Plasma Focus Device: Deposition of Zirconium Nitride Films and Characterization, Slides of Materials Processing

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"In the name of Allah, most Gracious, most Compassionate"

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LAYOUT

1 Introduction

2 Motivation

3 Experimental Setup

4 Diagnostics Techniques for Plasma

5 Characterization of Ion Beams

6 Ion implantation & Deposition of Composite Films

8 Conclusions

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MOTIVATION

PF device is being used to deposit

1 Hard

2 Protective

3 Decorative Coatings

ON

Machine tool,

Cutting tools,

Turbine blades

and

Different substrates

For decorative purpose

Pens

Jewelry

Watches

Surgical tools

Artificial implants

To improve the surface

properties of the

materials

Such as

1 Crystal Structure

2 Residual Stresses

3 Crystallite Size

4 Crystal Growth

5 Crystallinity

6 Surface Morphology

7 Microhardness

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Desired surface properties of the deposited films

1 Number of focus shots

2 Sample axial positions

3 Sample angular positions

4 Insert materials

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Wilson Seal

ChamberVacuum

SampleHolder

Shutter

Cathode

Anode

Trigger

S

HV

C

InsulatorSleeve

Vacuumpump Gas Inlet

Guage

Samples

High densities (10^25 – 1026 ) m-

High temperature (1 – 2 ) KeV

Small time ~ 10-7^ sec.

HV 32 F

12 kV

Arrangement and Operation of PF

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Plasma Diagnostic Techniques & Ion Beam Analysis

1 High Voltage Probe

2 BPX65 Photodiode

Detector

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

40 keV to 1.2 MeV

d

V N RqAv



9.7×10^19 to 1.796×10^19 m-

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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.

• Zirconium nitride films are being used to deposit

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

I.A. Khan, et al. Thin Solid Films, 516 (2008) 8255

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 d

d

d

Strain 

( ) d

d Stress E

  

I.A. Khan, et al. Thin Solid Films, 516 (2008) 8255

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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

I.A. Khan, et al. Thin Solid Films, 516 (2008) 8255

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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

I.A. Khan, et al. Thin Solid Films, 516 (2008) 8255

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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.

I.A. Khan, et al. Thin Solid Films, 516 (2008) 8255

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.