Zinc alloys are cost able to closer tolerances than other metals or molded plastics,

therefore presenting the opportunity to reduce or eliminate machining. Net Shape is Zero
Machining manufacturing is a major advantage of zinc casting.
Zinc alloys offer high strengths (to 60,000 pies) and superior elongation for strong designs and
formability for bending, crimping and riveting operations. Few materials provide the strength
and toughness of zinc alloys. Impact resistance is significantly higher than cast aluminum alloys,
plastics, and grey cast iron. Zinc alloys have the rigidity of metals with

Modulus of elasticity characteristics equivalent to other die cast able materials. Stiffness
properties are, therefore, far superior to engineering plastics. Zinc alloys are non sparking and
suitable for hazardous location applications such as coal mines, tankers and refineries. Bushing
and wear inserts in component designs can often be eliminated because of zinc's excellent
bearing properties. For example, zinc alloys have outperformed bronze in heavy duty industrial
applications. Zinc castings are readily polished, plated, painted, chromate or anodized for
decorative and functional service. High casting fluidity, regardless of casting process, allows for
thinner wall sections to be cast in zinc compared to other metal. Fast, trouble-free machining
characteristics of zinc materials minimize tool wear and machining costs. Because of their low
melting temperature, zinc alloys require less energy to melt and cast versus other engineering
alloys. Low casting temperatures result in less thermal shock and, therefore, extended life for
die casting tools. For example, tooling life can be more than 10 times that of aluminum dies.
Zinc alloys are among the cleanest melting materials available. Zinc metal is non-toxic, and
scrap items are a reusable resource which is efficiently recycled.


CHAPTER-V

RESULT AND DISSCUSION

5.1 INTRODUCTION

In this present study, the zinc material is deposited on copper substrate by thermal
evaporation method. Thin film preparation is very important process of control the particle size,
particle shape and morphology. The deposited zinc thin films were characterized by X-ray
diffraction and field emission scanning electron microscope studies. XRD study is the most
important tool in thin film technology. In X-ray diffraction spectrum film morphology, FWHM
(Full Width at Half Maximum), Diffraction angle, intensity, diameter of particle, d-spacing has
been calculated. The X-ray diffraction results shows the particle size is less than 100 nm at
100C and particle size is less than80 nm at 200C.

Metal thin films are attracting the attention of present science field because of their
physical and chemical properties these are quite dissimilar from those of bulk materials. Various
techniques have been adopted to produce thin films on copper substrates.

The field emission scanning electron microscope (FE-SEM) is a type of electron
microscope that images the sample surface by scanning it with a high energy beam of electrons
in a raster scan pattern. Electron emitter from field emission gun was used. These types of
electron emitters can produce up to 1000x the emission of a tungsten filament. However, they
required much higher vacuum conditions. After the electrons beam exit the electron gun, they
then confined and focused, monochromatic beam using metal apertures and magnetic lenses.
Finally, Detectors of each type of electrons are placed in the microscopes that collect signals to
produce an image of the specimen particles morphology of our samples was investigated using
Nova 200 Nano Lab field emission scanning electron microscope (FE-SEM).

Field emission scanning electron microscopy (FE-SEM) demonstrates spectacular
changes in morphology of zinc thin films is deposited on copper substrate at different
temperature 100C &200C. Using the fractional dimension of the assembly of nanostructures in
the thin films has been estimated. The effects of thin films surface morphology and fractal
dimension, structure, composition have been discussed.

4.2 ENERGY DISPERSIVE X-RAY SPECTROSMETRY (EDS)

EDS has a much finer spectral resolution. EDS avoids the problems associated with
artifacts in EDS (false peaks, noise from the amplifiers, and micro phonics). EDS gathers
a spectrum of all elements, within limits, of a sample. Four primary components of the EDS
setup are, 1. The excitation source (electron beam or x-ray beam) 2.The X-ray detector 3.The
pulse processor 4. The analyzer.

EDS makes use of the X-ray spectrum emitted by a solid sample bombarded with a
focused beam of electrons to obtain a localized chemical analysis. All elements from atomic
number 4 (Be) to 92 (U) can be detected in principle, though not all instruments are equipped for
'light' elements (Z < 10). Qualitative analysis involves the identification of the lines in the
spectrum and is fairly straightforward owing to the simplicity of X-ray spectra. Quantitative
analysis (determination of the concentrations of the elements present) entails measuring line
intensities for each element in the sample and for the same elements in calibration Standards of
known composition.
By scanning the beam in a television-like raster and displaying the intensity of a selected
X-ray line, element distribution images or 'maps' can be produced. Also, images produced by
electrons collected from the sample reveal surface topography or mean atomic number
differences according to the mode selected. The Scanning Electron Microscope (SEM), which is
closely related to the electron probe, is designed primarily for producing electron images, but can
also be used for element mapping, and even point analysis, if an X-ray spectrometer is added.
There is thus a considerable overlap in the functions of these instruments.

4.3 X- RAY DIFFRACTION STUDIES

Powder X-ray diffraction (XRD) is one of the primary techniques used to characterize the
zinc sample is coated on copper substrate. X-ray diffraction is most important characterization of
used materials size, particle diameter, Full Width at Half Maximum, diffraction angle, intensity,
shape can be calculated.
XRD analysis of the prepared sample of zinc nano thin films was done by a Goniometer
smart lab 2-theta gonio, under 30kv, 100mA X-ray, scanning mode continuous.

The scherrer equation is used to calculate, the grain size of zinc thin films from X-ray
diffraction results. The scherrer equation for particle size as follows,


1

D = particle diameter size in thin films (which may be smaller or equal the grain size)
= Wavelength of the X-ray (0.1542nm)
= Diffraction angle
0.9
D = -------------
Cos

= Full Width at Half Maximum intensity after subtracting the instrumental line broadening, in
(radian). This quantity is also sometimes denoted as (2).
K = is the dimension less shape factor, with a value close to unity the shape factor has typical
Value is (0.9)

Braggs law

2dsin=n

- Is the wavelength of the X- ray

- Diffraction angle

d - Interplannar distance

n - Order of the thin films layer

4.3.1 XRD PATTERN OF ZINC THIN FILMS AT 100c

Figure.1 shows the XRD pattern of diffraction of zinc thin films deposited on copper
substrate at 100C. The diffraction peaks are observed and the peaks are shown from
36.4446(degree) to 77.2666(degree). The full width half maximum (FWHM) indicated in the
range from 0.00211 (radian) to 0.00209(radian) and the diatomic spacing of the zinc thin films
2.4571 to 1.2338. The maximum height of the peaks is 26393(cps) at 36.4446(degree) to
895(cps) at 77.2666(degree).


Figure.4.1 XRD Pattern of Zinc Thin Films at 100C

Figure 4.2 Zinc Thin Films at 100C on Copper Substrate
Table.1 Zinc Thin Films at 100C 2 values in (degree) and Height in (cps)
20 30 40 50 60 70 80
0e+000
1e+004
2e+004
3e+004
Z
i
n
c
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5
2-theta (deg)
I
n
t
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n
s
i
t
y

(
c
p
s
)
2(degree) d(angle) Height(cps) FWHM(degree)
36.4446 2.45711 26393 0.1210
37.78 2.3792 249 0.13
43.409 2.08291 17425 0.162
54.557 1.6807 614 0.104
70.249 1.33807 1497 0.118
77.266 1.23380 895 0.120

Table.1 shows the XRD pattern of diffraction thin films on copper substrate at 100C.
The different 2 values are observed. Then corresponding theta values, the d-spacing values in
angle, Height values in (cps), Full width at half maximum values in (degree) are observed.
The 2 value is 36.4446 (degree), at the time the d-spacing value is 2.45711 (angle), the
Height of the peak is 26393 (cps), the full width at half maximum value is 0.1210 (degree).
The 2 value is 37.78 (degree), at the time the d-spacing value is 2.3792 (angle), the
Height of the peak is 249 (cps), the full width at half maximum value is 0.13 (degree).
The 2 value is 43.409 (degree), at the time the d-spacing value is 2.08291 (angle), the
Height of the peak is 17425 (cps), the full width at half maximum value is 0.162 (degree).
The 2 value is 54.557 (degree), at the time the d-spacing value is 1.6807 (angle), the
Height of the peak is 614 (cps), the full width at half maximum value is 0.104 (degree).
The 2 value is 70.249 (degree), at the time the d-spacing value is1.33807 (angle), the
Height of the peak is1497 (cps), the full width at half maximum value is 0.118 (degree).
The 2 value is 77.266 (degree), at the time the d-spacing value is1.23380 (angle), the
Height of the peak is 895 (cps), the full width at half maximum value is 0.120 (degree).
Table2 Zinc Thin Films at 100C Miller Indices, d-spacing values in (nm)
2 of the intense peak
(degree)
Miller indices (h k l) d-spacing (nm)
36.4446 002 0.2459
39.1380 100 0.2381
43.3866 101 0.2084
54.5453 102 0.1682
70.3911 103 0.1336
70.9202 110 0.1327
77.4246 004 0.1231

From Table.2 the X-ray studies the distance along the film from the center, the Bragg angle 2
and therefore the d-spacing for each reflection can be calculated. The 2 value is 36.4446
(degree) at corresponding Miller Indices is (002) the d-spacing value is 0.2459nm.
The intense peak 2 value is 39.1380 (degree) at corresponding Miller Indices values is
(100), and d-spacing value is 0.2381(nm).
The intense peak 2 value is 43.3866 (degree) at corresponding Miller Indices values is
(101), and d-spacing value is 0.2084 (nm).
The intense peak 2 value is 54.5453 (degree) at corresponding Miller Indices values is
(102), and d-spacing value is 0.1682 (nm).
The intense peak 2 value is 70.3911 (degree) at corresponding Miller Indices values is
(103), and d-spacing value is 0.1336 (nm).
The intense peak 2 value is 70.9202 (degree) at corresponding Miller Indices values is
(110), and d-spacing value is 0.1327 (nm).
The intense peak 2 value is 77.4246 (degree) at corresponding Miller Indices values is
(004), and d-spacing value is 0.1231 (nm).
Table 3 Zinc Thin Films at 100C Size of the Particle and FWHM () values in radians

FWHM of intense peak
(radians)
Size of the particle (nm) d-spacing(nm)
0.00211 69.26 0.2459
0.00226 64.90 0.2381
0.00282 52.855 0.2084
0.00181 86.07 0.1682
0.00205 82.79 0.1339
0.00340 51.13 0.1280
0.00209 84.88 0.1234

The intense peak value of (FWHM) full width at half maximum is 0.00211(radians), the
corresponding size of the particle is 69.26 nm, and the d-spacing value is 0.2459 nm.
Intense peak value of (FWHM) full width at half maximum is 0.00226 (radians), the
corresponding size of the particle is 64.90 nm, and the d-spacing value is 0.2381 nm.
Intense peak value of (FWHM) full width at half maximum is 0.00282 (radians), the
corresponding size of the particle is 52.855 nm, and the d-spacing value is 0.2084 nm.
Intense peak value of (FWHM) full width at half maximum is 0.00181 (radians), the
corresponding size of the particle is 86.07 nm, and the d-spacing value is 0.1682nm.
Intense peak value of (FWHM) full width at half maximum is 0.00205 (radians), the
corresponding size of the particle is 82.79 nm, and the d-spacing value is. 0.1339nm.
Intense peak value of (FWHM) full width at half maximum is 0.00340 (radians), the
corresponding size of the particle is 51.13 nm, and the d-spacing value is. 0.1280nm.
Full Width Half Maximum intense peak value is 0.00209(radians) the corresponding size
of the particle 84.88 nm d-spacing value is 0.1234 nm.
4.3.2 XRD PATTERN OF ZINC THIN FILMS AT 200c
Figure.3 shows the XRD pattern of diffraction of zinc thin films deposited on copper
substrate at 200c. The diffraction peaks are observed at 2 values. The peaks are shown from
43.348(degree) to 74.024(degree). The full width half maximum (FWHM) indicates the range
from 0.00300 (radian) to 0.00324(radian) and the diatomic spacing of the zinc thin films
2.0857 to 1.2796. The maximum height of the peaks about 23974(cps) at 43.348 (degree)
to 778 (cps) at 74.024 (degree).
Figure.4.3 XRD Pattern of Zinc Thin Films at 200C

Figure 4.4 Zinc Thin Films at 200C on Copper Substrate
Table.4 Zinc Thin Films at 200C 2 values in (degree) and Height in (cps)
2(degree) d(angle) Height(cps) FWHM(degrees)
20 30 40 50 60 70 80
0e+000
1e+004
2e+004
3e+004
C
o
p
p
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r
,

C
u
,

(
1

1

1
)
,

2
.
0
8
7
2
,

4
3
.
3
1
5
8
C
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,

C
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(
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8
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4
4
8
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3
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8
9
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9
3
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4
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3

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8
9
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9
3
4
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1
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0
4
3
6
,

9
5
.
1
4
4
2
20 30 40 50 60 70 80
0.0e+000
5.0e+003
1.0e+004
I
n
t
e
g
r
a
t
e
d

I
n
t
e
n
s
i
t
y

(
c
p
s

d
e
g
)
2-theta (deg)
I
n
t
e
n
s
i
t
y

(
c
p
s
)
5000216
43.348 2.0857 23974 0.172
50.461 1.8071 3317 0.207
74.024 1.2796 778 0.186
In the Debye-Scherrer photographic method, a film was wrapped around the inside of X-
rays camera. The powder, sealed in a glass capillary tube, diffracts the X-rays (Braggs law) to
produce cones of diffracted beams. These cones intersect a strip of photographic film located in
the cylindrical camera to produce a characteristic set of arcs on the film. The film can be
removed and examined. Using the radius of the camera and the distance along the film from the
center, the Bragg angle 2 and therefore the d-spacing for each reflection can be calculated. The
2 value is 43.348 (degree), at the time the d-spacing value is 2.0857 (angle), the Height of the
peak is 23974 (cps), the full width at half maximum value is 0.172 (degree).
The 2 value is 50.461 (degree), at the time the d-spacing value is1.8071 (angle), the
Height of the peak is 3317 (cps), the full width at half maximum value is 0.207 (degree).
The 2 value is 74.024 (degree), at the time the d-spacing value is1.2796 (angle), the
Height of the peak is778 (cps), the full width at half maximum value is 0.186 (degree).
Table 5 Zinc Thin Films at 200C Miller Indices, d-spacing values in (nm)

2 of the intense peak
(degree)
Miller indices (h k l) D spacing (nm)
43.348 111 0.2087
50.461 200 0.1808
74.024 220 0.1280

The 2 value is 43.348at corresponding Miller Indices is (111) the D-spacing value is
0.2087nm, next 2 value is 50.461 at corresponding Miller Indices is (200) the D-spacing value
is 0.1808nm, and 2 value is 74.024 at corresponding Miller Indices is (220) the D-spacing
value is 0.1280nm.
Table6 Zinc Thin Films at 100C Size of the Particle and FWHM () values in radians

FWHM of intense peak
(radians)
Size of the particle (nm) d-spacing(nm)
0.00300 49.77 0.2087
0.00361 42.48 0.1808
0.00324 53.56 0.1280

The intense peak value of (FWHM) full width at half maximum is 0.00300(radian), the
corresponding size of the particle 49.77nm, the d-spacing value is 0.2087nm , FWHM value is
0.00361(radian) the corresponding size of the particle 42.48nm d-spacing value is 0.1808nm,
FWHM value is 0.00324(radian) the corresponding size of the particle 53.56nm d-spacing value
is 0.1280nm,
Zinc nano thin films studied extensively due to their potential technological applications
in various fields. X-ray diffraction is an easy and one of the most important characterization
tools used in nano thin films research field. Here, an important zinc nano thin film has been
successfully prepared physical vapour deposition in thermal method Different Temperature
100C and 200C its structural characterizations have been studied by important tool - X-ray
diffraction.
The results confirm nano thin films, uniformed size at 100C less than92 nm. seven peaks
at 2_ values of 36.4446(degree) ,d-spacing values is0.2459nm, Miller Indices is (002) to 2
values is 77.4246(degree),d-spacing values is 0.1234(nm), Miller Indices is (004), the zinc is
(HCP) Hexagonal Closed Packed structure standard powder diffraction. The XRD study
confirms / indicates that the resultant particles are (HCP) Zinc Nano particles .In addition to this
100C&200C, the experimental powder diffraction pattern (HCP) structure are presented.

4.4 FE-SEM
Zinc is an n-type wide band gap semiconductor with the band gap of 3.37eV and as
various potential applications such as optoelectronic devices, chemical sensors and gas sensors.
Also, bio-safe characteristics of zinc make them very attractive for biomedical applications.
Moreover, zinc in the form of nano structures would enhance the gas-sensing properties of gas
sensors due to a huge surface area. Thus it is a great interest to study the synthesis of zinc
structure.
The zinc thin film is rarely reported. The zinc structure is synthesized by zinc thin films
by physical vapour deposition technique. The zinc thin film is prepared by thermal evaporation
method at different temperatue100C and 200C. Zinc structures were investigated by (FE-
SEM) field emission scanning electron microscopy. To obtained the zinc thin films in (FE-SEM)
structure of zinc and present of the compositions.








4.4.1 FE-SEM AT 100C

















Figure.
4.5 EDX compositions present in zinc thin films at 100C



Figure.4.6 FE-SEM Zinc Thin Films structure at 100C


A typical color of zinc thin film is grey. After heating a color of thin film turns white. This is
typical color for zinc nanostructures. The general morphology of the heated zinc nanostructures
is shown in figure 6. The (FE-SEM) Figure 5 is zinc nanostructure deposited composition on
copper substrate is temperature 100
o
C


Fig .4.7 FE-SEM Zinc Structure at 100
o
C



Fig.4.8 FE-SEM Zinc Structure at 100
o
C

Figure7, 8 shows zinc morphological structure of copper substrate at100C. The (FE-SEM) field
emission results the structure of zinc is hexagonal structure or hexagonal closed packed structure.
The size of particle on100C is 100nm and the most intense diffraction lines is (002), (100),
(101), (102), (103), (110), (004) respectively. This texture is in accordance with the hexagonal
surface morphology usually detected for these deposits. The development if a different texture is
possible during the growth of metal coatings and is a consequence of surface energy differences,
which are responsible for the selective growth of the grains that have the lowest surface free
energy. For the zinc crystal the lowest surface energy is the basal (002) plane, owing to its
compactness
4.4.2 FE-SEM AT 200C

A typical color of zinc thin film is grey. After heating a color of thin film turns white.
This is typical color for zinc nanostructures. The general morphology of the heated zinc nano
structures is shown in figure10. The (FE-SEM) figure 9 of zinc nanostructure deposited
compositions on copper substrate is temperature 200
o
C
Figure11,12 shows zinc morphological structure of copper substrate at200C . The (FE-
SEM) field emission results the structure of zinc is hexagonal structure or hexagonal closed
packed structure. The size of particle on200C is 100nm and the most intense diffraction lines is
(111), (200), (220) respectively. This texture is in accordance with the hexagonal surface
morphology usually detected for these deposits. The development if a different texture is
possible during the growth of metal coatings and is a consequence of surface energy differences,
which are responsible for the selective growth of the grains that have the lowest surface free
energy. For the zinc crystal the lowest surface energy is the basal (002) plane, owing to its
compactness



Figure.4.9 EDX compositions present in zinc thin films at 200C





Figure .4.10 FE-SEM Zinc Thin Films structure at 200C




Fig .4.11 FE-SEM Zinc Structure at 200
o
C



Fig .4.12 FE-SEM Zinc Structure at 200
o
C


Table 7 Shape and Size of the Zinc Thin Films at Different Temperature
Substrate
Substrates
Temperature(C)
Shape Size(nm)
Copper 100C Hexagonal 39-92 nm
Copper 200C Hexagonal 36-77 nm

The zinc thin films on coated on copper substrate by thermal evaporation method at
different temperature 100C and 200C. The size of the particle (or) grain size is observed by
XRD results. The shape of the zinc particle is Hexagonal is confirmed by (FE-SEM) results. Zinc
thin films at 100C the shape is hexagonal, the grain size is 39-92 (nm). Is the same for zinc thin
films at 200C the shape is hexagonal, the particle size is 36-77 (nm).
Table 8 EDX present chemical composition at100C
Element Weight Atomic
Cu K 2.84 13.27
OK 1.18 4.16
Zn K 95.98 82.5

The EDX results from presenting the element, and their element Weight, Atomic with percentage
is represented. The copper is present at weight is 2.84, Atomic is 3.27. The Oxide is present
at Weight is1.18, Atomic 4.16. The Zinc is presented at Weight is 95.98, Atomic is
82.5.these are chemical composition of the EDX results at100C.




Table 9 EDX present chemical composition at 200C
Element Weight Atomic
OK 28.85 62.18
Cu K 19.99 10.85
Zn K 51.16 26.98

The EDX results from presenting the element, and their element Weight, Atomic with
percentage is represented. The copper is present at weight is 19.99, Atomic is 10.85. The
Oxide is present at Weight is28.85, Atomic 62.18. The Zinc is presented at Weight is
51.16, Atomic is 26.98.these are chemical composition of the EDX results at200C.