Chapter – I General Introduction

Chapter - I
General Introduction
1.1 Introduction
Over the past few decades a prefix “nano” has gained tremendous popularity
among scientists and technologists and it has created its own identity in the form of
nano science and nanotechnology. The term nano etymologically from the Greek and
the meaning is “dwarf”, which was first coined by Richard Feynman in 1959 in his
famous often cited lecture [1]. The word nano science refers to the study,
manipulation and engineering of matter, particles and structures on the nano-meter
scale. Important properties of materials, such as the electrical, optical, thermal and
mechanical, are determined by the way molecules and atoms assemble on the nano
scale to form larger structures. However, in the nano-meter size structures various
properties are often different from those of the macro-scale ones because of quantum
mechanical effects coming into the picture. Moreover, nanotechnology is the
application of nano science leading to the use of new nano-materials and nano size
components in various products. Nanotechnology provides the ability to design
custom made materials and products with new or enhanced properties. It is interesting
to note that these are interdisciplinary subjects often combining physics, chemistry,
materials science, biotechnology, biochemistry, electronics, engineering technology,
etc. [2]. According to Drexler [3] the nanotechnology is the principle of manipulation
atom by atom through control of the structure of matter at molecular level and
developing ability to build molecular system with atom by atom precision to yield a
varieties of nano machines.
Broadly, speaking, the nano-particles can be divided into two categories;
naturally occurring nano-particles and synthesized in the laboratory. The naturally
occurring nano-particles include organic and in-organic types. The examples of
organic type nano-particles are proteins, polysaccherides, viruses, etc, whereas the
inorganic nano-particles like iron oxyhydroxides, aluminosillicates, metals, etc are
produced by weathering, volcano eruption, wild fires or microbial processes [4,5].
Also on the other hand, a variety of nano-materials such as nano-particles,
nano-wires, and nanotubes have been synthesized in laboratory or modified in order
to obtain superior properties with greater functional versatility. In particular, nano-

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Chapter – I General Introduction

particles due to their size, in the range of 1-100 nm, have been examined for their uses
as tools for a new generation of technological devices.
The history tells that in the past most spectacular effects were obtained by
incorporating nano-particles, perhaps, without proper recognition, in different
artefacts. The most eye-catching effects were obtained with metal nano-particles as
colour pigments in lustre and in glass technology. Metal lustre decorations of glazed
ceramics in Mesopotamia in 9th century was due to silver and/or copper nano-particles
dispersion within the outermost layer [6]. Metal nano-particles were used to colour
glasses in extraordinary ways. The Lycurgus cup made by Romans in fourth century
has striking features due to gold nano-particles; it appears green colour in daylight but
appears red when illuminated from the inside [7, 8].
Nano-particles often have unique physical and chemical properties, for
example, the electronic, optical, and chemical properties of nano-particles may be
very different from those of each component in the bulk. In nano-particles, on
increasing the surface area with respect to the volume, the increase in the contribution
of the surface atoms in the behaviour of the particles can be observed and as a
consequence of this the properties of the particles gets altered as well as their
interaction with the surrounding environment takes place. As the surface area
increases, the larger is the contribution of the surface energy to overall energy of the
whole system and, thus, results in a reduction of the impact of the bulk atoms on the
properties of a material. Therefore, the properties of nano-structures are more directly
related to those of individual molecules or atoms.
The nano-scale structures permit the control of fundamental properties of the
materials without changing their chemical structure. The nano-particles are of great
scientific interest as they are effectively a bridge between the bulk materials and the
atomic or molecular structures. A bulk material is having consistent physical
properties regardless its size, but in contrast to this the nano-particles do not exhibit
this. The properties of materials change as their size approaches to the nano-scale,
where the percentage of atoms on the surface of a material becomes significant. The
interesting and sometimes unexpected properties of nano-particles are partly due to
the high surface to volume ratio present in the material. The era of nano materials and
nano technologies promises to be one of the major scientific developments and
breakthroughs that, in not too distant future, will permanently affect our everyday
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Chapter – I General Introduction

lives. Several of these products are already being used and many organizations
estimated its market contribution in 2015 of the order of US dollars 1000 billion [9].
Two main factors may be responsible for the changes of properties observed
in nano-particles:
(i) A much greater relative surface area per unit of mass
(ii) Predominance of quanta effects.
1.2.1 Surface effect:
For bulk materials, usually greater than one micron size, the percentage of
atoms at the surface is infinitesimally small compared to the total number of atoms of
the material. As the size of the material is reduced, the ratio of surface atoms to inner
atoms (or total atoms) starts increasing. Atoms on the surface of a bulk crystalline
solid are principally located on basal planes, but they transform almost completely in
edge and corner atoms with a decrease in size. Because of the low coordination
number, edge and corner atoms are highly chemically reactive, catalytically active,
highly polarizable, and so on, in comparison with the atoms on basal planes. As a
result, in the nano meter size range, the role of surface atoms starts becoming
predominant in determining the properties of the material (surface effect) instead of
the inner atoms. The very high surface area to volume ratio provides a tremendous
driving force for diffusion, especially at elevated temperatures. Sintering can take
place at lower temperatures, over shorter time scales than for bigger particles. This
theoretically does not affect the density of the final product, though flow difficulties
and the tendency of nano-particles to agglomerate complicates the matters. The large
surface area to volume ratio also reduces the incipient melting temperature of nano-
particles.
1.2.2 Quantum-size effect
The processes of diminishing the macroscopic size to nano meter range in one,
two or all the three dimensions lead to the confinement of movement of conduction
electrons in a very small space, which is comparable to their De Broglie wavelength.
This leads to the formation of discrete energy levels in nano-materials similar to
atoms, unlike the continuous energy levels in the bulk materials.
The first factor is responsible for the changes in reactivity, which can increase
considerably as particles decrease in size. The second factor, observed in particles of a
few dozen nm, explains the changes in terms of optical, electrical, mechanical and
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Chapter – I General Introduction

magnetic properties. Due to the quantum confinement effect and the large surface to
volume ratio, small nano-crystals show very special physical and chemical properties
corresponding to their bulk materials, when their size is close to or smaller than that
of the Bohr exciton. Therefore, optical, thermal, and electrical properties of the
particles become dependent on their sizes and shapes. These properties have been
reviewed by Burda et al [10]. However, some of the properties of the nano-particles
might not be predicted by understanding the increasing influence of surface atoms or
quantum effect. While the nano-particles display properties that differ from those of
the bulk samples of the same material, the groups of nano-particles can have
collective properties different from those displayed by the individual nano-particles
and the bulk samples. For realizing versatile functions, an assembly of nano-particles
in regular patterns on surfaces and at interfaces is required [11].
The physical properties of nanoparticles are mainly shape, size, specific
surface area, agglomeration/aggregation, state of size distribution, surface
morphology/topology, crystallinity, defect structure and solubility [12-14]. These are
given in schematic diagram in figure 1.1

Figure 1.1: Parameters affecting physical properties of Nano-particles

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Chapter – I General Introduction

Because of the change in physical and chemical properties along with particle
size reduction in nano-particles, various properties like optical, electrical transport,
magnetic properties, hardness, chemical reactivity, toxicity, etc. are getting altered.
[15, 16]
The startling properties of various types of nano particles can be studied by
hosts of characterization techniques, which are reviewed by several authors [17, 18].
Nano-particles that are small enough to enter human cells have the opportunity
to interact (in a positive or negative sense) with the biochemical functions of the cells.
Biological systems have the capabilities to covert metal ions into metal nano-particles
in a friendly manner. Nano particles can be used in fluorescent biological labels, drug
and gene delivery, tissue engineering etc. [16]. There are several articles written by
different authors [15,19-23] as well as several well written books are published [11,
24-33] on nano-science, nano-technology and nano-materials.
1.3 Synthesis Methods of Nano Particles
The synthesis of nano particle is categorized as: (1) Top down (2) Bottom up
methods. Figure 1.2 shows the schematic block diagram of the process. Various
techniques used under these categories are tabulated in table 1.1. This has been
discussed in detail by Ealias and Saravana kumar [18].

Figure 1.2: Categories of Nano-particles synthesis

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Chapter – I General Introduction

Table 1.1: Various techniques used under top down and bottom up categories
Category Method
Bottom up Sol-gel
Spinning
Chemical vapor deposition (CVD)
Pyrolysis
Biosynthesis
Top Down Mechanical Milling
Nanolithography
Laser ablation
Sputtering
Thermal decomposition

In another attempt, various techniques of synthesis of nano particles are

categorized as: chemical, physical and biological [16], which is described in a
schematic presentation in figure 1.3. A brief review on methods of synthesis of nano-
particles is given by Rajput [34].

Figure 1.3: Broad synthesis routes of nano-particles

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Chapter – I General Introduction

Further, the synthesis methods are divided into three categories depending on
its physical state, i.e., vapour phase, liquid phase and solid phase techniques. Table
1.2 shows the techniques employed under these categories. This has been discussed in
detail by Su and Chang [35].
Table 1.2: Various methods categorised on the basis of three physical states
Category Technique
(1) Vapour Phase Synthesis Flame Synthesis
Laser Ablation
Arc Discharge
(2) Liquid Phase Synthesis Chemical Precipitation
Hydrothermal
(3) Solid Phase Synthesis Sol -gel
Mechanical Milling

The present author has used the liquid phase synthesis, also known as wet
chemical method, to synthesize her nano particles. This synthesis approach is very
popular in industries. This technique involves mixing solutions of different ionic salts
in well-defined quantities and subjected it to controlled temperature and pressure to
promote the formation of insoluble nano particles, often separated as precipitates from
the solution. This is energy efficient technique and generally carried out at low
temperatures and often at ambient pressure. In other words, it does not require high
temperature, expensive energy sources or high pressure. Moreover, liquid phase
synthesis provides precise control of stoichiometry/ composition of the end products
and the synthesized nano-particles can be stabilized or functionalized during the
synthesis. However, there are certain limitations of this method such as, some time
chemicals used in the synthesis are explosives or toxic in nature, synthesized nano-
particles require further processing and purification and the purity of the nano-
particles is usually less than those synthesized by vapour phase. [35]. Different wet
chemical methods are briefly described as follows:
1. Hydrothermal method
Hydrothermal method is simple and versatile method to synthesis inorganic nano
particles under high temperature and high pressure condition. It is possible to change

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Chapter – I General Introduction

the characteristics of the nano-particles by adjusting processing conditions such as

temperature, pressure and precursor concentrations. The density of water and
dielectric constant are highly dependent on temperature and pressure. As the dielectric
constant of water reduces, the reaction rate increases and the ionic species begin to
precipitate to form solid phase [35, 36]. Block diagram of hydrothermal route used for
nano particles preparation is shown in figure 1.4.

Figure 1.4: Block diagram of hydrothermal route used for nano particles
preparation
2. Sol-gel process
The sol-gel process, involves the evolution of inorganic networks through the
formation of a colloidal suspension (sol) and gelation of the sol to form a network in a
continuous liquid phase (gel). The precursors for synthesizing these colloids consist

8
Chapter – I General Introduction

usually of a metal or metalloid element surrounded by various reactive ligands. The

starting material is processed to form a dispersible oxide and forms a sol in contact
with water or dilute acid. Removal of the liquid from the sol yields the gel, and the
sol/gel transition controls the particle size and shape. A schematic diagram of sol-gel
process is shown in figure 1.5.

Figure 1.5: A schematic diagram of sol-gel process

3. Chemical Precipitation
The main advantage of this method is its simplicity and ability to obtain final
product of near perfect stoichiometry without high temperature treatment. Figure 1.6
shows the broad scheme of the process. Two solutions are mixed with another direct
or drop-by-drop manner. The co-precipitation takes place when the reactant products
are dissolved and precipitating agent is added to precipitate the reaction products.
These precipitates undergo aging process to obtain the larger particles, which are
recovered by filtration or centrifuge method. Further washing with distilled water
and ethanol to remove the impurities present. Afterwards, as per the requirement
post treatment like annealing, calcination or sintering is done to obtain desired
structure and morphology [35].

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Chapter – I General Introduction

Figure 1.6: Scheme of wet chemical synthesis of nano-particles

The chemical precipitation involves simultaneous occurrence of nucleation,
growth and coarsening or agglomeration. The critical step to precipitation is
nucleation and that is governed by the degree of super-saturation. Initially a large
number of small crystallites are formed and, thereafter, through Ostwald ripening the
aggregates are formed. The control of nucleation and growth is necessary. The main
parameters affecting the nano-particles are surface charge-zeta potential, reactant
concentration, reaction temperature, PH, degree of mixing and recrystallization of the
precipitates. By controlling these parameters, the particle size distribution and
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Chapter – I General Introduction

stoichiometry of nano-particles can be changed [35]. The mechanism of nucleation

and growth of nano-particles in solution is reviewed by Thanh et al. [37]. Often
surfactant is used to maintain separation between the nano-particles formed [34, 38].
In the present study, various metal tartrate, i.e., strontium tartrate, magnesium
tartrate and iron-tartrate, nano-particles were synthesized by the surfactant mediated
wet chemical approach. The block diagram of the process is given in figure 1.7

Figure 1.7: Scheme of process for synthesis of metal tartrate nano-particles

The direct reaction between tartaric acid and metal salt does not give
precipitation. Here, sodium hydroxide or sodium metasilicate is used as precipitating
agent. The precipitates are filtered and dried and resulted into metal-tartrate nano
particle samples. This will be discussed in following chapters of the thesis.
Surfactants:
Surfactants are materials which exhibit the characteristics of reducing the
interfacial tension between two immiscible liquids by way of enhanced adsorption at

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Chapter – I General Introduction

the interface. These surfactants or “surface active reagents” are usually amphiphilic
organic compounds, i.e., the same molecule possess two distinct groups which differ
greatly in their solubility relationships. Generally speaking, the surfactants possess a
hydrophobic tail group and a hydrophilic head group. The hydrophobic tail is usually
a long chain hydrocarbon and the hydrophilic head is an ionic or highly polar group
that imparts water solubility to the molecule. The unique amphiphilic structure of
surfactants gives rise to some characteristic properties which fall into two broad
categories.
(i) Adsorption, which is the tendency of a surfactant molecule to collect at an
interface. The adsorption properties of surfactants means these molecules are usually
found at the interface between oil and water phases with the hydrophilic head groups
favouring inclusion in the water phase and the hydrophobic tails favouring inclusion
in the oil phase. This is displayed in figure 1.8.
(ii) Self – assembly, is the property of surfactants where they arrange themselves into
organized structures in aqueous solutions, once a certain concentration is reached,
usually referred to as the critical micelle concentration (CMC) [39]. At low
concentrations, the surfactant molecules form solutions in water but some molecules
will be adsorbed at the air/solution interface and onto the walls of the containing
vessel. As the concentration is increased, the surface become covered with a
monolayer of surfactant molecules. Further increase in the concentration causes the
normal dissolution processes to cease and the molecules in solution begin to aggregate
into organized micelles, which occurs at a precisely defined concentration [40]. The
schematic diagram of micelle is shown in figure 1.9.

Figure 1.8: Adsorption of surfactant molecules at an oil/water interface

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Chapter – I General Introduction

Figure 1.9: Spherical surfactant micelle

Micelles are often globular and roughly spherical in shape but ellipsoids,
cylinders and bilayers or vesicles are also possible. The shape and size of a micelle
depends on the molecular geometry of its surfactant molecules and solution
conditions such as surfactant concentration, temperature, pH and ionic strength.
Surfactants can be classified in a number of ways but the most useful
classification method is based on the nature of their hydrophilic head groups, which is
given in table 1.3.
Table 1.3: Types of surfactant and their properties
Sr.No. Types of Properties
surfactant
1 Anionic Composed of highly electro-negative atoms making these
groups strongly polar. For example - Sodium Dodecyl
Sulphate (SDS)
2 Cationic Possess positively charged head groups which usually
contain a nitrogen atom or an amide group. For example –
Cetyltrimethy lammonium bromide (CTAB)
3 Non-ionic They do not ionize in aqueous solution, because their
hydrophilic group is of a non-dissociable type, such as
alcohol, phenol, ether, ester, or amide. For example –
Triton X-100
4 Zwitterionic Zwitterionic or amphoteric surfactants contain, or have the
potential to form, both positive and negative functional
groups under specified conditions

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 Chapter – I General Introduction

In the present study Triton X-100 surfactant is used, which is non-ionic in

nature. The chemical formula of this surfactant is C14H22O(C2H4O)n (n = 9-10) and
structural formula is as shown in figure 1.10. There are also other synonyms of Triton
X-100 like Polyethylene glycol p-(1,1,3,3-tetramethylbutyl)-phenyl ether, Octyl phenol
ethooxylate, Polyoxyethylene octyl phenyl ether, 4-octylphenol polyethoxylate, Mono
30, TX- 100, t-octylpheneoxypolyethoxyethanol, octoxynol-9.

Figure 1.10: Chemical structure of Triton X-100

Uses of Nano-particles:
Nano-particles have diverse applications in various fields and it is difficult to cover
each field, however, a broad attempt is made hereby to mention major fields where
nano-particles find applications. [14,16, 18, 23, 41-48]
(1) Drugs and medications
(2) Electronics
(3) Environment
(4) Energy harvesting
(5) Mechanical industry
(6) Sports equipment
(7) Dye and veneers
(8) Textiles and clothing
(9) Cosmetics and sunscreens
(10) Food and nutrition
(11) Catalysts
(12) Ferro fluids
(13) Defence
(14) Space science

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Chapter – I General Introduction

1.4 Tartrate Compound:

Tartrate compound is defined as a salt or ester of tartaric acid containing the group of
C4H4O6.
1.4.1 Types of tartrate compound
Naturally occurring tartaric acid is chiral, meaning it has molecules that are
not superimposable on their mirror images. It is a useful raw material in organic
chemistry for the synthesis of other chiral molecules. The naturally occurring form of
the acid is L-(+)-tartaric acid or dextro-tartaric acid. The mirror-image (enantiomeric)
form, levo-tartaric acid or D-(−)-tartaric acid, and the achiral form, mesotartaric acid,
can be made artificially. The dextro and levo prefixes are not related to the D/L
configuration (which is derived rather indirectly [49] from their structural relation to
D- or L-glyceraldehyde), but to the orientation of the optical rotation, (+) =
dextrorotatory, (−) = levorotatory. Sometimes, instead of capital letters, small italic d
and l are used. They are abbreviations of dextro- and levo- and, nowadays, should not
be used. Levotartaric and dextrotartaric acid are enantiomers, meso-tartaric acid is a
diastereomer of both of them.
Levotartaric acid (D-(−)- Dextrotartaric acid (L-(+)-
tartaric acid) tartaric acid)

A rarely occurring, optically inactive form of tartaric acid, DL-tartaric acid is a

1:1 mixture of the levo and dextro forms. It is distinct from meso-tartaric acid and was
called racemic acid (from Latin racemus – "a bunch of grapes"). The word racemic
later changed its meaning, becoming a general term for 1:1 enantiomeric mixtures –
racemates.
Tartaric acid is used to prevent copper (II) ions from reacting with the
hydroxide ions present in the preparation of copper (I) oxide. Copper (I) oxide is a

15
Chapter – I General Introduction

reddish-brown solid, and is produced by the reduction of a Cu (II) salt with an

aldehyde, in an alkaline solution.
1.5 Importance of Metal Tartrate Compounds
The organo metallic compounds of tartaric acid finds various applications in
science and technology [50]. For example, ferroelectric applications of sodium
potassium tartrate [51] and calcium tartrate [52], ferroelectric-Ferro elastic
applications of sodium ammonium tartrate [53] and dielectric applications of lithium
thiallate tartrate [54]. Many tartrate compounds have exhibited novel properties,
which has lead to several applications, for example, piezoelectric application of
cadmium tartrate [55], the addition of lead tartrate in gasoline to prevent knocking in
motors [56], ferroelectric properties of sodium potassium tartrate [51] and
ferroelectric, dielectric, optical and thermal properties calcium tartrate [52, 57]. The
formation of potassium hydrogen tartrate crystals in wine bottles is unwanted and
efforts are made to avoid it by a trap process or by influence of external electric field
[58]. There are certain tartrate compounds find applications in cosmetics. The
synergist effect of tartaric acid for zinc ion in cosmetics has been reported [59]. Some
tartrate compounds are used in military applications. Strontium tartrate is used as a
trace compound in ammunition units [60, 61]
There are several industrial and chemical application of metal tartrate
compounds. Sodium-iron tartrate complex is useful for the preparation of solvent for
cellulose [62]. This has significance in paper industry. Bayer [63] had studied iron
tartrate alkali system and its complexing reaction with cellulose related polyhydroxy
compound for paper industry.
Manganese tartrate crystals being temperature sensitive can be used to sense
and measure the temperature in terms of precise change in coloration. A wax pencil is
developed to sense the surface temperature of heated substance in terms of change in
the coloration upon contact. The change in coloration of these crystals occurs at
4100C from pink to black. The coloration change is almost instantaneous and
occurring within 1 to 2 seconds. Gvozdov and Erunov [64] have described this
method. The effect of light on copper tartrate has been examined [65].
There are certain industrial applications of different tartrate compounds. Zinc
tartrate with other compounds form a bright coating and protecting powder for metals
[66]. Also, antimony tartrate is used in corrosion inhibitive composition for coolant
16
Chapter – I General Introduction

systems [67]. Cobalt doped calcium tartrate is used as a catalyst in synthesis of carbon
nano tubes using CVD technique by Asanov et al. [68].
As discussed above, there are several applications of various metal tartrate
compounds in different fields, however, it is difficult to cover each one. Till today,
major reports are available on the growth of metal-iron tartrate crystals by the gel
growth technique only, which is discussed in brief in the following section. A scheme
to set gel in glass test tube is shown in figure 1.11.

Figure 1.11: A scheme of gel growth process and schematic diagram of crystal
growth in gel containing glass test tube.
1.6 Growth of Metal Tartrate Crystals
Tartrate crystals are grown by gel growth technique. In this context, the gel
method has emerged as a convenient growth technique. The utilization of gel as a
medium of crystal growth was put forward by Fisher and Siemen [69-71] in 1926.
However it remained as an unused work till 1962. Then increased interest in crystal
growth by gel technique led scientists to notice its capability and advantage in
generating relatively perfect defect free crystals. The reports describing the growth of
crystals appeared frequently in popular journals during this period [72-76]. The

17
Chapter – I General Introduction

method became very popular due to the pioneer work of H. K. Henisch [77], who
gave an authentic and narrative record of this method in his famous book. The crystals
of a new polymorphic modification of monobasic sodium tartrate monohydrate
NaHC4H4O6 · H2O have been grown in a metasilicate gel and their atomic structure is
solved by X-ray diffraction [78]. Also, Ahmed et al [79] have studied single crystal
growth of lithium hydrogen tartrate by gel encapsulation technique and reported that
the correlated barrier hopping is the dominant charge-transport mechanism.
In the present author’s laboratory, several predecessors [65, 80-88] have
successfully grown several pure metal tartrate crystals, doped metal tartrate crystals,
mixed metal tartrate crystals and ternary metal tartrate crystals by the gel method in
more than last two and half decades and reported widely in their theses and
dissertations. Exhaustive literature survey has been included by these researchers in
their theses as well as dissertations and hence the detailed literature survey is avoided
here. However, some important publications from our research group are cited hereby
covering last two decades, for instance, thermal studies, MÖssbauer spectroscopic and
magnetic studies of iron tartrate [89,90]; thermal studies of calcium tartrate [91], zinc
tartrate [92] and cadmium tartrate [93]; growth and characterization of iron-
manganese mixed tartrate [94], calcium-strontium mixed tartrate [95]; thermal studies
of lead-cadmium mixed tartrate [96]; thermal and dielectric studies of manganese –
copper mixed levo tartrate [97]; thermal studies of lead-cobalt mixed tartrate [98],
lead- cadmium tartrate [99]; impedance and dielectric study on lead-cobalt mixed
tartrate [100] ; dielectric study of Mn++ doped calcium tartrate [101], dielectric study
of Cu++ doped calcium tartrate [102]; Vickers micro-hardness studies of Mn++ and
Cu++ doped calcium tartrate [103]; detailed characterization of ternary iron-
manganese-cobalt tartrate [104], etc.
To avoid the repetition, notwithstanding, the present author has attempted to
refer last five years research publications and it is found that the major focus has
remained on mixed or doped systems of metal tartrate crystals rather than pure metal
tartrate crystals. The reason is very simple and clear that most of the pure metal
tartrate crystals are already studied in detail earlier by several authors [74, 77, 105-
113]. Most of the tartrate crystals have been characterized by TGA for thermal
stability, FTIR for functional group identification, EDAX for compositional study,
dielectric and impedance studies and powder XRD for structural informations;
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Chapter – I General Introduction

however, only few reports are available on magnetic studies. In the last five years
only few reports are available on pure metal-tartrate crystals growth by gel method
such as lead tartrate [114], nickel tartrate [115], cobalt tartrate [116], cadmium tartrate
[117], calcium tartrate [118] and magnesium tartrate [119]. There are reports available
on gel growth and characterization of mixed tartrate crystals, for example, silver-
manganese mixed tartrate [120], cadmium- calcium tartrate [121, 122] and iron-
manganese-nickel tartrate [123]. Moreover, some reports are available on various
doped metal tartrate crystals grown by the gel technique such as, copper doped iron-
tartrate [124], calcium doped cadmium tartrate [125] and organic dye Eosin doped
strontium tartrate crystals [126]. Recently, Jethva [127] has reviewed various metal
tartrate crystals grown by the gel method.
A plethora of literature is available on metal tartrate crystal growth by the gel
method, nevertheless, very scanty work is reported in the literature on the synthesis of
metal tartrate nano-particles. By careful literature survey the present author finds only
few references. The synthesis of strontium tartrate nano particles using Triton X-100
surfactant is reported by Abdel-Aal and El- Shazly [128]. The only other reference is
found that is of the present author on the synthesis of calcium tartrate nano-particles
by surfactant mediated approach [129].
1.7 Objective of the Present Study
There are very scanty reports available on tartrate nano particles. Most of the
applications of the metal tartrate compounds are in the bulk or in a crystalline form,
however, no major reports are available till date regarding the applications of metal
tartrate compounds in the nano-particle forms. The physical properties of the bulk
form and nano-particle forms are expected to be different and hence the present
author has selected three well studied metal tartrate compounds in her laboratory, i.e.,
strontium tartrate, magnesium tartrate and iron tartrate, to synthesize in the nano-
particle form and characterize them by employing various techniques and compare the
properties with the respective bulk form available in the literature. It is important to
note that very scanty work is reported on magnesium tartrate in bulk form.
1.8 Scope and Aim of the Thesis
(i) To synthesize strontium tartrate, magnesium tartrate and iron tartrate nano
particles and characterize them. Here, dextro-tartaric acid is used in the

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Chapter – I General Introduction

synthesis of nano particles, however, for simplicity, it is avoided in the name

of the compound.
(ii) To evaluate crystallite size and strain by using Scherrer’s formula and
Williamson and Hall formula from respective powder XRD patterns.
(iii) To identify the morphology of nano-particles by TEM.
(iv) To study the molecular vibrations of various function groups using FT-IR
spectroscopy.
(v) To study the thermal stability of nano particles by TGA and DTA.
(vi) Dielectric and a.c. conductivity studies for polarization nature and
identification of electrical transport nature.

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Chapter – I General Introduction

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6. P. Sciau, C. Mirguet, C. Roucau, D. Chambanne, M. Schvoerer, J. Nano. Res, 8
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