monolayer coverage of

gold nanocrystals on the surface of the CNTs was obtained after precipitation from

solution. It was anticipated that the deposition of Au nanocrystals on the CNT

surface would be similar to that of phase - transfer catalyst - stabilized gold nano-

crystals adsorbed as a monolayer onto the surface of [60]fullerene [91] . Subsequent

heat treatment of the gold nanocrystal - coated CNTs yielded a continuous polycrys-

talline gold nanowire with a CNT core. These ﬁ ndings were of general interest as

they showed that nanometer - scale structures self - assembled from nanocrystals

might subsequently be processed to yield polycrystalline, nanoscale structures.

In contrast to the use of MWNTs to template the assembly of aligned nanopar-

ticles, which is a relatively common practice, Correa - Duarete and coworkers [92]

showed for the ﬁ rst time that the nanorods were assembled with a preferential

286 7 Gold Nanoparticles and Carbon Nanotubes: Precursors for Novel Composite Materials

Figure 7.28 (a – c) TEM images of Au nanorods (average

aspect ratio 2.94), assembled on MWNTs (average diameter

30 nm) at various magniﬁ cations. Reprinted with permission

from Ref. [95] .

string - like alignment on the surface of MWNTs. The group showed that the forma-

tion of uniform electrostatic assembly of Au nanorods on MWNTs occurred in

such a way that the nanorods formed strings with end - to - end contacts (Figure

7.28 ). Such a morphology would result in uniaxial plasmon coupling, and the

nanorods could serve as a label to monitor the alignment of CNTs within polymer

ﬁ lms or other nanostructured systems, as demonstrated through optical absorp-

tion measurements on stretched poly(vinyl alcohol) ﬁ lms loaded with the nano-

composite arrays. Fabrication of the aligned Au nanorods was achieved using

the LBL technique. Prior to the assembly of gold nanorods, the MWNTs were

wrapped with the negatively charged polyelectrolyte PSS, followed by an electro-

static assembly of the positively charged polyelectrolyte PDDA.

A different approach to fabricate MWNT – AuNPs was proposed via the noncova-

lent functionalization of MWNTs with surfactants such as sodium dodecyl sulfate

( SDS ) using the LBL - mediated assembly of a MWNT multilayer ﬁ lm onto indium

tin oxide ( ITO ) - coated glass plates [93] . The supramolecular interactions [94]

between the alkyl chains of the SDS and the surface of the MWNTs leads to a good

dispersion of MWNTs in water and, on the other hand, creates a distribution of

electronic charges at the tube surface. This is very useful for the LBL assembly

of uniform MWNT multilayer ﬁ lms on the solid substrate and the fabrication of

MWNT – AuNP composites. Hence, it was possible to assemble the MWNT mul-

tilayer ﬁ lm onto the ITO plate via the electrostatic interaction of oppositely charged,

SDS - modiﬁ ed MWNTs and polyelectrolyte (e.g., PDDA). The same properties of

the SDS - functionalized MWNTs were also shown to be useful for mediating the

attachment of AuNPs onto the surface of the tubes. This approach to assembling

CNT multilayer ﬁ lms and the resultant composites may both ﬁ nd application in

the development of bioelectronic nanodevices such as biosensors and biofuel cells.

Biju and coworkers [95] used the functionalization of SWNTs to produce a

hierarchical nanoscale composite material of SWNT – AuNPs as well as SWNT –

CdSe – ZnS quantum dot s ( QD s), and studied the photoluminescence properties

of the resulting hybrid materials. The excessive sidewall functionalization of the

SWNTs into nitro and amino derivatives provided water - solubility to the SWNT

7.5 CNT–AuNP Composites 287

Figure 7.29 Steps involved in the functionalization of SWNTs,

including successive conjugation to AuNPs and AFM phase

image of SWNT – AuNP conjugates dispersed on a mica plate.

Adopted and modiﬁ ed according to Ref. [95] ; AFM image

reprinted with permission from Ref. [95] .

derivatives. The AuNPs modiﬁ ed with mercaptoacetic acid, which provides free

surface carboxylic acid groups, were attached to SWNTs through quaternary

ammonium salt formation (Figure 7.29 ). Based on absorption and photolumines-

cence spectroscopic measurements, it was observed that the conjugation of AuNPs

to the SWNT templates induced electronic interactions between the components,

which perturbed their energy states, absorption, and photoluminescence proper-

ties. The hierarchical nanoscale hybrid structures based on the SWNT and nano-

particle hybrid materials, together with an understanding of their optical properties,

288 7 Gold Nanoparticles and Carbon Nanotubes: Precursors for Novel Composite Materials

were suggested to represent promising building blocks for a light - harvesting

system [96] and nanoscale optoelectronic devices.

Another novel method was demonstrated by which to electroporate Gram -

negative bacteria (e.g., Acidothiobacillus ferrooxidans ) through MWNTs [97] . The

addition of MWNTs into a solution containing bacteria and AuNPs, and subse-

quent exposure to microwave radiation, facilitated a rapid transport of AuNPs

across the cell wall, without affecting cell viability. In fact, both cell viability and

growth provided an insight into the stability of cell under microwave exposure,

the reversibility of electroporation via MWNTs, and demonstrated the cells ’ ability

to withstand a high intake of AuNPs. Upon the random addition of MWNTs to a

bacteria – AuNPs solution, both the MWNTs and AuNPs remained uniformly sus-

pended, without any strong tendency to accumulate on the bacterial cells. However,

upon exposure to microwaves, a large fraction of MWNTs and AuNPs was seen

to accumulate on the cell surfaces.

7.6

Applications

It is well known that much attention has been paid to metal nanoparticles based

on their pivotal applications as advanced materials in an ample diversity of areas

such as catalysis, optical devices, nanotechnology, and the biological sciences

[98 – 100] . Today, many applications of metal nanoparticles are close to proﬁ table

implementation, with AuNPs in particular having attracted most attention based

on their potential use in applications such as catalysis [101, 102] , chemical sensors

[103] , biological and/or medical areas [104, 105] , and the miniaturization of elec-

tronic devices due to their unique optical and electrical properties [4] . The applica-

tions of thiol - stabilized AuNPs in catalysis comprise asymmetric dihydroxylation

reactions [106] , carboxylic ester cleavage [107] , electrocatalytic reductions [108] , and

particle - bound ring - opening metathesis polymerization [109] , among others [4] .

These catalytic applications have in common an exploitation of the carefully

designed chemical functionality of the ligand shell, rather than the potential cata-

lytic activity of a nanostructured clean metal surface. From a biological aspect, a

color change of AuNP aggregates, from ruby - red to blue, has been exploited in the

development of a highly sensitive calorimetric technique for DNA analysis, capable

of detecting trace amounts of oligonucleotide sequences. The same effect has also

been used to distinguish between perfectly complementary DNA sequences and

those exhibiting different degrees of base pair mismatches [110] . One of the most

famous potential long - term applications of AuNPs is the fabrication of new (even-

tually small) electronic devices [111, 112] ; for example, a single - electron transistor

action has been demonstrated for systems that contain ideally only one particle in

the gap between two contacts separated by only few nanometers.

CNTs are of great interest due to their unique mechanical, electronic, and optical

properties, as well as their interesting applications [68, 77] . Both, SWNTs and

MWNTs have been investigated in numerous promising areas such as ﬁ eld emit-

7.7 Merits and Demerits of Synthetic Approaches 289

ters [113] , memory elements [114] , sensors [46] , and nanotube aquators [115] . In

order to optimize the applications of CNTs, it is necessary to modify the sidewalls

by chemical functionalization and to attach suitable nanoclusters to the nanotubes

[90, 116] . In this way, functionalized nanoparticles could be used as versatile

building blocks in the construction of nanodevices. An example of this includes

the decoration of AuNPs on to the surface of CNT sidewalls, which has shown

particular promise towards the development of novel, highly, efﬁ cient photoelec-

trochemical cells, fuel cells, or sensor devices. The noble metal nanoparticles in

general – and AuNPs in particular – have become the focal point for many research

groups on the basis of their special optical properties [117] , their unusual electronic

properties, including conductivity by activated electron hopping [118] , and their

remarkably high catalytic activity [119] . Hybrid nanostructures combining these

two types of material might improve these performances, and further extend

the applications.

Considering that the broad spectrum of studies connecting metal nanoparticles

and CNTs composites are mainly focused on the noble metals (e.g., Pt, Pd, Au,

Ag, Ru), it is hardly surprising that the most potential applications of these com-

posite materials are in the ﬁ eld of catalysis. The anchoring of metal nanoparticles

in general (and of AuNPs in particular) to CNTs represents another means of

producing new types of composite materials with useful properties for gas sensors

and catalytic applications [45, 120] . For example, Fasi and coworkers [121] have

shown that AuNPs deposited on the surface of the MWNTs were active catalysts

in the transformation of methyloxirane (Figure 7.30 ).

Methyloxirane, which can react in more than one direction and has a versatile

functionality, is a favorite of synthetic chemists when creating complicated

molecules from relatively simple synthons. It has also been reported that AuNP –

CNT composites have been used as catalysts for some environmentally advanta-

geous reactions [41, 71] . Gold - covered MWNTs were proposed as the basic element

of a glucose biosensor [122] , while the attachment of SWNTs to gold tips not

only allowed observations to be made with both AFM and STM [123, 124] , but

also permitted an investigation of the potential of MWNTs as a solid phase for

the adsorption and concentration of true metal ions [125] . A key element

when exploring the use of nanoparticle – CNT composites as sensors or catalytic

materials is the possibility of an effective and controllable assembly of AuNPs on

the surface of CNTs. Such attachment might also serve to detect the presence of

certain functional groups on the CNT surface, thus proving that the derivatization

had been successful.

7.7

Merits and Demerits of Synthetic Approaches

Several pathways have been introduced to either decorate or attach AuNPs onto

the outer walls of CNTs, including processes of reduction, deposition, and chemi-

cal linking. By comparing and analyzing these different techniques, it can be

290 7 Gold Nanoparticles and Carbon Nanotubes: Precursors for Novel Composite Materials

Figure 7.30 Experimentally proven products obtained in the

ring - opening reaction of methyloxirane by using AuNP – CNT

composite as a catalyst. Reprinted with permission from

Ref. [121] .

concluded that each and every approach has its merits and demerits. Although,

on each occasion the preferred approach can be selected depending on the condi-

tions and speciﬁ c application purposes, a direct reduction or deposition of AuNPs

on the surface of CNTs is generally the easiest and most effective way of ensuring

that large quantities of nanoparticles are coated or deposited onto the CNT sur-

faces. Controlling the shape, size, and distribution of the nanoparticles, as well as

the number deposited on the CNT surface, may be very difﬁ cult when using this

approach, however.

The alternative approach, to link already modiﬁ ed AuNPs with the CNT surface,

is a rather complicated, expensive, multistep procedure that typically would include

the synthesis and modiﬁ cation of AuNPs, chemical modiﬁ cation of the CNTs, and

then linking of the two components. As well as being a very time - consuming

process, the formation of composite materials by covalent linking is highly

complex, as the number of AuNPs anchored covalently to the surface of the CNTs

will be associated with the number of carboxyl groups or other chemical function-

alities of the CNT surface. The major advantages of such a linking procedure are

that the size and shape of AuNPs can be tuned; likewise, under certain conditions

the connection between AuNPs and CNTs is reversible.

7.8 Conclusions 291

The linking of AuNPs to the CNT surface through hydrophobic or electrostatic

interactions may be more beneﬁ cial, as a ﬁ ne dispersion with a high density of

composite materials can be achieved if previously modiﬁ ed AuNPs are deposited

onto the CNT surface in this way. This is especially the case if the CNTs are pre-

modiﬁ ed by polymers or surfactants, which enhance such interactions.

7.8

Conclusions

Owing to their unique geometry, exceptional properties and large surface

area, CNTs are excellent candidates as support materials for metal nanoparticles

in general, and for AuNPs in particular. The blending of these materials to

create new composites should in turn lead to the generation of new hybrid materi-

als with applications in catalysis, electronics, and nanotechnology. Moreover,

the formation of such composites can be achieved either by the deposition or

attachment of AuNPs onto the CNT surface, or by their entrapment within the

nanotube cavities.

In this chapter, we have discussed not only the synthetic approaches, assembly

and interaction related to AuNP – CNT composites, but also their potential applica-

tions. The strategies used to create hybrid materials are variable and depend on

the requirements and applications of the composite product. The interaction of

CNTs with AuNPs provides the ability to generate signiﬁ cant composite deriva-

tives with numerous potential applications, including advanced catalytic systems,

biosensors, electronic nanodevices, probe tips for scanning probe microscopy,

electrochemical sensors, and gas sensors. It is perhaps surprising to note that most

potential applications for these composites involve catalytic systems, with the high

surface area : volume ratio, excellent mechanical properties, thermal and electrical

conductivity, chemical stability and inertness, and lack of porosity forming the

basis of CNTs being used to support AuNPs. Indeed, with remarkable advances

having been made in the area of catalysis, the efﬁ cient industrial use of AuNP –

CNT composites as catalysts will inevitably attract much interest in the future. Yet,

perhaps the most signiﬁ cant point for the future development of these hybrid

materials would be to determine inﬂ uential synthetic protocols and methodologies

for the fabrication of composite materials with reproducible properties and per-

formances. Extensive studies are also required with regards to the possible re - use

of the composites as catalysts, and consequently attention must be focused on

their catalytic reaction mechanisms. Moreover, the spectrum of catalytic activity

for AuNP – CNT composites must be extended to the production of industrially

important compounds. In addition, simple but effective methods must be identi-

ﬁ ed to deposit gold nanowires and nanorods onto the CNT surface, creating high -

density packaging suitable for both electrical and electronic applications. The

electron - transfer phenomenon that occurs between deposited AuNPs and CNTs

should also be addressed in greater detail, as this may open new opportunities for

the development of optoelectronic and light - to - energy - conversion devices. Another

292 7 Gold Nanoparticles and Carbon Nanotubes: Precursors for Novel Composite Materials

future task will be to explore multicomponent systems that contain several differ-

ent types of structurally cooperating component, including combinations of metal

semi - conductor nanoparticles. This may lead in turn to the development of new

materials and structures with functional properties that are superior to those of

currently available, “ conventional ” materials. It is envisaged, therefore, that the

future will bear witness to a whole range of novel alloys related to AuNP and CNTs,

while the list of applications of CNTs that have been functionalized with AuNPs,

other metals, metal oxides and semiconductor nanoparticles, should expand sig-

niﬁ cantly in the near future. Undoubtedly, the great attraction of these composite

materials will lead to many research groups undertaking increasing numbers of

investigations into their properties and practical applications.

In conclusion, it is clear that the extraordinary diversity of structures, properties,

and applications of the AuNP – CNT composites will stimulate many investigations

into the fundamental properties and applications of these materials. Moreover,

such studies will be conducted in association with other molecular, inorganic, and

biological areas of research involving chemistry, physics, biology, and medicine.

Acknowledgments

The authors acknowledge ﬁ nancial support from the “ Brain Korea 21 ” project from

the Ministry of Education, Science, and Technology, as well as from the World -

Class University (WCU), Ministry of Education, Science and Technology (MEST)

of Korea (Project No. R31 - 2008 - 000 - 10026 - 0).

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