impact of reactor design on plasma polymerization processes - an international round-robin study

Impact of Reactor Design on Plasma Polymerization Processes - An

International Round-Robin Study

J.D.Whittle, A.Michelmore, D.A.Steele, R.D.Short

AVS Tampa 2012 PsThA8

www.bdbiosciences.com/purecoat

www.myskin-info.com/

www.youtube.com/watch?v=Oe3St1GgoHQwww.hi-tec.com/infinity/uk/liquid-mountaineering/

www.liquipel.com

Biomaterials SurfacesA method for the deposition of controllable chemical gradients. J.D.Whittle, D.Barton, M.R.Alexander, R.D.Short. Chemical Communications pp1766-1767 (2003)

COOR Component of C1s region at 0.5mm intervals

Protocols

• Argon Plasma Treatment– 2 samples – spin-cast polystyrene– Treatment at 5W for 20 seconds at 2sccm argon

• Acrylic Acid plasma polymer deposition– 3 runs– 2 samples per run– All at 2sccm for 20 minutes, at 2, 5 and 20W continuous wave rf

power

Run Samples Process Gas Flow Rate Power Duration

1 2x PS film on glass coverslip Argon 2sccm 5W 30 seconds

2 3x Si wafer Acrylic Acid 2sccm 2W 20 mins



Responses

• Samples from 16 different reactors at 11 different labs

• Study requirements are fairly arbitrary and not well suited to some plasma set-ups – samples which did not meet the requirements are not used in the analysis- e.g. Some were unable to measure flow-rate

online for AA, so calculate post-plasma.

Reactor Types

Steel Barrel (2)• non-coaxial geometry• Internal Electrodes

Steel Cylinder (3)• Axial Symmetry• Internal Electrodes

Glass Barrel (7)• Substrates parallel to flow• External Electrodes• Band (5) or Coil (2) Electrodes

Glass Cylinder (2)• Substrates perpendicular to flow• Insulating walls, Internal Electrodes

Glass Cross-piece (2)• Substrates parallel to flow• External Coil electrodes

Argon Plasma Treatment

Operator variability

Add XPS and Deposition rate data here for the 6 runs in warwick. Plus quickie description.

Treatment Measure Average SD (n=6)

Argon Plasma O/C ratio 0.08 0.01

Acrylic Acid Plasma Polymerisation 2W

O/C ratio 0.38 0.02

%COOR 13.8 1.1Deposition Rate(nm/min) 0.96 0.16


O/C ratio 0.35 0.01

%COOR 12.3 0.7

Deposition Rate(nm/min) 1.17 0.17


O/C ratio 0.32 0.01

%COOR 9.5 0.4Deposition Rate (nm/min) 1.42 0.2


• Oxygen ranged from 6 - 15%• Nitrogen ranged from 0.1 – 2.4%• No correlation between incorporation of N and O

A B C D E F G H I J M N

• Oxygen ranged from 6 - 15%• Nitrogen ranged from 0.1 – 2.4%• No correlation between incorporation of N and O

• Oxygen ranged from 6 - 15%• Nitrogen ranged from 0.1 – 2.4%

B

GD

I

M


• No correlation between N and O incorporation• No correlation between reactor base pressure and N or O incorporation

Acrylic Acid DepositionComparison – Typical Low and High Power

Acrylic Acid Deposition

Processing Correlations

Conclusions

• W/F provides insufficient information for us to use it to compare treatments between systems

• Within-system variation is very low and processes can be very well controlled

• There appear to be no simple correlation between pressure, flow, power, residence time, number of molecules etc.

• For some reactors this exercise was outside the normal operating regime, which leads to non-representative treatments

• We would like to add more data points – [email protected]

Future Work

• Trying to link internal measures with outcome• Example: Ion flux (Andrew Michelmore presented earlier

in week)

Acknowledgements

Prof. Hynek Biederman, Dr. Anton Serov, Charles University, Prague, CZ.

Dr. Francois Rossi, Dr. Giacomo Ceccone, Dr. Jan Hanus, European Commission Joint Research Centre, IT.

Prof. Renate Förch, Dr. Juan-Carlos Ruiz, Max Plank Institute for Polymer Research, Mainz, DE

Prof. Gary Kinsel, Kristopher Kirmess, Stephanie Eastwood, Southern Illinois University, US

Prof. Sally McArthur, Dr. Thomas Ameringer, Swinburne University of Technology, AU

Dr. Dirk Hegemann, Dr Enrico Körner, Swiss Federal Laboratory for Materials Testing, CH

Prof. Morgan Alexander, Dr. Andrew Hook, University of Nottingham, UK

Prof. James Bradley, Dr. Faiq Jan, University of Liverpool, UK

Prof. David Castner, Dr. Winston Ciridon, University of Washington, Seattle, US

Dr. Toby Jenkins, Dr. David Jamieson, University of Bath, UK.

Dr. Sue Low, Dr. Karyn Jarvis, Dr. Louise Smith, Dr. David Robinson, Carla Daunton, Agnieska Zuber, Emily Mitchell, Shima, Taheri, Akash Bachhuka, Mawson Institute, University of South Australia, AU

impact of reactor design on plasma polymerization processes - an international round-robin study

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