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Chapter 1

Introduction

Chapter 1 Introduction

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1.1 Introduction to Nanomaterials

The materials having their structured components with one or more dimensions

in the nanometer range are designated as nanomaterials. Although, these materials have

a long history (Faraday, 1857), but it was only in last few decades (Kroto et al., 1985;

Keribeg & Vollmer, 1995; Porel et al., 2007; Abargues et al., 2008; Leong et al., 2008;

Meng et al., 2008; Ramesh et al., 2009) that this field has touched new heights. This

became possible only due to the invention of revolutionary imaging methods and

sophisticated experimental techniques, which made the characterization of these

materials easy. Nanomaterials are broadly classified into three categories depending on

their one, two and three dimensions, respectively in nanometer range. The materials,

such as thin films, surface coatings, etc. where only one of three dimensions is in

nanometer range, are categorized as one dimensional nanomaterials. Materials with two

of the three dimensions in nanometer scale, like nanowires, nanotubes, etc. and those

having all the three dimensions in nanometer range, e.g. quantum dots, fall in the

category of two and three dimensional nanomaterials, respectively.

The nanostructured materials have attracted the attention of researchers mainly

due to their unique and distinctive properties. Materials, with their constituents having

dimensions in micrometer scale, exhibit the properties mostly similar to that of their

bulk counterpart. As the dimensions are reduced to nanometer scale, the properties of

the materials, like electrical, thermal, optical, mechanical, etc. are changed significantly

(Cao, 2004). Such changes in the properties of the material at the nanometer scale are

originated mainly due to the following reasons:

(a) Surface to Volume Ratio: The ratio of surface area to volume is actually a

measure of the percentage of molecules or atoms that are on the surface of the

material as compared to the total number of molecules or atoms in the entire piece

of material. As an illustration, figure 1.1 clearly demonstrates how the surface area

increases with the reduction in the dimensions of the material. For the single cube

of side 1 cm, the volume 1 cm3 comprises the surface area 6 cm

2. With the

consistent reduction in the dimensions of the cube, a proportional increase in

surface area is clearly evident. For the cube of side 0.5 cm, 0.25 cm and 100 nm,


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the surface area increases from 12 cm2 to 24 cm

2 and finally, to 6,00,000 cm

2,

respectively for the same volume of 1 cm3. Such an increase in surface area of the

material constituents leads to the increased number of atoms on the surface, which

are more reactive than those present in its bulk. This is because of the reduced

number of nearest neighbours of the surface atoms, presence of unsaturated sites

or dangling bonds at the surface etc., which result in their enhanced surface

energy. This is responsible for the change in chemical and physical properties of

nanoparticles as compared to their bulk counterpart (Nei & Emroy, 1997; Shipway

& Willner, 2001; Wang et al., 2004).

Figure 1.1: A schematic representation of the increase in surface area of the cube

with reducing dimensions for the same volume of 1 cm3.

(b) Quantum Size Effect: When the particle size is reduced and attains the limit

of the Bohr’s radius, its electronic energy structure changes from continuous

energy bands to discrete energy levels (Kubo, 1962; Cottey, 1971; Ventra et al.,


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2004), as shown in figure 1.2. Such a transition is termed as the quantum size

effect (Daniel & Astruc, 2004). This is the major cause, which is responsible for

the modification in the properties of materials at nanometer scale. Also due to this,

the continuous optical transitions between the electronic bands become discrete

and the properties of the nanomaterials become size-dependent (figure 1.2) (Wang

and Herron, 1991; Bharagava et al., 1994; Keribeg and Vollmer, 1995) unlike to

that for bulk materials. For example, colloidal solution of gold nanoparticles has a

deep red colour, which becomes progressively yellowish with increasing particle

size. Such unique properties lead to the wide applications of nano-scale materials

into the emerging areas of technological importance (Pillai et al., 2007; Matheu et

al., 2008; Atwater and Polman, 2010; Christopher et al. 2012; Liu et al., 2013; Qi

et al., 2013).

Figure 1.2: A schematic representation of electronic energy levels in atoms, molecules,

clusters, nanoparticles and bulk.


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1.2 Synthesis of Nanomaterials

Nanomaterials can be synthesized either by bottom-up or top-down approach, as

discussed below. Under the situation, when both top down and bottom up processes are

involved, the technique is referred to as hybrid approach. Figure 1.3 highlights a

schematic representation of bottom-up and top-down approach.

a) Bottom‒up Approach: According to this approach, constituents of the material

are arranged into more complex assemblies atom‒by‒atom or molecule‒by-

molecule or cluster-by-cluster (Klabunde, 2001), like that of the growth of a

crystal, till the desired dimensions of the material are achieved. Synthesis of

nanoparticles by electro-deposition, vapor phase deposition, sol-gel, ion beam

epitaxial technique, etc. are some examples of the bottom-up approach (Cao,

2004). This approach generally provides nanostructures with better homogeneity

in chemical composition and precise control on their size and shape.

Figure 1.3: A schematic representation of Bottom‒up and Top‒down approach.


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b) Top‒down Approach: In this approach, the material constituents with larger

dimensions are processed to reduce their size until the nanoscale dimensions are

achieved. The top-down approach (Klabunde, 2001; Whitesides & Love, 2001;

Schmid, 2004) often involves the methods, like ball milling, sputtering, etc.

However, the limit up to which the size can be reduced depends on the process

involved.

1.3 Nanocomposites

The direct use of nanoparticles in different applications is limited because of

their instability due to their high surface to volume ratio, easily oxidizing nature and

contamination to impurities besides the problems associated in their handling due to

their small size (Henglein, 1993). Such difficulties can be resolved by embedding the

nanoparticles into suitable host matrix supplementing the additional benefit of

manipulating the shape and organization of nanoparticles (Biswas et al., 2004; Jiang et

al., 2007). This new class of materials, generally named as nanocomposites, takes the

advantage of both the host matrix as well as of the embedded nanoparticles.

Depending upon the nature of the host material and embedded nanoparticles,

nanocomposites are generally classified into the three combinations, i.e. Organic-

Organic, Organic-Inorganic and Inorganic-Inorganic. In Organic‒Organic combination,

both the host matrix and nano-fillers are of organic nature. Suitable examples are

polymers based host matrices dispersed with nanoparticles of biomaterials, conducting

polymers, etc. In Organic‒Inorganic combination, the host matrix and nano-fillers are

of organic and inorganic nature, respectively. Nanocomposites of thermoplastic

polymers dispersed with carbon nanotubes, metal nanoparticles, etc. fall in this

category. Inorganic‒Inorganic combination contains both host matrix and filler

particles of inorganic nature. The relevant examples include ceramic or metal based host

matrices with the dispersion of metal nanoparticles, oxide form of nanoparticles, etc.

1.4 Polymer‒Metal Nanocomposites

Among the nanocomposites, the polymer‒metal nanocomposites have gathered a

lot of interest because of their potential applications in many diverse fields of science


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and technology (Mayer, 2001; Corbierre et al., 2005; Porel et al., 2005; Sih & Wolf,

2005; Zhu & Zhu, 2006; Porel et al., 2007; Abargues et al., 2008; Leong et al., 2008;

Meng et al., 2008; Ramesh et al., 2009; Hariprasad & Radhakrishnan, 2010; Ramesh &

Radhakrishnan, 2011; Singh et al., 2012; Sandeep et al., 2013; Qi et al., 2013). This is

because of the excellent inherent properties of the polymers (Darraud et al., 1997; Ruck

et al., 1997; Hong et al., 2001; Lee et al., 2001; Thompson, 2001; Liu et al., 2002;

Singh, 2002; Fink, 2004; Singh et al., 2005; Kondyurin & Bilek, 2008; Hadjichristov et

al., 2009) as host matrix coupled with the unique features of metal nanoparticles (Yu et

al., 1997; Link & El-Sayed, 1999; Mohamed et al., 2000; Peng et al., 2000; Jin et al.,

2001; Hao et al., 2002; Jin et al., 2003).

1.4.1 Polymers as Host Matrices

Polymers, due to their extraordinary properties, such as their easy

processability, light weight, flexibility and mouldability, etc. are best suited materials to

be utilized as host matrices for the synthesis of nanocomposites. Further, due to high

chemical reactivity, the oxidation of nanoparticles occurs readily leading to their

agglomeration, which finally results into their larger structures. Therefore, any

stabilizing agent is required to enhance their chemical stability retaining their basic

properties. A proper choice of the polymer facilitates environmentally safe synthesis

without the requirement of any additional stabilizing agent (Nadagouda & Varma,

2007). Also suitable combinations of polymers as host matrices and nanoparticles as

fillers lead to the synthesis of nanocomposites possessing novel catalytic, conductive,

magnetic or optical properties (Balan & Burget, 2006).

1.4.2 Metal Nanoparticles

Metals exhibit high electrical and thermal conductivity and thus, have

tremendous applications in diverse disciplines. The main interest of researchers towards

metallic particles lies due to the demonstration of their unique and brilliant colours

when their size is reduced to nano-scale. Such a variety of colours is observable due to

the interaction of light with metal particles when their size becomes smaller than the

wavelength of light (Faraday, 1908). Therefore, metallic nanoparticles act as excellent


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chromophores and show plasmonic band in the visible and near infrared region of

electromagnetic spectrum (Toshima & Yonezawa, 1998; Huang et al., 2004;

Namboothiry et al., 2007; Dahal, 2010). Nanoparticles of noble metals such as gold,

silver, platinum and copper have been extensively studied as these particles form stable

dispersions and find applications in photography, biological labeling, catalysis, sensors,

optoelectronics and photonics (Wohltjen & Snow, 1998; De et al., 2000; Kim et al.,

2001; Gudiksen et al., 2002; Krasteva et al., 2002; Obare et al., 2002; Zamborini et al.,

2002; Kang et al., 2005; Sonnichsen et al., 2005; Lee & El-Sayed, 2006; Wang &

Halas, 2006; Zhang et al., 2006; Sharma et al., 2009). In addition, these nanoparticles

show excellent optical properties, which find many scientific applications (Barnes et al.,

2003; Naryanan & El-Sayed, 2005; Eustics & El-Sayed, 2006; Homola, 2006; Hu et al.,

2006; Ozbay, 2006; Pillai et al., 2007; Awazu et al., 2008; Matheu et al., 2008; Larsson

et al., 2009; Atwater & Polman, 2010; Garcia, 2010).

1.5 Surface Plasmon Resonance

Surface Plasmon Resonance (SPR) is defined as the collective oscillation of

conduction band electrons at the metal surface when the electromagnetic radiation of

wavelength comparable to the size of the particles is incident on the metal surface.

Figure 1.4 schematically shows the origin of surface plasmon resonance of a spherical

metallic nanoparticle.

In general, when the electromagnetic radiation falls on the metal surface, it

displaces the electron cloud of the conduction band from the positive nuclei giving rise

to the surface charge distribution, as illustrated in figure 1.4. Due to this surface charge

distribution, restoring force due to the Columbian attraction between positive and

negative charge center comes into picture, which causes the oscillations of the dipole

charges with the periodic phase reversal of the electromagnetic radiation. When the

dipole oscillating frequency matches with the frequency of incident electromagnetic

radiation, a resonance is occurred and the metal particles on the surface absorb the

energy; the phenomenon is known as surface plasmon resonance absorption. The

energy corresponding to this absorption band depends on the free electron density,

shape & size of the nanoparticle and the dielectric function of the surrounding medium.


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In case of noble metal nanoparticles, like Cu, Ag and Au, this SPR absorption band falls

in the visible region of the electromagnetic spectrum resulting in their optical response

novel for various applications (Atwater & Polman, 2010; Garcia, 2010).

Figure 1.4: Schematic of plasmon oscillation for a spherical nanoparticle showing the

displacement of the conduction electron charge cloud relative to the nuclei

1.6 Unique Features of Polymer‒Metal Nanocomposites

As discussed in the above section, polymer‒metal nanocomposites combine the

remarkable properties of metal nanoparticles and inherent characteristics of polymer

matrix to make them important candidates for various applications, highlighted as

under:

Metal nanoparticles dispersion in the polymer matrix improves the optical,

mechanical and thermal properties of polymers, which are very important for


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their use in applications, like photonics, sensors, solar cells, optoelectronics,

coating, etc. (Tokizaki et al., 1994; Wang et al., 2005; Gradess et al., 2009).

Non-linear optical properties shown by polymer‒metal nanocomposites find

applications in non‒linear optical devices, electro-optics, etc. (Maier et al.,

2003; Lu et al., 2006).

The surface plasmon behaviour of metal nanoparticles depends on the shape &

size of nanoparticles and the surrounding environment of embedded

nanoparticles. By changing these parameters, the surface plasmon of metal

nanoparticles embedded in polymer matrix can be tuned, which find applications

in biological sensors, filters, optical switching devices, etc. (Caseri, 2000;

Biswas et al., 2004; Xia & Halas, 2005; Srivastavas et al., 2008).

When nanoparticles embedded in a dielectric matrix, like polymer, are excited

by light, the absorption of light and subsequent surface plasmon oscillations lead

to the strongly enhanced electric field (Sarychen and Shalaev, 2000) within the

nanoparticles and the interparticle gaps. Such unusual excellent optical features

of these nanocomposites find their applications in high efficiency solar cells

(Grangvist, 2003), infrared photo detectors, sensors, and solar control glazing

windows, etc.

The superparamagnetism shown by magnetic nanoparticles can be explored by

combining magnetic nanoparticles with polymers, which makes them excellent

materials for magneto‒optical devices, magnetic tapes, magnetic recording,

electromagnetic wave absorbers, etc.

The combination of low refractive index of polymer and high refractive index of

metal nanoparticles can be utilized in antireflective coating, high refractive

index lenses, optical fibers, waveguides, etc. (Fang et al., 2005; Althues et al.,

2007; Li et al., 2010).

The Surface Enhanced Raman Scattering observed in polymer‒metal

nanocomposites can be explored in applications, such as active Raman scattering

substrates (Erturk et al., 1983; Wang & Li, 1997; Li et al., 2010).


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Further, the properties of polymer‒metal nanocomposites can be regulated

through various treatments like gamma, ultraviolet, X-rays, ion beam irradiation etc.

(Gavade et al., 2010; Shah et al., 2010; Gavade et al., 2011; Puiso et al., 2011; Singh et

al., 2011). Due to the complexity of the phenomenon involved, it is not possible to

probe the overall damage directly; rather one can study individual effects of radiation

damage, e.g. chemical changes, structural changes or changes in its mechanical, optical,

electrical properties, etc. To understand the basic mechanism responsible for these

changes, one must know the interaction process of these radiations with matter as

discussed in the next section.

1.7 Interaction of Ionizing Radiations with Matter

The ionizing radiations include all kinds of electromagnetic and corpuscular

radiations, e.g. UV‒rays, X‒rays, gamma rays, ion beam, etc. with energies appreciably

greater than the dissociation energy of the bonds present in the material.

1.7.1 Electromagnetic Irradiation

Electromagnetic radiations, while traversing through a material medium, transfer

their energy (Evans, 1955; Chapiro, 1962; Leo, 1994) to the medium as a result of

photoelectric absorption, Compton scattering and pair production processes. These

radiations do not produce ionization directly but lose their energy to the target material

by the absorption of photons through any of the processes mentioned above and results

into the creation of fast moving electrons. These electrons as a result of their interaction

inside the medium produce secondary electrons and so on. Since electromagnetic

photons do not lose their energy in a continuous manner and are simply attenuated;

therefore, the entire bulk structure of the material gets modified after electromagnetic

irradiation. The energy transferred by the electromagnetic rays, especially in polymers,

is responsible (Sinha et al., 2001; Saad et al., 2005; Saqan, 2007; Zaki, 2008) for the

changes at molecular level, such as chain‒scissioning, cross-linking, free radical

formation, elimination of volatile species, reordering the chemical bonds, etc. which are

finally responsible for the modification in their properties.


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1.7.2 Swift Heavy Ions Irradiation

When an energetic ion penetrates through the material, it loses energy mainly by

two nearly independent processes: (i) elastic collisions of the incident ion with the

nuclei of the target atoms, usually referred to as nuclear energy loss (dE/dx)n (ii)

inelastic collisions of the incident ion with the atomic electrons of the target atoms,

generally expressed as electronic energy loss (dE/dx)e (Ritchie & Claussen, 1982; Fink

& Chadderton, 2005). The relative contribution of the energy loss through these two

processes depends upon the nature of the incident ion and the target material

parameters. For MeV heavy ions, usually the electronic energy loss dominates while the

nuclear energy loss remains almost negligible. However, when the ion velocity reduces

to the extent that the ion behaves almost as a neutral atom, the ion-matter interaction

occurs via hard sphere scattering and under this situation the nuclear energy loss starts

dominating over electronic energy loss. Thus, for swift heavy ions, where the ion

velocity remains considerably higher than that for its orbital electrons, the electronic

energy loss remains into picture with nuclear energy loss to be almost negligible.

Finally, the energy deposited by the swift heavy ions during their passage,

particularly in polymers, leads to the processes of macromolecular destruction,

chain‒scissioning, cross‒linking, free radicals formation, carbonization, oxidation, etc.

These processes are responsible for the modification in the optical, electrical, thermal,

mechanical and chemical properties of the polymeric material.

1.8 Motivation

Due to the unique features of polymer-metal nanocomposites and the feasibility

to tune their structural, electrical, optical, mechanical, thermal and other properties as a

result of electromagnetic and ion beam irradiation, these nanocomposites are promising

futuristic materials in device applications at a larger scale (Mayer, 2001; Corbierre et

al., 2005; Sih & Wolf, 2005; Zhu & Zhu, 2006; Avasthi et al., 2007; Puiso et al., 2011;

Sharma et al., 2011). The characteristic features of polymer-metal nanocomposites not

only depend on the concentration and dispersion of the embedded metal nanoparticles

but also on their size, shape and orientation within the polymer matrix. These


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parameters of embedded nanoparticles, which are responsible for the change in the

properties of polymer-metal nanocomposites, can be regulated through irradiation

(Abyanesh et al., 2007; Bernard et al., 2011; Puiso et al., 2011; Sharma et al., 2011)

besides their synthesis mechanism. Although, sufficient literature is available related to

the synthesis and characterization of polymer-metal nanocomposites (Khanna et al.,

2005; Gautam & Ram, 2009; 2010) but the studies related to irradiation induced effects

on their optical, electrical, thermal and structural behaviour are scarce.

Motivated with the feasibility of tuning the properties of polymer-metal

nanocomposites as a result of irradiation, in the present work, we have concentrated on

a comprehensive study related to the effect of gamma, ultraviolet and swift heavy ion

irradiation on the optical, electrical and structural behaviour of PVA-Ag

nanocomposites. The observed changes in the optical and electrical properties have been

tried to be correlated with the induced structural changes, revealed through X-ray

diffraction (XRD), Fourier Transform Infrared (FTIR) and Raman Spectroscopy. The

selection of PVA in PVA-Ag nanocomposites is due to its high dielectric strength, good

charge storage capacity, dopant-dependent electrical and optical properties and

capability to act as good stabilizing and capping agent for embedded metal

nanoparticles (Khanna et al., 2005; Bhajanti et al., 2007; Mahendia et al., 2010; Voue

et al., 2011) while silver nanoparticles provide interesting optical and electrical

properties.

1.9 Objectives of the Present Study

The following were the specific objectives of the present study:

1. To synthesize PVA‒Ag nanocomposites by in-situ chemical reduction method

and preparation of their films by solution casting method.

2. To reveal the size distribution and dispersion of embedded nanoparticles through

Transmission Electron Microscopy.

3. To study the optical, electrical and structural behaviour of prepared PVA‒Ag

nanocomposite films using UV‒Visible spectroscopy, I-V measurements, FTIR

and Raman Spectroscopic techniques and XRD analysis.


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4. To analyze the variation in optical, electrical and structural properties of

prepared PVA‒Ag nanocomposite films as a result of gamma, UV and swift

heavy ion irradiation at different doses.

5. To understand the irradiation induced changes in optical and electrical behaviour

of PVA‒Ag nanocomposite films in terms of induced structural changes.

In order to meet the objectives as stated above, the procedure followed for

experimental measurements, obtained results and their interpretation are

presented in the subsequent chapters.


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