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AVS 56 th International Symposium & Exhibition November 9, 2009 San Jose, California a Department of Materials Science and Engineering b Department of Nuclear, Plasma, and Radiological Engineering Contact: [email protected] Time-resolved plasma characterization in modulated pulse plasma (MPP) magnetron sputtering A.N. Cloud a , R.E. Flauta b , M.J. Neumann b , S.L. Rohde b , and D.N. Ruzic b

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Page 1: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

a Department of Materials Science and Engineeringb Department of Nuclear, Plasma, and Radiological Engineering

Contact: [email protected]

Time-resolved plasma characterization in modulated pulse plasma (MPP)

magnetron sputtering

A.N. Clouda, R.E. Flautab, M.J. Neumannb, S.L. Rohdeb, and D.N. Ruzicb

Page 2: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Overview

• Introduction and motivation

• Experimental apparatus and diagnostics

• Vacuum system and magnetron

• Triple Langmuir probe

• Gridded energy analyzer (GEA)

• Quartz crystal microbalance (QCM)

• Results

• Time-resolved electron temperature and density

• Growth rate dependence on plateau current and repetition rate

• Time-resolved ion current at the substrate level

• Conclusions

2

Page 3: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Introduction and motivation

3

Page 4: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Modulated Pulse Plasma (MPP)

• Relatively new method of applying the basic principles of HPPMS / HIPIMS

• Allows the generation of an arbitrary voltage waveform

• Most studies of discharges produced by this technology have been inherently time-averaged.• Time-averaged plasma diagnostics• Film properties

• In order to intelligently apply this technology and create improvement, the underlying physics must be understood.

• We are conducting time-resolved diagnostics of this interesting type of discharge.

4

Page 5: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Multi-step power delivery of MPP

• Step 1 – Ignition• Step 2 – Low power (DC-like) discharge• Step 3 – Current ramp• Step 4 – High power discharge

5

Voltage

Current

Power

Page 6: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Experimental apparatus and diagnostics

6

Page 7: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Magnetron sputtering tool 7

MRC Galaxy

• Planar circular rotating magnetron

• Designed for 20kW DC sputtering

14” (36 cm) diameter sputtering

targets

• 1000 cm2

• <150 W/cm2 power density

Page 8: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Triple probe theory and setup8

From T.K. Gray

• Probe 2 is allowed to float in the plasma.

• Probes 1 and 3 are biased using a floating voltage source.

Probe 1 is held above floating potential while probe 3 is held

below Vf. While ΔV13 remains constant, the exact values for V1

and V3 are dependant on the need to satisfy Kirchhoff’s current

law.

• Determining electron temperature (t):

• To determine the electron density (t), the following

relation is solved for ne:

•Assumptions:

• Maxwellian electron energy distribution function

• Collisionless thin sheath

• No interaction between probe tips

From S. Chen and T. Sekiguchi.

Instantaneous direct-display system of

plasma parameters by means of triple probe.

J. Appl. Phys., 26(8):2363{2375, 1965.

Probe tips

Page 9: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Gridded energy analyzer

• Gridded Energy Analyzer

• Custom built at CPMI

• Can be used as an ion collector and ion energy discriminator

• Schematic:

• Quartz crystal microbalance

• Used to determine deposition rate

• Also can be used in conjunction with the GEA to determine ionization fraction

• Previous work at CPMI has shown ~6% metal ionization at the substrate level in this sputtering tool.

9

Range of voltage to measure energy

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AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Results

10

Page 11: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

0.00E+00

5.00E+10

1.00E+11

1.50E+11

2.00E+11

2.50E+11

3.00E+11

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

ne (

eV

)

0

5

10

15

20

25

30

35

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

kTe

(eV

)

Triple probe results (1)11

• Pressure: 2 mTorr

• Distance from target:~12.5 cm (far)

• Plateau “temperature” is ~20 eV.

• Peak density is 0.9 x 1011 cm-3

.

• Density tracks Z-pulser current on target.

• High energy electrons are present, likely responsible for ionizing the metal atoms.

Voltage

Current

Power

Electron “Temp.”

Electron Density

Page 12: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

-5.00E+10

0.00E+00

5.00E+10

1.00E+11

1.50E+11

2.00E+11

2.50E+11

3.00E+11

3.50E+11

4.00E+11

4.50E+11

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

n e (c

m-3

)

0

5

10

15

20

25

30

35

40

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

kTe

(eV

)

Triple probe results (2)12

• Pressure: 2 mTorr

• Distance from target:~6.3 cm (near)

• Plateau “temperature” is ~20 eV.

• Peak density is 1.4 x 1011 cm-3

.

• Density is higher near the target as expected.

Voltage

Current

Power

Electron “Temp.”

Electron Density

Page 13: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

-5.00E+10

0.00E+00

5.00E+10

1.00E+11

1.50E+11

2.00E+11

2.50E+11

3.00E+11

3.50E+11

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

n e (c

m-3

)

Triple probe results (3)13

• Pressure: 30 mTorr

• Distance from target:~12.5 cm (far)

• Plateau “temperature” is ~24 eV.

• Peak density is 1.3 x 1011 cm-3.

• Higher pressure of process gas leads to higher density as expected (compared to the density at same distance, lower pressure).

Voltage

Current

Power

Electron “Temp.”

Electron Density

0

5

10

15

20

25

30

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

kTe

(eV

)

Page 14: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

0.00E+00

1.00E+11

2.00E+11

3.00E+11

4.00E+11

5.00E+11

6.00E+11

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

n e (c

m-3

)

0

5

10

15

20

25

30

35

40

45

50

-0.0014 -0.0012 -0.001 -0.0008 -0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006

t (s)

kT

e (

eV

)

Triple probe results (4)14

• Pressure: 30 mTorr

• Distance from target:~6.3 cm (near)

• Plateau “temperature” ~22 eV.

• Peak density is 1.6 x 1011 cm-3.

• Again, density is slightly higher near the target.

Voltage

Current

Power

Electron “Temp.”

Electron Density

Page 15: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Growth rate behavior• Lower pressure

gives higher deposition rate.

• Deposition rate not proportional to current plateau value

• Deposition rate not constant with power

15

Deposition rate versus time as deposition conditions are altered.

Pressure (mTorr)

Peak Current (A)

Deposition Rate (Å/s)

30 230 1.86

2 160 3.92

2 125 4.52

2 40 5.13

Pressure (mTorr)

Peak Current (A)

Deposition Rate (Å/s)

2 172 2.55

2 135 2.20

2 122 2.02

2 54 1.60

Constant average power (2.0 kW)Constant repetition rate (39 ±1 Hz)

Page 16: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Time-resolved ion current at the substrate

• When do the ions arrive at the substrate?

• At 2mTorr, 160A plateau current:

• Note that these are not necessarily metal ions; most likely Ar+.

16

-0.2

-0.15

-0.1

-0.05

0

0.05

0.1

0.15

0.2

0.25

0.3

-0.0015 -0.001 -0.0005 0 0.0005 0.001 0.0015 0.002

t (s)

Ion

Curr

ent (

mA)

Ion current follows the shape of

plasma density curves found

with triple probe.

Voltage

Current

Power

ion current to grid

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AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Energy of time resolved ion current17

-0.4

-0.3

-0.2

-0.1

0

0.1

0.2

0.3

0.4

-6 -5 -4 -3 -2 -1 0 1 2 3

Stopping potential (V)

Cu

rren

t (m

A)

2 mTorr

30 mTorr

At 30 mTorr ions have less than 1 eV

of energy at substrate.

At 2 mTorr ions have less than 3 eV

of energy at substrate.

Page 18: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Conclusions

• The plasma is very hot during the pulse.

• 20 eV and greater.

• Likely a non-Maxwellian electron energy distribution

• Density is on the order of 2 x 1011 cm-3 and follows input current.

• Density increases with pressure and falls off with distance from target.

• Deposition rates are not strictly a function of power or plateau current.

• Energy of ions reaching substrate is very low (< 3eV), though we are not measuring metal ions at this point.

18

Page 19: Time-resolved plasma characterization in modulated pulse ...zpulser.com/assets/2012/01/AN-Cloud-et-al-AVS-2009.pdf•Quartz crystal microbalance •Used to determine deposition rate

AVS 56th International Symposium & ExhibitionNovember 9, 2009 San Jose, California

Thank you for your attention.

Andrew N. CloudPhD candidate, Department of Materials Science and Engineering

University of Illinois at Urbana-Champaign

Acknowledgements:

19

Graduate student support provided by the National Defense Science and Engineering Graduate research fellowship program (NDSEG).

This research was funded in part by a grant from the National Science Foundation, under Grant #CMMI09-53057.