Hanna skliarova porosity of nb magnetron sputtered thin films and dependence on sputtering...

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description

Pinholes (or through film porosity) in Nb thin film deposited on the inner walls of SRF cavities are harmful for cavity performance because they may expose inferior copper that has much higher resistance than niobium at 4.2 K. Aluminated quartz substrates allowed us to make visible the pore sites for inspection and counting by production visible corrosion products. We showed the correlation between the amount of pinholes in niobium thin film prepared by magnetron sputtering and the deposition parameters, such as sputtering gas pressure, substrate temperature, applied bias, placing of the sample in UBM sputtering mode. Thus low temperature of the substrate and high sputtering gas pressure promoted growth of a voided film (that corresponds to SZM approach) with high amount of pinholes. Heating of the substrate during deposition has resulted in moderate decrease of the pinhole amount, while negative bias applied to the substrate showed stronger decrease of the pinhole amount thanks to additional bombardment of the substrate by Ar+ serving to remove weakly bounded particles during deposition.

transcript

1

of Nb magnetron sputtered

thin films and dependence on sputtering parameters

Anna Skliarova, O. Azzolini, V. Palmieri

Porosity

2

Pinholes in Nb film in SRF cavities

Resistance

to RF at

4.2K

RCu≈105RNb

Pinholes

expose

underlying

Cu

Cavity

surface

resistance

increase

Q-factor

EAcc

are lower

• To correlate Nb film porosity vs

sputtering parameters

• To find approaches to less porous Nb

films

3

Aim of the research:

4S. Amorosi, C. Benvenuti, P. Chiggiato, M. Malabaila, Vacuum, V. 60, 1–2, 2001, 275-278

Method proposed by Amorosi et al.

5

Our method of porosity evaluation

Al is providing fast reaction with

visible product revealing the pore sites

6

Our method of porosity evaluation

Sputtering of Al onto polished quartz allowed

minimizing the influence of the substrate defects

and focus on sputtering parameters

7

Our method of porosity evaluation

8

1 2 3 4 5

Acid test evaluation: SCALE

9

Standard conditions

- conditions to be considered standard if other

information is not provided below

10

Standard conditions:

2” Planar UBM II type

STANDARD SAMPLE POSITION

11

Standard conditions:

SAMPLE HOLDER

6 cm

12

Standard conditions:

Ar as sputtering gas

Nb target RRR 300

Pbase ~10-6 mbar

IDC = 0.5 A

No heating/cooling substrate

Film thickness ~1.5 µm

13

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

14

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

15

Magnetron position: acid test

MAGNETRON

MAGNETRON

SAMPLE HOLDER

Standard

16

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

17

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

18

Pressure influence: acid porosity test

310-2

mbar310-3

mbar

19

Pressure influence: acid porosity test

310-2

mbar310-3

mbar

20

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

21

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

44

44

33

3

22

Temperature influence: acid test

Floating (~250°C)

400°C

500°C

0°C

-100°C

-50°C

300°C

Standard

44

44

33

3

23

Temperature influence: acid test

Floating (~250°C)

400°C

500°C

0°C

-100°C

-50°C

300°C

Standard

24

Optical profilometry

Scan area: 200 μm × 200 μm

Result: % of area covered by

holes deeper than 0.5 μm

25

4 0.5 %

-100 °C

4 0.4 %

0 °C

4 1 %

Floating

3 0.04 %

500 °C

- 0 %

800 °C

Temperature influence: SEM

Acid test (1÷5)

Optical profilometry

(%)

26

4 0.5 %

-100 °C

4 0.4 %

0 °C

4 1 %

Floating

3 0.04 %

500 °C

- 0 %

800 °C

Temperature influence: FIB SEM

27

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

28

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

29

Influence of film thickness: acid test

43

22

28 µm

6 µm

1.5 µm

4 µm

10 µmStandard

30

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

31

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

32

UBM II type: sample position

33

UBM II type: sample position

ON AXIS OUT OF AXIS

34

UBM II type: sample position

ON AXIS OUT OF AXIS

1 5Acid porosity test :

35

1

ON AXIS

5

OUT OF AXIS

UBM II type: position influence

Acid test (1÷5)

36

1

ON AXIS

5

OUT OF AXIS

UBM II type: position influence

37

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

38

Investigated parameters:

• Magnetron position1

• Pressure2

• Temperature3

• Film thickness4

• Sample position 5

• DC-Biased MS6

DC bias -80 V -50 V -80 V -80 V -150 V

Arpressure,

mbar310-2 510-3 510-2 310-3 310-3

Porosity acid test 3 2 1 1 2

39

DC-biased MS

DC bias -80 V -50 V -80 V -80 V -150 V

Arpressure,

mbar310-2 510-3 510-2 310-3 310-3

Porosity acid test 3 2 1 1 2

40

DC-biased MS

DC bias -80 V -50 V -80 V -80 V -150 V

Arpressure,

mbar310-2 510-3 510-2 310-3 310-3

Porosity acid test 3 2 1 1 2

41

DC-biased MS

Amount of holes deeper 0.5 μm is 0.1 %

42

DC-biased MS

SEM HR SEM

FIB SEM

43

Winners!

132

44

Winners!

132

Biased MS

45

Winners!

132

Biased MSHigh T MS

46

Winners!

132

Biased MSHigh T MS

Thick film

• Increase film thickness1

• Substrate above magnetron2

• Proper substrate preparation3

• Avoiding UBM far out of axis4

• Clean room + vacuum cleaner5

47

Methods to decrease porosity:

47

48

Research team:

LNL INFN:

H.Skliarova, O. Azzolini, V. Palmieri

Hanna.Skliarova@lnl.infn.it

LIME Roma-Tre:

M. Renzelli, D. De Felicis, E. Bemporad