Chapter-4 Characterization Techniques X-Ray Diffraction (XRD)

CHAPTER-4
CHARACTERIZATION TECHNIQUES
X-RAY DIFFRACTION(XRD):
X-ray diffraction interprets the definitive method to regulate the lucid
construction of solid fabrics.For X-rays to yield useful data about the social
system,the wavelength of the incident X-rays should be of the like ordination of
magnitude as the interatomic spatial arrangement in the crystal construction.The
prevailling effectuate that occurs when an incident radiate of monochromm X-rays
interacts with a aim substantial is dispersion of those X-rays from particles within
the mark substantial.
In substantial with unconstipated social system,the dispersed X-rays undergo

constructive and destructive preventative.This is the operation of
diffraction.Intervention occurs among the waves disconnected by particles when
lucid solids are uncovered to X-rays.Constructive intervention haps when the
waves are motivating in stage with each other.Destructive intervention comes when
the flaps are out of stage.The diffraction form received acts as like a singular
fingermark of fabrics.recognition is done by comparison it to the known standars.
 To seperate between limpid and unstructured fabrics.
 To influence the construction of transparent substantial
 Recognition of lucid ph and mesuration of the congenator ratio.
 To meter diverse kinds of entropy disquiet and imperfections in quartzes.
APPLICATIONS OF FTIR:
 Recognition of unsubdivided mixes of constitute and inorganic
combines.
 Rotaine qualitative and quantitative FTIR depth psychology.
 Decision of useable groups in unknown fabrics.
 Designation of polymers and polymer combines.
 Purpose of grades of crystallinity in polymers
 Collateral check of follow oconstitutional contaminants on rises up.
 Thin film analytic thinking.
 Depth psychology of adhesives,coverings adhesion promoters or matching

factors.
 Recognition of condoms and occupied gum elastics.
 Relative string durations in organics.
 Extent of themic,UV or other abjection or depolymerization of polymers and

pigment coverings.
 Analysis of gaseous tries using a gas cell for environmental survey.
 Analytic thinking of unknown dissolvents, clean up factors and detergents.
ADVANTAGES OF FT-IR:
1. Better speed:
As noted sooner, because all of the frequencies are quantified

simultaneously, most measurations by FT-IR are caused in a few minutes rather
than several proceedings. It is also consulted to as the felgett Advantage.
2. Sensitivity:
Sensibility is dramatically bettered with FT-IR for many causes. The

demodulators applied are much more sensible, the ocular end to end is much
gamier which solutions in much lower interference grades, and the fast scans
enable the co addition of various scans in order to break down the random
mensuration resound to any hoped level.
3. Mechanical calibrated:
The proceeding mirror in the interferometer is the only endlessly

proceedings part in the pawn. Thus, there is very small possibleness of mechanical
breakdown.
4. Internally calibrated:
These pawns hire a He-Ne laser as an interior wavelength standardization

measure. The use of helium- neon laser as the intimate citation in many FT-IR
systems supplies an robotic standardization in an accuracy of better than
0.01.These official document are self-standardization and never need to be
graduated by the user.
5. Increased optical throughput:
Energy- atropy slices are not demanded in the interferometer because

distribution or filtrating is not needed.alternatively,a rotary ocular aperture is
usually used in FT-IR shemes.The beam area of an pawn is normally 75 to 100
clocks bigger than the slice breadth of a dispersive spectrometer. Thus more
irradiation vigour is made usable. This consitutes a major vantage for many tries or
tasting proficiencies that are vitality bounded.
6. Elimination of stray light and emission contributions:
The interferometer in FT-IR regulates all the frequencies. The

unmodulated isolated brightness and taste discharge are not discovered.
7 .Power data station:
Modern FT-IR spectrometer are usually fitted out with a mighty, computerized
data organisation.It can be execute a wide diversity of data treating labors such as
Fourier shift,interactional spiritual deduction,servise line
rectification,shining,consolidation,and library probing.
8. Resolving force of FT-IR Instrumentate is invariable over the intact spectrum,
whereas it several with oftenness in the formal proficiencies.

9.IR depth psychology can be guided at room temperature.
10.Equaly applicable to both expelling and concentration spectroscopy.
DIELECTIC STUDIES:
Every fabric has a singular set of electrical features, which are insulator
attributes, like permittivity, permeableness, impendence, conductivity,etc. A fabric
is sorted as dielectric if it has the power to shop vigour when an extraneous electric
field is employed.In other quarrel,textiles,which are electric dielectrics or in which
an electric field can be maintained with a lower limit dissolution of force, are
known as dielectric fabrics.simply,dielectrics are isolating materials.
In dielectrics all the electrons are edge to their parent motes and there are
no free alternation. even with rule electric potential or caloric vitality the electrons
are not loosed. Dielectrics are non metallic of high particular impedance and have
minus temperature coefficient of immunity. the dielectric features of the substantial
are significant to study the grille kinetics in the crystal. it is significant to note that
permittivity and permeability are not invarient.they can alternation with oftenness,
temperature, orientation,mixing,force,and molecular construction of the fabric.
Many authors hashed out several dielectric attributes, dielectric diligence and
dielectric hypotheses in details.
In the represent probe the dielectric survey was conducted out by valuating
dissimilar parametric quantities such as condenser and dielectric loss of the
compressed shots of tastes of known proportion at room temperature on Agilent
4284 pression inductor,codensor and immunity meter using particularly planned
sample holder, within the frequance rate from 1KHZ to 1MHZ.
DIELECTIRC LOSS:
The dielectric loss is a loss of vigor which finally create a accession in

temperature of a dielectric located in an understudying electrical field. In other
words it isa mensuration of the energy intent by dielectric. it is the electrical energy
lost as hotness in the polarization operation in used AC electric field. The ratio of
notional part to the real part of the comparative permittivity is known as dielectric
deprivation or the profligacy element D.
CAPACITANCE VOLTAGE MEASUREMENT (C-V):

Capacitance -voltage trying is widely used to influence semiconducting
material parametric quantities in MOSFET constructions. It is an electric, non-
destructive measuration of the roadblock condenser of semiconductor
conjugations, like p-n junctions, metal semiconductor colligation and even metal
-oxide-semiconductor constructions. it can help to interpret the attributes of the
SiO2 and Si interface trap compactness. The canonic expression used to make C-V
mensuration is the MOS condenser, dwelling of a semiconductor, a dielectric
stratum and a metal dire acting electrode. The capacitance- voltage proficiencies
banks on the fact that the width of a opposite founded distance-mission area of a
semiconductor conjunction twist depends on the used potential. The scr width
addiction on potential rests at the center of the C-V Technique.
The process for taking C-V measurations regards the diligrnce of DC bias potential
crosswise the condenser while making the measurations with an AC indicate.
OPTICAL CHARACTERIZATION BY UV-Vis SPECTROSCOPY:
The absorbance spectrum of as grown CuS single crystals was calculated

using 600UV-Vis Spectrometer. The absorbance spectrum of the as grown CuS
Single crystal.The received spectrum distinctly condition that the as grown CuS
Single crystal has acute absorbtion edge at 498nm folled by addition in absorbance
with increase in wavelength which due to the free bearer infra band absorbance
.This result is in good accord with the earlier covered absorbance spectrum for
bulk CuS.The nature of the absorbance cure of CuS Single crystal is an ideal
features of covellite CuS and it adapt that growth of covellite form of copper
sulphate has taken place rather than any other phase.
The visual bandgap of the CuS Single crystal was driven from the absorbance
spectrum using the near-band edge absorption telling. The psychoanalysis showed
that the as grown CuS posses lineal visual bandgab.
PHOTO LUMINESCENCS (PL) SPECTRUM:
The photo luminescence spectra of CuS Single crystals were registered

using Perkin-Elmer LS-55 spectrometer. The room temperature photoluminescence
spectra of the as grown CuS single crystals for three dissimilar fervour
wavelengths.

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CHAPTER-4

In substantial with unconstipated social system,the dispersed X-rays undergo

 To seperate between limpid and unstructured fabrics.

 To influence the construction of transparent substantial

 Recognition of lucid ph and mesuration of the congenator ratio.

 To meter diverse kinds of entropy disquiet and imperfections in quartzes.

 Designation of polymers and polymer combines.

 Purpose of grades of crystallinity in polymers

 Collateral check of follow oconstitutional contaminants on rises up.

 Thin film analytic thinking.

 Depth psychology of adhesives,coverings adhesion promoters or matching

 Recognition of condoms and occupied gum elastics.

 Relative string durations in organics.

 Extent of themic,UV or other abjection or depolymerization of polymers and

 Analysis of gaseous tries using a gas cell for environmental survey.

 Analytic thinking of unknown dissolvents, clean up factors and detergents.

As noted sooner, because all of the frequencies are quantified

Sensibility is dramatically bettered with FT-IR for many causes. The

The proceeding mirror in the interferometer is the only endlessly

These pawns hire a He-Ne laser as an interior wavelength standardization

5. Increased optical throughput:

Energy- atropy slices are not demanded in the interferometer because

6. Elimination of stray light and emission contributions:

The interferometer in FT-IR regulates all the frequencies. The

7 .Power data station:

8. Resolving force of FT-IR Instrumentate is invariable over the intact spectrum,

whereas it several with oftenness in the formal proficiencies.

10.Equaly applicable to both expelling and concentration spectroscopy.

The dielectric loss is a loss of vigor which finally create a accession in

CAPACITANCE VOLTAGE MEASUREMENT (C-V):

OPTICAL CHARACTERIZATION BY UV-Vis SPECTROSCOPY:

The absorbance spectrum of as grown CuS single crystals was calculated

PHOTO LUMINESCENCS (PL) SPECTRUM:

The photo luminescence spectra of CuS Single crystals were registered

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