MULTISCALE SIMULATION OF FUNCTIONALIZATION OF SURFACES USING ATMOSPHERIC PRESSURE DISCHARGES * Ananth N. Bhoj a) and Mark J. Kushner b) a) Department of.

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MULTISCALE SIMULATION OF FUNCTIONALIZATION OF SURFACES USING ATMOSPHERIC PRESSURE DISCHARGES * Ananth N. Bhoj a) and Mark J. Kushner b) a) Department of Chemical and Biomolecular Engineering University of Illinois, Urbana, IL b) Department of Electrical and Computer Engineering Iowa State University, Ames, IA nd IEEE International Conference on Plasma Science, 18 th – 23 rd June 2005, Monterey, CA. *Work supported by the NSF.

Iowa State University Optical and Discharge Physics OUTLINE ICOPS05_agenda  Functionalization of Surfaces using Plasmas  Modeling Platform  Pulsed Coronas in Humid Air, He/O 2 /H 2 O mixtures  Uniformity of surface treatment  O 2 fraction  Discharge Polarity  Surface microstructure  Concluding remarks

Iowa State University Optical and Discharge Physics FUNCTIONALIZATION OF SURFACES USING PLASMAS ANANTH_ICOPS05_01  Functionalization of surfaces occurs by their interaction with plasma species - ions, radicals, and photons. For hydrocarbon polymer:  Surface groups created in an O 2 containing plasma include  Acids –C(OH)=O  Carbonyl -C=O  Alkoxy –C-O  Peroxy –C-O-O  Alcohols –C-OH

Iowa State University Optical and Discharge Physics SURFACE MODIFICATION OF POLYMERS ANANTH_ICOPS05_02  Functionalization increases surface energy and enhances wettability and adhesion.  Akishev, et al, Plasmas Polym., 7, 261 (2002).  Pulsed atmospheric discharges (coronas) are widely used in industry to treat commodity polymers like polypropylene (PP).  Tantec, Inc.  PE Film

Iowa State University Optical and Discharge Physics TREATMENT OF NON-PLANAR SURFACES ANANTH_ICOPS05_03  Penetration of plasma species into surface features determines the extent and uniformity of functionalization.  SEM of polyester fabric (Borcia, et al, Plasma Sources Sci. Technol, 12, 235 (2003).  Roughness of surface to be treated may range from 100s nm to few µm.  M. Strobel, 3M Untreated PP Plasma Treated PP

Iowa State University Optical and Discharge Physics SCHEMATIC OF THE 2-D MODELING PLATFORM ANANTH_ICOPS05_04  Unstructured mesh  Plasma hydro- dynamics (multi-fluid, Poisson’s equation)  Radiation transport  Integrated plasma- surface kinetics model

Iowa State University Optical and Discharge Physics DBD TREATMENT OF PP SURFACE WITH MICROSTRUCTURE ANANTH_ICOPS05_05  Corona treating a polymer on the grounded electrode acts as a DBD.  Gas mixtures  He/O 2 /H 2 O  Humid air - N 2 /O 2 /H 2 O  How does uniformity of treatment vary over microscopic and macroscopic scales when repetitively pulsed?  PRF – 10 kHz

MIN MAX Iowa State University Optical and Discharge Physics PLASMA PROPERTIES IN He/O 2 /H 2 O MIXTURES  - 5 kV, 760 Torr He/O 2 /H 2 O=98/1/1, 0 – 2.5 ns ANANTH_ICOPS05_06 Potential (V)T e (eV) [Positive Ions] cm - 3 [O] cm – 0 0 – – – ANIMATION SLIDE

Iowa State University Optical and Discharge Physics PLASMA PENETRATION INTO SURFACE FEATURES ANANTH_ICOPS05_07  - 5 kV, 760 Torr, He/O 2 /H 2 O=98/1/1 [e] cm - 3 t = 2.5 nst = 5 ns t = 2.5 ns t = 5 ns [O] cm - 3 t = 2.5 ns t = 5 ns [Positive ions] cm - 3 MIN MAX – – – 10 13

Iowa State University Optical and Discharge Physics  At higher O 2 fraction, the density of reactive [O] radicals at the surface increases during the pulse. ANANTH_ICOPS05_08  - 5 kV, 760 Torr (log scale) [O] cm - 3 EFFECT OF O 2 FRACTION ON [O] DENSITY He/O 2 /H 2 O = 98 / 1 / 1 He/O 2 /H 2 O = 69 / 30 / 1 t = 5 ns 2x10 11 t = 3 ns 2x10 14 He/O 2 /H 2 O = 89 / 10 / 1 t = 3 ns

ANANTH_ICOPS05_09 Iowa State University Optical and Discharge Physics SURFACE REACTION MECHANISM FOR PP  Gas phase radicals abstract H from the surface and produce radical sites on the PP surface. 1 R. Dorai and M.J.Kushner, J. Phys. D 36, 666 (2003).  Further reactions lead to formation of functional groups like peroxy, alkoxy, alcohols and other groups 1.

Iowa State University Optical and Discharge Physics DENSITY OF SURFACE RADICALS ANANTH_ICOPS05_10  - 5 kV, 760 Torr, 10 kHz, He/O 2 /H 2 O=98/1/1  ALKYL (PP  ) are formed by O + PP  PP  + OH  Nonuniformities result from both fluxes and shadowing.  ALKOXY (PP-O  ) O 3 + PP   PP-O  O + PP   PP-O  take longer to form but eventually dominate.

Iowa State University Optical and Discharge Physics DENSITY OF -OH FUNCTIONAL GROUPS ANANTH_ICOPS05_11  - 5 kV, 760 Torr, He/O 2 /H 2 O=98/1/1, 10 kHz  Non-uniformities occur on the macroscopic and microscopic (< 1 µm) length scales; and are site dependent

Iowa State University Optical and Discharge Physics TEMPORAL VARIATION OF FLUXES WITH O 2 FRACTION ANANTH_ICOPS05_13  Larger fraction of reactive [O] is lost in the interpulse period at higher O 2 fraction by three-body recombination and ozone formation.  Optimum composition is at O 2 = 10% with significant [O] flux maintained through the long interpulse period.  At position along surface: 0.05 cm, He/O 2 /H 2 O=99-x/x/1  IP - interpulse period (duration – 100  s at 10 kHz) IP END IP START

Iowa State University Optical and Discharge Physics SPATIAL VARIATION OF FLUXES WITH O 2 FRACTION ANANTH_ICOPS05_13  As O 2 fraction increases, there is greater non-uniformity in fluxes of [O] and O 3 at the surface.  At end of IP, He/O 2 /H 2 O=99-x/x/1  IP - interpulse period (duration – 100  s at 10 kHz) [O 2 ]=75% [O 2 ]=10%

Iowa State University Optical and Discharge Physics EFFECT OF O 2 FRACTION ON TREATMENT ANANTH_ICOPS05_14  Macroscopic non-uniformities in –OH and –OO ultimately arise from significant spatial variation of O, O 3 and OH fluxes.  Microscopic scale non-uniformities arise due to transport limitations of reactive [O] at higher O 2 fractions.  - 5 kV, 760 Torr, He/O 2 /H 2 O=99-x/x/1, 10 kHz, 1 s

Iowa State University Optical and Discharge Physics HUMID AIR - EFFECT OF VOLTAGE POLARITY ANANTH_ICOPS05_15  760 Torr, N 2 /O 2 /H 2 O=79/20/1 cm kV, 2.5 ns MAX  Positive discharge spreads more uniformly on surface.  Surface recombination of O + enhances [O] at surface kV, 10 ns - 15 kV, 2.5 ns +15 kV, 10 ns  [O]  [e] MIN x x10 14 log scale  [e]

Iowa State University Optical and Discharge Physics EFFECT OF POLARITY ON TREATMENT  Pulsed positive polarity operation gives higher uniformity of functionalization due to more uniform formation of [O] and O 3 near the surface. ANANTH_ICOPS05_16  760 Torr, N 2 /O 2 /H 2 O=79/20/1, 10 kHz, 0.15 s

ANANTH_ICOPS05_17 Iowa State University Optical and Discharge Physics IONS AND PHOTONS IN SURFACE CHEMISTRY  UV photons from the plasma can cleave surface bonds.  Ions striking the surface transfer energy and can activate sites.  Postulate creation of intermediate active sites.  Active sites may crosslink in addition to standard reaction pathways.

Iowa State University Optical and Discharge Physics NON-UNIFORMITY DUE TO ‘SHADOWING’ ANANTH_ICOPS05_18  Line-of-sight photon transport fails to reach deep inside surface features.  Crosslinking is relatively higher on surface features exposed to the avalanche where ion and photon fluxes are higher.  - 5 kV, 760 Torr, He/O 2 /H 2 O=98/1/1, 10 kHz, 0.2 s [CROSSLINKS]

Iowa State University Optical and Discharge Physics CONCLUDING REMARKS ANANTH_ICOPS05_19  Multiscale modeling using unstructured meshes was applied to study DBD corona treatment of PP surface with microstructure.  Non-uniformity in functionalization occurs on the macroscopic (few mm) and microscopic ( < 1 µm) scales.  In He/O 2 /H 2 O mixtures, the O 2 fraction can be used to optimize uniformity of treatment.  In humid air, pulsed positive polarity discharges produce more uniform functionalization.  ‘Shadowing’ by surface microstructure results in non-uniform crosslinking with a mechanism using photon and ion fluxes.