SYNTHESIS OF CuO NANOPARTICLES BY HYDROTHERMAL

METHOD
Introduction:
A versatile and surfactant free hydrothermal method was adopted to synthesize CuO
nanoparticles. Using hydrothermal method CuO nanoparticles can be synthesized
without organic solvents, expensive raw materials and complicated equipments. CuO
nanoparticles were characterized by X-ray diffraction analysis (XRD), High resolution
scanning electron microscopy (HRSEM), Energy dispersive X-ray analysis (EDAX), Fourier
transform infrared (FTIR) and UV- visible spectroscopy. Structural analysis reveals that
CuO nanoparticles have monoclinic structure with single crystalline phase. High
resolution scanning electron microscopy exhibits rod like CuO nanostructures. Fourier
Transform Infrared Spectroscopy spectra showed the vibrational bands of Cu-O metal
oxygen bonds. Absorption spectra of CuO nanoparticles show broad absorption bands
and band gap energy were determined. [1] Spherical, ellipsoidal and needle-shaped
CuO nanocrystals can be obtained simply by varying the reaction temperature and
controlling the addition of NaOH. Hydrothermal processing where high temperature–
high pressure aqueous solutions, vapors and/or fluids react with solid materials is a well-
known process in mineralogy and geology fields for formation, alteration or deposit of
minerals, ores or rocks The homogeneity of composition, structure and microstructure
as well as much finer particles in molecular or atomic size can beachieved in the gas or
solution systems of hydrothermal process The hydrothermal processing is suitable for
the preparation of powders; from nano-particles to single crystals. . Furthermore,
several physical and chemical parameters can be effectively controlled by hydrothermal
treatments. This method may be suitable for large scale production of nano CuO
particles for practical applications. [2] Metal oxides represent the most diverse class of
materials with properties covering almost all aspects of materials science and physics.
Copper oxide, an important p-type semiconductor with the band gap in the range of 1.8
– 2.5 eV has obtained increasing interest because it has many potential applications in
solar energy conversion, photocatalytic degradation of organic pollutants. Copper oxide
is used in consumer products such as pillow cases socks due to its cosmetic and
antimicrobial properties. In the present study nano CuO was prepared without any
additive like ionic liquids, capping agents and used (CuSO4. 5H2O) as base. Here in, we
report a hydrothermal synthetic method and physicochemical characterization of CuO
nanostructures with spherical like shape, moreover, these type of CuO nanostructures
show an excellent electrochemical behavior and good cycle stability.[3]
Nanotechnology
Nano is derived from a Greek word "vaos" meaning "dwarf" (extremely small). It is a
prefix literally refers to 1 billionth of physical size. Technology is the making, usage and
knowledge of tools, machines and techniques in order to solve a problem or perform a
specific function.

So, Nanotechnology can be defined as:

Nanotechnology is the study of manipulating matter on a nano meter scale (one

billionth of a meter). It is study and application of extremely small things that can be
used across all other science fields, such as chemistry, biology , physics material science
and engineering.

In order to understand the unusual world of nanotechnology, we need to get an idea of

the units of measure involved. A centimeter is one-hundredth of a meter, a millimeter is
one-thousandth of a meter, and a micrometer is one-millionth of a meter, but all of
these are still huge compared to the nanoscale. A nanometer (nm) is one-billionth of a
meter, smaller than the wavelength of visible light and a hundred-thousandth the width
of a human hair.[4]

History
Early contributors to this nanotechnology field include James Clark Maxwell (Scottish
physicist and mathematician, 1831-1879) and Richard Adolf Zsigmondy (Austrian-
German chemist, 1865-1929). Zsigmondy studied colloids (chemical mixtures where
one substance is dispersed evenly throughout another) and looked at gold sols and
other nanomaterials. Other important contributors in the first half of the 20th century
include Irvin Langmuir (American chemist and physicist, 1881-1957) and Katherine B.
Blodgett (American physicist, 1898-1910), the first woman to get her Ph.D. studying
Physics at the University of Cambridge. The earliest systematic discussion of
nanotechnology is considered to be a speech given by Richard Feynman (American
physicist, 1918-1988) in 1959. It was titled:

"There's Plenty of Room at the Bottom."

 In this speech Feynman discussed the importance "of manipulating and controlling
things on a small scale" and how they could "tell us much of great interest about the
strange phenomena that occur in complex situations." He described how physical
phenomena change their manifestation depending on particular scale.

The term 'nanotechnology' was used first by the Japanese scientists Norio Taniguchi
(1912-1999) in a 1974 paper on production
technology that creates objects and features onon
the order of a nanometer. The American engineer
K. Eric Drexler (b. 1955) is credited with the
development of molecular nanotechnology,
leading to nanosystems machinery manufacturing.

The invention of tunneling microscope in the

1980s by IBM Zurich scientists and then the atomic
force microscope scanning allowed scientists to
see and study materials at an unprecedented
atomic level. These studies provided insight into
nanoscale material structvities in1980s.
.Significant progress was obtained by IBM in 1990
when a team of physicists had spelled out the
letters "IBM" using 35 individual atoms of xenon.
Another breakthrough came in 1985 with the
discovery of new shapes for molecules of carbon,
known as the buckyball, which are round and
consist of 60 carbon atoms. This k led to the
discovery of a related molecular shape known as
the carbon nanotube in 1991. Carbon nanotubes
are still one of the most promising areas of
nanotechnology as they are about 100 times stronger than steel but just a sixth of the
weight; they have unusual heat and conductivity characteristics.[5]
In parallel, studies Experts Saying About Nanotechnology
In June 1999, Richard Smalley, Nobel laureate in chemistry, addressed the US House
Committee on Science on the benefits of nanotechnology. "The impact of
nanotechnology on the health, wealth, and lives of people," he said, "will be at least
equivalent of the combined influences of microelectronics, medical imaging,
computer-aided engineering and man-made polymers developed in this century."
Nano particle
A nanoparticle is the most fundamental component in the fabrication of nanostructure,
and is far smaller than the world of everyday objects that are described by Newton ’ s
laws of motion, but bigger than an atom or a simple molecule that are governed by
quantum mechanics.In general, the size of a nanoparticle spans the range between 1
and 100 nm. [6]
Table 1.1 Definitions of nanoparticles and nanomaterials by various organizations: International Organization for
Standardization ( ISO ), American Society of Testing and Materials ( ASTM ), National Institute of Occupational Safety
and Health ( NIOSH ), Scientifi c Committee on Consumer Products ( SCCP ), British Standards Institution ( BSI and
Bundesanstalt für Arbeitsschutz und Arbeitsmedizin ( BAuA ).

Composition
NPs are not simple molecules itself and therefore composed of three layers [7]i.e.
(a) The surface layer, which may be functionalized with a variety of small molecules,
metal ions, surfactants and polymers.
(b)The shell layer, which is chemically different material from the core in all aspects,
(c) The core, which is essentially the central portion ofthe NP and usually refers the NP
itself

Properties of Nanoparticles
Physical Properties
The physical properties include optical such as the colour of the nanoparticle, its light
penetration, absorption and reflection capabilities, and UV absorption and reflection
abilities in a solution or when coated onto a surface. [8]

This extraordinary cup is

the only complete historic
example of a very special
type of glass, known as
dichroic glass, that changes color when held up to the light. The opaque green cup turns to a
glowing translucent red when light is shone through it internally.[9]

It also includes the mechanical properties such as elastic, ductile, tensile strengths and
flexibility that play a significant factor in their application. Other properties like
hydrophilicity, hydrophobicity, suspension, diffusion and settling characteristics has
found its way in many modern everyday things. Magnetic and electrical properties such
as conductivity, semi conductivity and resistivity has led a path for the nanoparticles to
be used in modern electronics thermal conductivity in renewable energy applications.
4.2. Chemical Properties
The chemical properties such as the reactivity of the nanoparticles with the target and
stability and sensitivity to factors such as moisture, atmosphere, heat and light
determine its applications. The antibacterial, anti-fungal, disinfection, and toxicity,
properties of the nanoparticles are ideal for biomedical and environmental applications.
Corrosive, anti-corrosive, oxidation, reduction and flammability characteristics of the
nanoparticles determine their respective usage.
Methods to synthesize nanoparticles
The nanoparticles are synthesised by various methods that are categorised into bottom-
up method or top-down method.[10]

3.1. Bottom-up method

Bottom-up or constructive method is the build-up of material from atom to clusters to
nanoparticles. Sol-gel, spinning, chemical vapour deposition (CVD), pyrolysis and
biosynthesis are the most commonly used bottom-up methods for nanoparticle production
3.2. Top-down method
Top-down or destructive method is the reduction of a bulk material to nanometric scale
particles. Mechanical milling, nanolithography, laser ablation, sputtering and thermal
decomposition are someof the most widely used nanoparticle synthesis methods.

The synthesis of nanoparticles requires the use of a device or process that fulfills the
following conditions [11]:
 control of particle size, size distribution, shape, crystal structure and composition

distribution
  improvement of the purity of nanoparticles (lower impurities)
 control of aggregation
 stabilization of physical properties, structures and reactants
 higher reproducibility
 higher mass production, scale-up and lower costs

a. Size Control Of Nanoparticles

The physical and chemical properties of nanomaterials depend not only on their
composition but also on the particle size and shape . For example, if the diameter of an
Au nanosphere is made to increase, the surface plasmon resonance will be gradually
shifted from 530 nm to the longer wavelength side Thus, if nanoparticles differ in size,
their optical characteristics will also change significantly.
b. Structure Control of nanoparticles:
Nanoparticles that are composed of two or more metals differ in their catalytic,
magnetic, and optical characteristics from nanoparticles that consist of a single
metal.[12] Such nanoparticles can be sub-divided into three kinds of structures:
(i) the alloy structure that exists randomly in a crystal;
(ii) the core–shell structure in which the metal at the center differs from the peripheral
metal; and
(iii) the twinned hemisphere structure wherein two sorts of hemispheres are joined.

Classification of nanoparticles
According to Siegel, Nanoparticles are classified as
 zero dimension nanoparticles
The electrons are confined along all directions.The electrons are not allowed to move anywhere in the
system.
E.g. Quantum dots ( small dia nanoparticles

• One dimension nanoparticles

The electrons are confined in two directions. The electrons are allowed to move in only one direction
in the system.

E.g. Nanowires, Nanotubes.

• Two dimension nanoparticles

The electrons are confined in only one directions. (X or Y or
Z)The electrons are allowed to move in any two directions in the
system.
Carbon nanotubes

• Three dimension nanoparticles

The electrons are confined in all directions. The electrons are
allowed to move in three directions in the system.
Dendrimers, Quantum Dots, Fullerenes (Carbon 60)QDs

Depending on the application (i.e. diagnosis, imaging or therapy), different types of NPs (Figure 3)
have been proposed, being some of them used for more than one aim. In this section, NPs types are
divided in two main groups:

1.organic Nanoparticles
The first group includes micelles, dendrimers, liposomes, hybrid and compact polymeric
NPs.These nanoparticles are biodegradable, non-toxic, and some particles such as micelles and
liposomes has a hollow core , also known as nanocapsules and are sensitive to thermal and
electromagnetic radiation such as heat and light.

2.InorganicNanoparticles
Inorganic nanoparticles are particles that are not made up of carbon.The second group
contains fullureenes quantum dots, silica and gold Nanoparticles..It also contain metal
based and metal oxide based nanoparticles.[13]
3. Carbon based nnanoparticles

The nanoparticles made completely of carbon are knows as carbon based [8]. They can
be classified into fullerenes, graphene, carbon nano tubes (CNT), carbon nanofibers and
carbon black and sometimes activated carbon in nano size [14] and are presented in
Figure

Applications of nanoparticles
Manufactured nanoparticles in recent years become available in products from paints to
cosmetics and car tyres to self-cleaning windows and printing inks to cosmetics [64, 65].
Fig. 1.10 shows the applications of nanomaterials in various fields.
1. Medicine

a) Nano drugs
Nanomaterials are used as nano drugs for the cancer and TB therapy.

b) Laboratories on a chip
Nanotechnology is used in the production of laboratories on a chip.

c) Nano-medibots
Nanoparticles function as nano-medibots that release the anti-cancer drug and treat
cancer.

d) Gold-coated nanoshells
It converts light into heat, enabling the destruction of tumours.

e) Gold nanoparticles as sensors

Gold nanoparticles undergo colour change during the transition of nanoparticles.

f) Protein analysis
Protein analysis can also be done using the nanomaterials.

g) Gold nanoshells for blood immuno assay

Gold nanoshells are used for blood immuno assay.

h) Gold nanoshells in imaging

Optical properties of the gold nano-shells are utilized for both imaging and therapy
i) Targeted drug delivery using gold nanoparticles
It involves slow and selective release of drugs to the targeted organs.

j) Repairing work
Nanotechnology is used to partially repair neurological damage.

1.5.2. Industries

(a) As catalyst
It depends on the surface area of the material. As nanoparticles have an appreciable
fraction of their atom at the surface, their catalytic activity is good.
Example: Bulk gold is chemically inert, whereas, gold nanoparticles have excellent
catalytic property.
(b) In water purification
Nano-filtration makes use of nanoporous membranes having pores smaller than 10 nm.
Dissolved solids and colour producing organic compounds can be filtered very easily
from water. Magnetic nanoparticles are effective in removing heavy metal contamination
from waste water.

(c) In fabric industry

The production of smart-clothing is possible by putting a nano-coating on the fabric.
(i) Embedding the nanoparticles on the fabric makes them stain repellent.
(ii) Socks with embedded silver nanoparticles fill all the bacteria and makes it odour free.

(d) In automobiles
(i) Incorporation of small amount of nanoparticles in car bumpers can make them
stronger than steel.
(ii) Specially designed nanoparticles are used as fuel additives to lower the
consumption in vehicles.

(e) In food industry

The inclusion of nanoparticles in food contact materials can be used to generate
the novel type of packing materials and containers.

(f) In energy sector

In solar power, nanotechnology reduces the cost of photovoltaic cells by 10 to 100 times.

1.5.3. In electronics
a) Quantum wires are found to have high electrical conductivity.
b) The integrated memory circuits are found to be effective devices.
c) Nanowires are used to build transistors without p - n junctions.
d) Nanoradios are the other important devices, using carbon nanotubes.

1.5.4. As biomaterials
a) Nanomaterials are used as bone cement and bone plates in hospitals.
b) It is also used as a material for Joint replacements
d) It is used in manufacture of some components like heart valves and contact lenses.

Nanoparticles in Textiles and Clothing

Within the last span, Nanotechnology based progress in textile laments, yarns, and fabric
finishing have directed to the growth of numerous new and enhanced textile
products.[15]

Nanoparticles in Cosmetics
Nanotechnology and nanomaterials are found to be useful in several cosmetics products
like conditioners, make up, suntan lotion and hair care products

Applications in the environment

Most of environmental applications of nanotechnology fall into three categories:
1. Environmentally benign sustainable products (e.g. green chemistry or pollution
prevention).
2. Remediation of materials contaminated with hazardous substances and
3. Sensors for environmental stage

Applications in energy harvesting

Recent studies warned us about the limitations and scarcity[16]
of fossil fuels in coming years due to their nonrenewable nature.
a) Scientists shifting their research strategies to generate renewable energies from easily available
resources at cheap cost.
b)NPs are widely used to generate energy from photoelectrochemical (PEC) and electrochemical
water splitting.

Material Required:
 Cu(CH3COO)2·H2O,
  polyvinylpyrrolidone
 PVP M. Wt. 55,000), ethylene glycol {HO(CH2)2 OH},
 1, 3 propanediol {CH2OH(CH2)2OH} and NaOH

Apparatus:

Centrifuge Machine

Hot plate

Magnetic stirrer

Beakers

Measuring cylinder

Conical flask

Procedure:

Required amount of PVP was added in 15 ml polyol (EthyleNe Glycol/TMEG)
 Now stirred the solution for about 15 minutes until it dissolved completely.
Different amounts of NaOH and (CH3COO)2Cu· H2O were also added to the
above solution and stirred it about 30 minutes in order to get the pH value of
reactants at 9.
 The solution was then poured in Teflon lined sealed stainless steel autoclave and
subjected to the hydrothermal treatment (HT) for 24 h at different temperature
under autogenous pressure.. It is then allowed to cool naturally to room
temperature. The precipitate so obtained is placed in a furnace and annealed in air
at particular temperature for 1 hour.
 After hydrothermal treatment, samples thus obtained was centrifuged, washed
several times with methanol and finally collected with drying in room temperature
separately. The dried samples were separated and powdered.
 The formation of nano CuO from Cu(OH)2 precipitant, the following reaction mechanism can
be formulated in terms of equations as followed,
  The X-ray characterization of the prepared powder samples was carried out using Rigaku
Xray diffractometer having Cu Kα radiation.
 The preliminary observation of the size and shape of the particles as well as the shape and
m
o
r
p
h
o
l
o
g
y of the fine particles were analyzed using were carried out by Scanning Electron
Microscope.[17]

X-Ray Diffraction
X-rays are electromagnetic radiation similar to light, but with a much shorter wavelength
(few Angstrom). They are produced when electrically charged particles of sufficient
energy are decelerated. In an X-ray tube, the high voltage maintained acrossthe electrodes
draws electrons toward a metal target (the anode). X-rays are produced at the point of
impact, and radiate in all directions. ZBasic Principle
If an incident X-ray beam encounters a crystal lattice, general scattering occurs. Although
most scattering interferes with itself and is eliminated (destructive interference),
diffraction occurs when scattering in a certain direction is in phase with scattered rays
from other atomic planes. Under this condition the reflections combine to form new
enhanced wave fronts that mutually reinforce each other (constructive interference). The
relation by which diffraction occurs is known as the Bragg’s law or equation. [18]As each
crystalline material have a characteristic atomic structure, it will diffract X-rays in a
unique characteristic diffraction order or pattern. S
Applications
X-ray diffraction (XRD) is a powerful method for the study of nanomaterials (materials
with structural features of at least one dimension in the range of 1-100 nm).
X-ray diffractograms of nanomaterials provide a wealth of information - from phase
composition to crystallite size, from lattice strain to crystallographic orientation.
The main use of powder diffraction is to identify components in a sample by a
search/match procedure. Furthermore, the areas under the peak are related to the amount
of each phase present in the sample.
In 1919 A.W.Hull gave a paper titled, “A New Method of Chemical Analysis”. Here he
pointed out that....
“The X-ray diffraction pattern of a pure substance
is, therefore, like a fingerprint of the substance.
The powder diffraction method is thus ideally
suited for characterization and identification of
polycrystalline phases".

Scanning Electron Microscopy (SEM)

The scanning electron microscope (Fig. 1) is an electron microscope that images the
sample surface by scanning it with a high energy beam of electrons. Conventional light
microscopes use a series of glass lenses to bend light waves and create a magnified
image while the scanning electron microscope creates the magnified images by using
electrons instead of light waves.[19]
Basic Principle
When the beam of electrons strikes the surface of the specimen and interacts with the
atoms of the sample, signals in the form of secondary electronsscattered electrons and
characteristic X-rays are back generated that contain information about the sample's
surface topography, composition, etc. The SEM can produce very high-resolution images
of a sample surface, revealing details about 1-5 nm in size in its primary detection mode
i.e. secondary electron imaging.

App
licat
ions
The
SEM
show
s
very
detailed three dimensional images at much high magnifications (up to ×300000) as
compared to light microscope (up to × 10000).
The surface structure of polymer nanocomposites, fracture surfaces, nanofibres,
nanoparticles and nanocoating can be imaged through SEM with great clarity
The SEM technique can also be used to view the dispersion of nanoparticles such as
carbon nanotubes, nanoclays and hybrid POSS nanofillers in the bulk and on the surface
of nanocomposite fibres and coatings on yarns and fabric sample.
In tissue engineering or cell culture applications, the SEM image is the prime
characterization technique for scaffold construction, cell development and growth .

Thermogravimetric Analysis (TGA)

: Thermogravimetric Analysis is a technique in which the mass of a substance is

monitored as a function of temperature or time as the sample specimenis subjected to a
controlled temperature program in a controlled atmosphere. TGA is a technique in
which, upon heating a material, its weight increases or decreases. TGA measures a
sample’s weight as it is heated or cooled in a furnace.

Basic Principle
A TGA consists of a sample pan that is supported by a precision balance. That pan
resides in a furnace and is heated or cooled during the experiment. The mass of the
sample is monitored during the experiment. A sample purge gas controls the sample
environment. This gas may be inert or a reactive gas that flows over the sample and
exits through an exhaust. [20]
The abscissa (X-e displayed as time or temperature and the ordinate (Y-axis) can be
displayed as weight (mg) or weight percent (%).

A TGA thermal curve is displayed from left to right. The descending TGA thermal curve
indicates a weight loss occurred. A 15.013 mg sample of calcium carbonate was
analyzed. Temperature Program = Heat from 100 °C to 900 °C @ 10 °C/minutein
Nitrogen atmosphere with a purge rate of 20 mL/minute
Applications
TGA is widely used as a QA/QC tool in the manufacture and use of Carbon Nano Tubes
(CNT). TGA is used in CNT manufacturing process to characterize the amount of
metallic catalytic residue that remains on the CNT.
TGA is used to characterize end products that contain Nanoparticles (NP) or CNTs as in
their usual end productscharacterizations.

TGA is used in the analysis of ceramics and thermally stable polymers.

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