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An overview of plasma focus devices, their motivation, experimental setup, diagnostics techniques, and the characterization of ion beams used for depositing zirconium nitride films. The importance of zirconium nitride films due to their durability, high hardness, and chemical stability, among other desirable properties. The document also includes information on the desired surface properties of the deposited films, the experimental setup of the plasma focus device, and the formation of zirconium nitride films.
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LAYOUT
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MOTIVATION
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Wilson Seal
ChamberVacuum
SampleHolder
Shutter
Cathode
Anode
Trigger
S
HV
C
InsulatorSleeve
Vacuumpump Gas Inlet
Guage
Samples
Arrangement and Operation of PF
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Plasma Diagnostic Techniques & Ion Beam Analysis
3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.
0
5
10
15
20
25
-0.
-0.
Time ( s)
BPX65 diode signal ............. HV probe signal
BPX65 signal intensity (arb. units)
HV signal intensity (arb. units)
(^12)
2
E mv
d
V N RqAv
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Why We form Zirconium Nitride?
1 The durability of Zirconium nitride films is about 5 times than that of TiN
film.
2 ZrN shows
a High hardness
b High chemical & thermal stability
c High melting point d High young’s modulus
e High corrosion resistance
f Low electrical resistivity
g Golden color.
a Hard coatings
b Decorative coatings
c Biocompatible materials
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33 36 39 42 45 48
^ ^
^
40 shots
30 shots
20 shots
10 shots
Unexposed
Intensity (arb. units)
Angle (2 )o
---- ZrN ---- Zr 2 N ---- Zr
33 36 39 42 45 48
^
^
20 degree
10 degree
0 degree
Unexposed
Intensity (arb. units)
Angle (2 )o
---- Zr ----ZrN ----Zr 3 N 4 ----Zr 2 N
XRD Analysis
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2.56 4.
6
3 1.
FWHM cos
k Crystallit e Size
λ = 1.54 Å k depends on particle shape, plane reflections etc and ranges from 0.85 to 0.
Residual stresses (compressive and tensile)
.
st
obs st
( ) d
d Stress E
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35
40
45
50
55
60
(a)
Crystallite size (nm) Peak intensity (arb. units)
Number of shots
Crystallite size, ZrN (200)
Peak intensity (arb. units)
Crystallite size (nm) 20
40
60
80
100
120
140
160
180
200 Peak intensity, ZrN (200)
10 15 20 25 30 35 40
10
20
30
40
50
60
70
80
90 Crystallite size, Zr 2 N (121)
(b)
80
100
120
140
160
Peak intensity, Zr 2 N (121) 180
Crystallite Size
and
Peak Intensity
vs
Focus Shots
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1 μm
100 nm
100 nm
(0)
(20)
(10)
100 nm
100 nm
100 nm
(0)
(10)
(20)
Surface Morphology
40 shots
Grain size ~ 50 nm
Grain size
~ 40 nm
10 shots
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Number of focus shots
Angular positions of the samples (degree)
Elemental concentrations
Oxygen Nitrogen
wt.% at. % wt.% at. %
Unexposed No 11 3 42 0 0
Elemental Concentrations
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0 1 2 3 4 5 6 7 8 9 10
1
2
3
4
5
6
7
Microhardness (GPa)
Indentation depth ( m)
Unexposed 0 o^ position 10 o^ position 20 o position
For 40 focus shots
Incorporation rate of nitrogen ions depends upon the nitrogen ion energy flux, which is highest at 0° angular position and decreases with increasing the sample angular positions.
Microhardness Analysis
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Results
1 Crystallinity of ZrN increases with increasing focus shots and decreases with increasing sample angular position.
2 Crystallite size of ZrN (200) and Zr2N (121) planes increases with increasing focus shots.
3 Residual stresses [compressive (~ 9.5 GPa) in ZrN (111) and (~ 1.5 GPa) in ZrN (200)) and tensile (~ 1 GPa) in Zr (101)] are observed in the deposited films.
4 Increasing growth behaviour of nitrides is responsible to decrease the stress level in the deposited films.
5 Tensile stress present in Zr has been transformed into compressive when the irradiated samples are displaced from zero to 20 degree angular positions.
6 Grain size increases with increasing focus shots and its distribution is homogeneous for 40 focus shots.
7 EDS results confirm the presence of nitrogen in the deposited films which increases with increasing focus shots and decreases with increasing sample angular positions.
8 Microhardness of the deposited films increases with increasing focus shots and it is 400 % greater for the film deposited for 40 focus shots.