1
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 (SiO 2 /Si/SiO 2 ) having thicknesses 286/571/143nm were deposited by RF magnetron sputtering deposition technique on 0.5mm thick Si(100)-substrates. Post-deposition annealing is also carried out in the temperature range 150-650 0 C for 4hr at the rate of 10 0 C/min. Si Optical window was designed at 4.2μm wavelengths and correlated with modeling software TFCAL. The films are transparent in the 35μm band of the electromagnetic spectrum, firmly adhered to the substrate. The prepared multilayer thin films are characterized optically and structurally using UV/VIS/IR spectrophotometer, Atomic Force Microscopy (AFM), X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive Microscopy (EDS). . Antireflection (AR) coating has significant role on optical and electro-optical applications[1]. This work was designed at 4.2μm wavelength, prepared and DESIGN OF Si/SiO 2 THIN FILMS The hybrid antireflective coating model was designed using thin film design TFCALC software. SiO 2 was used as the low index material, while high index material was Si Refractive indices were calculated by Sellmeiers dispersion equation. n 2 - 1 = A 1 λ 2 / (λ 2 -C 1 2 ) + A 2 λ 2 / (λ 2 -C 2 2 ) + A 3 λ 2 / (λ 2 -C 3 2 ), [C 1 , C 2 , C 3 and λ] = [μm] (3) S.No. Material A 1 A 2 A 3 C 1 (μm) C 2 (μm) C 3 (μm) 1 SiO 2 0.696166 0.407943 0.897480 0.068404 0.116241 9.89616 2 Si 10.668429 0.00304347 1.5413341 0.30151648 1.1347511 1104.0 Before Annealing 1µm Before Annealing K. Iqbal*, A. Maqsood, M. Mujahid and M. H. Asghar School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), Sector H-12, Islamabad, Pakistan E-mail Address: [email protected] INTRODUCTION 1.05 FC= 0.39 Parametric values of Sellmeier equation Si (100) 650 0 C 550 0 C 450 0 C 350 0 C 250 0 C 150 0 C As-deposited MATERIALS AND METHODS RESULTS 1. Structural identification Atomic compositions were computed with the help of ZAF method. designed at 4.2μm wavelength, prepared and characterized for non-quarter-wave thick multilayer AR coatings based on low-high refractive indexes in the 3–5μm bands and total thickness was determined by Fresnel equations. At 4.2μm wavelength, mainly carbon dioxide takes part in reducing the %transmittance [2]. n 2 AR = n s ×n air (1) d = λ 0 / (4 n AR ) (2) S.No Material Deposition rate (Å/sec) Argon flow rate (sccm) Oxygen flow rate (sccm) 1 SiO 2 1.1 190 21 2 Si 1.5 130 - The crystal structure was determined and lattice parameters a = 5.44 Å of the samples were calculated by using Bragg’s equation. Satellite peaks (or doublet or rocking curves) near at 69 0 degree shows unstrained from top layer to Si substrate. Sin 2 θ / (h 2 +k 2 +l 2 )=λ 2 / 4a 2 (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 Counts OKa SiKa 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 OKa SiKa Sample : 650 0 C Acc. Voltage : 10.0 kV Probe Current : 1.0 nA Sputtering system Sputtering System RF magnetron Sputtering Target Materials Si / SiO 2 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 SiO2/Si/SiO2 Layer Material Physical thickness (nm) 1 SiO 2 143 2 Si 571 3 SiO 2 286 Deposition rate, Argon flow rate and Oxygen flow rate for the individual layers Refractive indices of SiO2 & Si in the 3-5μm wave band Transmittance (%) vs Wavelength (μm) profile of Si/SiO2 layers Si/O ratio of the surface of Multi-layer Thin Films EDS analysis of As-deposited and 650 0 C sample 1 µm 0.5µm 1 µm SiO2 Si SiO2 Si substrate CONCLUSIONS 2. Film surfaces and roughness Films have columnar structure and the surface of the film is smooth and featureless. 3. Spectral distribution of Si/SiO2 coatings transmittance An Average transmission of Si/SiO 2 coatings is achieved 75% in the 3-5μm wave bands. 0 5 10 15 20 25 RMS Roughness (nm) Sample As-deposited T1 = 150 C T2 = 250 C T3 = 350 C T4 = 450 C T5 = 550 C T6 = 650 C Multilayer thinfilms of Si and SiO 2 are successfully prepared by RF magnetron sputtering. Annealed at 650 0 C generates smooth films as well as enhanced optical properties. The resulting models were helpful for determining the errors in deposition processes 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 assistance offered by greatly acknowledged: A. A. Khan M. Islam ACKNOWLEDGEMENTS Annealing of Samples Temperatures 1 50 - 650 0 C Time 4 hr Rate 10 0 C Technique Model Scanning Electron Microscope (SEM) / Energy Dispersive Microscopy (EDS) JSM-6490A, Joel X- Ray Diffraction (XRD) Siemens / Bruker D 8 Conditions Tube Voltage 40 kV Tube Current 40 mA Wavelength CuKα 0.154178 nm Step 0.04 Scan Speed 1°/ min AFM JSPM5200, Jeol Conditions Cantilever tip Si 3 N 4 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 between intensity and angle 2θ RMS roughness of the as-deposited and annealed samples Three-dimensional AFM image of the as-deposited and 650 0 C sample Typical SEM image of cross-sectional morphologies of 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 CO 2

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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