Latest Results and Advancements with HIPIMS Coatings

G. Terenziani, S.Calatroni, A. P. Ehiasarian, T. Junginger

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

XRDRRROESMS

• HIPIMS Cavity Results

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

XRDRRROESMS

• HIPIMS Cavity Results

DC Magnetron Sputtering (DCMS)

DCMS FeaturesPros:

• High deposition rate

• Good film adherence to the substrate

Cons:

• Difficulty to coat complex geometry

• Columnar growth of the film

• Porosity of the film

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

XRDRRROESMS

• HIPIMS Cavity Results

From DCMS To HIPIMS

© Andre Anders, 2010 11

Generalized Structure Zone Diagram

A. Anders, Thin Solid Films 518, 4087 (2010).

derived from Thornton’s diagram, 1974

Based on “Structure Zone Model” - Thornton, J.Vac. Sci. Technol. 11 (1974) 666

From DCMS To HIPIMS

To enhance Ions production

Higher power

Higher Plasma density and higher cathode current

Overheating and possible melting of the cathode

HIPIMS (High Power Impulse Magnetron Sputtering)

HPIMS

Typical voltage and current trace from a high power pulsed magnetron discharge.

Example of a duty cycle.

HIPIMS – Characteristics

Pros:

• Smoother thin film surface

• Very good film adherence to the substrate

• Possibility to coat complex geometries

• Possibility of self-sputtering and resulting removal of defects and impurities

Cons:

• Low deposition rate

Outline• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

OESMSXRDRRR

• HIPIMS Cavity Results

HIPIMS Samples – Optical Emission Spectroscopy (OES)

50 88 125 165 180 270 340 410 480 550

21

37

53

69

85

Pulse Duration (µs)

Pea

k C

urre

nt (A

)

0.05000

0.1250

0.2000

0.2750

0.3500

0.4250

0.5000

0.5750

0.6500

Nb II / Nb I Ratio

HIPIMS Samples – Optical Emission Spectroscopy (OES)

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

OESMSXRDRRR

• HIPIMS Cavity Results

0 5 10

0.1

1

10

100

1000

10000

100000

1000000

1E7

Intensity Linear Fit of Sheet1 B

Inte

nsity

Energy

Equation y = a + b*x

Weight No Weighting

Residual Sum of Squares

0.02028

Pearson's r -0.99077

Adj. R-Square 0.97957Value Standard Error

IntensityIntercept 6.08974 0.01431Slope -0.99225 0.04526

0 10 20 30

0.01

0.1

1

10

100

1000

10000

100000

1000000

1E7

Inte

nsity

Energy

Intensity Linear Fit of Sheet1 B

Equation y = a + b*x

Weight No Weighting

Residual Sum of Squares

0.26334

Pearson's r -0.99737

Adj. R-Square 0.99471Value Standard Error

IntensityIntercept 5.37594 0.00808Slope -0.14611 9.00585E-4

0 20 40 60

0.1

1

10

100

1000

10000

100000

1000000

1E7

Inte

nsity

Energy

Intensity Linear Fit of Sheet1 B

Equation y = a + b*x

Weight No Weighting

Residual Sum of Squares

1.65281

Pearson's r -0.97238

Adj. R-Square 0.94526Value Standard Error

IntensityIntercept 4.16017 0.02843Slope -0.06511 0.00111

Low Energy zoneMedium Energy zone

High Energy zone

HIPIMS Samples – Mass Spectrometer (MS) – Nb+ case

HIPIMS Samples – Mass Spectrometer (MS) – Nb+ case

0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 2.2

-1.2

-1

-0.8

-0.6

-0.4

-0.2

0

Zone Slope Vs Peak Current Density

Zone ILinear (Zone I)Zone IILinear (Zone II)Zone IIILinear (Zone III)Sl

ope

0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 2.20.00E+00

2.00E+05

4.00E+05

6.00E+05

8.00E+05

1.00E+06

1.20E+06

IEDF Area Vs Peak Current Density

AreaLinear (Area)

Peak Current Density

IEDF

Are

a

HIPIMS Samples – Mass Spectrometer (MS) – Nb+ case

0 20 40 60 80 100 1201

10

100

1000

10000

100000

1000000

10000000Nb+ energy density function

NbI 0.55 A/cm2NbI 1.3 A/cm2NbI 2 A/cm2

Energy (eV)

Arbi

trar

y Un

itHIPIMS Samples – Mass

Spectrometer (MS) – Nb+ case

HIPIMS Samples – Mass Spectrometer (MS)

0 0.5 1 1.5 2 2.5 30.00E+00

2.00E+00

4.00E+00

6.00E+00

8.00E+00

1.00E+01

1.20E+01

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

IEDF Area and Nb+/Nb0 Ratio Vs Peak Current Density

AreaRatio I

Peak Current Density

IEDF

Are

a

Arbi

trar

y Un

it

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

OESMSXRDRRR

• HIPIMS Cavity Results

HIPIMS Samples – X-Ray Diffraction

Cu <200>

Cu <200>

Cu <200>

Nb <110>

Nb <110>

Nb <110>

HIPIMS Samples – X-Ray Diffraction

0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 2.20

2000

4000

6000

8000

10000

12000

Crystallographic Orientation Vs Peak Current Density

Cu <200> IntensityLinear (Cu <200> Intensity)Nb <110> IntensityLinear (Nb <110> Intensity)

Peak Current Density

Coun

ts

0 0.5 1 1.5 2 2.5 30

0.050.1

0.150.2

0.250.3

0.350.4

Nb+ and Nb0 vs Peak Current Density

Ratio ILinear (Ratio I)Ratio IILinear (Ratio II)

Peak Current Density

Coun

ts

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

OESMSXRDRRR

• HIPIMS Cavity Results

HIPIMS Samples – Residual Resistance Ratio (RRR)

0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 2.20

2000

4000

6000

8000

10000

12000

Crystallographic Orientation Vs Peak Current Density

Cu <200> IntensityLinear (Cu <200> Intensity)Nb <110> IntensityLinear (Nb <110> Intensity)

Peak Current Density

Coun

ts

40 60 80 100 120 140 160 180 200 2200

2

4

6

8

10

12

14

RRR Vs Peak Current

200 usLinear (200 us)

Peak Current

RRR

HIPIMS Samples – Residual Resistance Ratio (RRR)

40 60 80 100 120 140 160 180 200 2200

2

4

6

8

10

12

14

RRR Vs Peak Current

200

Peak Current

RRR

0 0.5 1 1.5 2 2.5 30

0.050.1

0.150.2

0.250.3

0.350.4

Nb+ and Nb0 vs Peak Current Density

Ratio ILinear (Ratio I)Ratio IILinear (Ratio II)

Peak Current Density

Coun

ts

Outline

• Dc Magnetron Sputtering – The Origins

• From Dc Magnetron Sputtering to HiPIMS

• HIPIMS Samples Analysis:

XRDRRROESMS

• HIPIMS Cavity Results

HIPIMS on 1.3 GHz Cavity – Deposition System

1.3 GHz Cavity

Magnet

Central Cathode

413 mm

HIPIMS on 1.3 GHz Cavity

Before coating After coating

HIPIMS on 1.3 GHz Cavity - Results

Thank you for your attention