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CHARACTERIZATION AND PREPARATION OF ANTI- REFLECTION COATINGS IN THE

RANGE OF 3-5 µm FOR Si OPTICAL WINDOW

ABSTRACT

Thin film multilayer anti-reflection coatings (SiO2/Si/SiO2)having thicknesses 286/571/143nm were deposited byRF magnetron sputtering deposition technique on 0.5mmthick Si(100)-substrates. Post-deposition annealing isalso carried out in the temperature range 150-6500C for4hr at the rate of 100C/min. Si Optical window wasdesigned at 4.2µm wavelengths and correlated withmodeling software TFCAL. The films are transparent inthe 3‐5µm band of the electromagnetic spectrum, firmlyadhered to the substrate. The prepared multilayer thinfilms are characterized optically and structurally usingUV/VIS/IR spectrophotometer, Atomic Force Microscopy(AFM), X-Ray Diffraction (XRD), Scanning ElectronMicroscopy (SEM) and Energy Dispersive Microscopy(EDS)..

Antireflection (AR) coating has significant role on opticaland electro-optical applications[1]. This work wasdesigned at 4.2µm wavelength, prepared and

DESIGN OF Si/SiO2 THIN FILMS

■ The hybrid antireflective coating model was designed using thin film design TFCALC software.

■ SiO2 was used as the low index material, while high index material was Si

■ Refractive indices were calculated by Sellmeiers dispersion equation.

n2 - 1 = A1λ2 / (λ2-C1

2) + A2λ2/ (λ2-C2

2) + A3λ2/ (λ2-C3

2), [C1, C2, C3 and λ] = [µm] (3)

S.No. Material A1 A2 A3 C1

(µm)

C2

(µm)

C3

(µm)1 SiO2 0.696166 0.407943 0.897480 0.068404 0.116241 9.896162 Si 10.668429 0.00304347 1.5413341 0.30151648 1.1347511 1104.0

Before Annealing 1µmBefore Annealing

K. Iqbal*, A. Maqsood, M. Mujahid and M. H. AsgharSchool of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), Sector H-12,

Islamabad, PakistanE-mail Address: [email protected]

INTRODUCTION

1.05

FC= 0.39

Parametric values of Sellmeier equation

Si (100)6500C

5500C

4500C

3500C

2500C

1500C

As-deposited

MATERIALS AND METHODS RESULTS

1. Structural identification

■ Atomic compositions were computed withthe help of ZAF method.

designed at 4.2µm wavelength, prepared andcharacterized for non-quarter-wave thick multilayer ARcoatings based on low-high refractive indexes in the3–5µm bands and total thickness was determined byFresnel equations. At 4.2µm wavelength, mainly carbondioxide takes part in reducing the %transmittance [2].

n2AR = ns×nair (1)

d = λ0 / (4 nAR ) (2)

S.No Material Deposition rate (Å/sec)

Argon flow rate (sccm)

Oxygen flow rate (sccm)

1 SiO2 1.1 190 212 Si 1.5 130 -

■ The crystal structure was determined andlattice parameters a = 5.44 Å of the sampleswere calculated by using Bragg’s equation.

■ Satellite peaks (or doublet or rocking curves)near at 690 degree shows unstrained from toplayer to Si substrate.

Sin 2θ / (h2 + k2 + l2) = λ2 / 4a2 (4)As- deposited

200X

200X

Before Annealing

Annealing at 650 0C

0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00

keV

0

100

200

300

400

500

600

700

800

900

1000

Cou

nts

OK

a

SiK

a

Sample : As-deposited

Acc. Voltage : 10.0 kV

Probe Current : 1.0 nA

0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00

keV

0

100

200

300

400

500

600

700

800

900

1000

OK

a

SiK

a

Sample : 650 0C

Acc. Voltage : 10.0kV

Probe Current : 1.0 nA

Sputtering system

Sputtering System RF magnetron Sputtering

Target Materials Si / SiO2

Target Size 4 inch

Forward Power 2.74 kW

Reflected Power 0.16 kW

Chamber Pressure 5.0 × 10-4 Pa

Characterization Techniques

Structural and Optical Analysis by following techniques:

Physical thickness SiO 2/Si/SiO2

Layer Material Physical thickness (nm)

1 SiO2 143

2 Si 571

3 SiO2 286

Deposition rate, Argon flow rate and Oxygen flow ra te for the individual layers

Refractive indices of SiO 2 & Si in the 3-5µm wave band Transmittance (%) vs Wavelength (µm) profile of Si/S iO2 layers

Si/O ratio of the surface of Multi-layer Thin Films

EDS analysis of As-deposited and 650 0C sample

1 µm

0.5µm1 µm

SiO2

Si

SiO2

Si substrate

CONCLUSIONS

2. Film surfaces and roughness

■ Films have columnar structure and the surface ofthe film is smooth and featureless.

3. Spectral distribution of Si/SiO2 coatings transmittance

■An Average transmission of Si/SiO2 coatings isachieved 75% in the 3-5µm wave bands.

0

5

10

15

20

25

RM

S R

ough

ness

(nm

)

Sample

As-deposited

T1 = 150 C

T2 = 250 C

T3 = 350 C

T4 = 450 C

T5 = 550 C

T6 = 650 C

Multilayer thin‐films of Si and SiO2 are successfully prepared by RF magnetronsputtering. Annealed at 6500C generates smooth films as well as enhanced opticalproperties. The resulting models were helpful for determining the errors in depositionprocesses of each of the utilized deposition techniques, and this was the main goal.

REFERENCES

[1] M. H. Asghar, M. Shoaib, F. Placido and S.Naseem, Cent. Eur. J. Phys., Vol. 6, No. 4,2008, pp. 853 - 863.[2] M. H. Asghar, M. B. Khan, and S. Naseem,Semiconductor Phys: Quan. Elect. & Optoelect.,Vol. 6, No. 4, 2003, pp. 508- 513.

This project was funded by NUST and the assistanceoffered by greatly acknowledged:■ A. A. Khan ■ M. Islam

ACKNOWLEDGEMENTS

Annealing of Samples

Temperatures 1 50 - 650 0C

Time 4 hr

Rate 10 0C

Technique ModelScanning Electron Microscope

(SEM) /Energy Dispersive Microscopy

(EDS)

JSM-6490A, Joel

X- Ray Diffraction(XRD)

Siemens / Bruker D 8

ConditionsTube Voltage 40 kV

Tube Current 40 mA

Wavelength CuKα 0.154178 nm

Step 0.04

Scan Speed 1°/ min

AFM JSPM5200, Jeol

ConditionsCantilever tip Si3N4

Operation Mode AC

Cantilever Frequency 174.161 kHz

Force Constant 1.00 N / m

Scan Speed 1°/ min

UV/VIS/IR Spectrometer U-3501, Hitachi

NANOPAPRIKA POSTER 2011

XRD analysis of As-deposited and annealed samples b etween intensity and angle 2 θ

RMS roughness of the as-deposited and annealed samp les

Three-dimensional AFM image of the as-deposited an d 650 0C sample

Typical SEM image of cross-sectional morphologies o f the as-deposited sample and surface of the as-deposited and 650 0C sample

Measured transmission spectra for the as-deposited and annealed samples

Si substrate

CO2

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