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Chemical Spray Pyrolysis (CSP)
“Spray pyrolysis is the aerosol process that atomizes a solution and heats the
droplets to produce solid particles.”
Chemical spray pyrolysis (CSP) is used for depositing a wide variety of thin films, which are used
in devices like solar cells, sensors, solid oxide fuel cells etc. It has evolved into an important thin
film deposition technique and is classified under chemical methods of deposition. This method
offers a number of advantages over other deposition processes, the main ones being scalability of
the process, cost effectiveness with regard to equipment costs and energy needs, easiness of
doping, operation at moderate temperatures (100-500˚C) which opens the possibility of wide
variety of substrates, control of thickness, variation of film composition along the thickness and
possibility of multilayer deposition.
Fig: Schematic of Chemical spray pyrolysis

CSP technique involves spraying a solution, usually aqueous, containing soluble salts of the
constituents of the desired compound onto a heated substrate. Typical CSP equipment consists of
an atomizer, a substrate heater, temperature controller and a solution container. Additional features
like solution flow rate control, improvement of atomization by electrostatic spray or ultrasonic
nebulization can be incorporated into this basic system to improve the quality of the films. To
achieve uniform large area deposition, moving arrangements are used where either nozzle or
substrate or both are moved.There are too many processes that occur sequentially or
simultaneously during the film formation by CSP.
These include atomization of precursor solution, droplet transport, evaporation, spreading on the
substrate, drying and decomposition. Understanding these processes will help to improve film
quality. Deposition process in CSP has three main steps: atomization of precursor solutions,
transportation of the resultant aerosol and decomposition of the precursor on the substrate.
Electron Microscopy:
The Basics
1. Introduction
Electron Microscopes are scientific instruments that use a beam of highly energetic electrons to
examine objects on a very fine scale. This examination can yield information about the topography
(surface features of an object), morphology (shape and size of the particles making up the object),
composition (the elements and compounds that the object is composed of and the relative amounts
of them) and crystallographic information (how the atoms are arranged in the object).
Given sufficient light, the unaided human eye can distinguish two points 0.2 mm apart. If the points are
closer together, they will appear as a single point. This distance is called the resolving power or resolution
of the eye. A lens or an assembly of lenses (a microscope) can be used to magnify this distance and enable
the eye to see points even closer together than 0.2 mm. For example, try looking at a newspaper picture, or
one in a magazine, through a magnifying glass. You will see that the image is actually made up of dots too
small and too close together to be separately resolved by your eye alone. The same phenomenon will be
observed on an LCD computer display or flat screen TV when magnified to reveal the individual “pixels”
that make up the image.
2. Types of microscopes
Most microscopes can be classified as one of three basic types: optical, charged particle (electron and ion),
or scanning probe. Optical microscopes are the ones most familiar to everyone from the high school science
lab or the doctor’s office. They use visible light and transparent lenses to see objects as small as about one
micrometer (one millionth of a meter), such as a red blood cell (7 μm) or a human hair (100 μm). Electron
and ion microscopes, the topic of this booklet, use a beam of charged particles instead of light, and use
electromagnetic or electrostatic lenses to focus the particles. They can see features as small a tenth of a
nanometer (one ten billionth of a meter), such as individual atoms. Scanning probe microscopes use a
physical probe (a very small, very sharp needle) which scan over the sample in contact or near-contact with
the surface. They map various forces and interactions that occur between the probe and the sample to create
an image. These instruments too are capable of atomic scale resolution.
Electron Microscopes were developed due to the limitations of Light Microscopes which are limited by the
physics of light to 500x or 1000x magnification and a resolution of 0.2 micrometers. In the early 1930's this
theoretical limit had been reached and there was a scientific desire to see the fine details of the interior
structures of organic cells (nucleus, mitochondria...etc.). This required 10,000x plus magnification which
was just not possible using Light Microscopes.
3. Scanning Electron Microscope (SEM)
Principle: “A scanning electron microscope (SEM) is a type of electron microscope that produces images
of a sample by scanning the surface with a focused beam of electrons. The electrons interact with atoms
in the sample, producing various signals that contain information about the sample's surface topography,
morphology, crystalline behavior and composition.”
Construction and Working Principle:
Figure 1 Schematic diagram of SEM
Scanning Electron Microscopes (SEMs) function exactly as their optical counterparts except that they use a focused
beam of electrons instead of light to "image" the specimen and gain information as to its structure and composition.
The basic steps involved in all Ems are the following: A stream of electrons is formed in high vacuum (by electron
guns). This stream is accelerated towards the specimen (with a positive electrical potential) while is confined and
focused using metal apertures and magnetic lenses into a thin, focused, monochromatic beam. The sample is irradiated
by the beam and interactions occur inside the irradiated sample, affecting the electron beam. These interactions and
effects are detected and transformed into an image.
Electron Gun
The first and basic part of the microscopes is the source of electrons. It is usually a V-shaped filament made
of LaB6 or W (tungsten) that is wreathed with Wehnelt electrode (Wehnelt Cap). Due to negative potential
of the electrode, the electronsare emitted from a small area of the filament (point source). A point source is
important because it emits monochromatic electrons (with similar energy). Thetwo usual types of electron
guns are the conventional electron guns and the fieldemission guns (FEG). Figure 1 illustrates the geometry
of an electron gun.In conventional electron guns, a positive electrical potential is applied to the anode, and
the filament (cathode) is heated until a stream of electrons is produced. The electrons are accelerated by the
positive potential down the column, and because of the negative potential of cap, all electrons are repelled
toward the optic axis. A collection of electrons occurs in the space between the filament tip and Cap, which
is called a space charge. Those electrons at the bottom of the space charge (nearest to the anode) can exit
the gun area through the small (<1 mm) hole in the Whenelt Cap and then move down the column to be
later used in imaging.
Figure 2 Electron Gun
Electron-specimen interactions
When an electron beam interacts with the atoms in a sample, individual incident electrons undergo two
types of scattering - elastic and inelastic (Figure 2). In the former, only the trajectory changes and the kinetic
energy and velocity remain constant. In the case of inelastic scattering, some incident electrons will actually
collide with and displace electrons from their orbits (shells) around nuclei of atoms comprising the sample.
This interaction places the atom in an excited (unstable) state. Specimen interaction is what makes Electron
Microscopy possible. The interactions (inelastic) noted on the top side of the diagram are utilized when
examining thick or bulk specimens (Scanning Electron Microscopy, SEM) while on the bottom side are
those examined in thin or foil specimens (Transmission Electron Microscopy, TEM).
Figure 3 Effects produced by electron bombardment of a material

Applications of SEM
1. Topography: The surface features of an object or "how it looks", its texture; direct relation
between these features and materials properties
2. Morphology: The shape and size of the particles making up the object; direct relation between
these structures and materials properties
3. Composition: The elements and compounds that the object is composed of and the relative
amounts of them; direct relationship between composition and materials properties
4. Crystallographic Information: How the atoms are arranged in the object; direct relation between
these arrangements and material properties

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Fig: Schematic of Chemical spray pyrolysis

Figure 1 Schematic diagram of SEM

Figure 3 Effects produced by electron bombardment of a material

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