Feasibility study on polyparylene deposition in a PECVD reactor E. - - PowerPoint PPT Presentation

feasibility study on polyparylene deposition in a pecvd
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Feasibility study on polyparylene deposition in a PECVD reactor E. - - PowerPoint PPT Presentation

Institute of Experimental and Applied Physics, University of Kiel Institute of Experimental and Applied Physics Feasibility study on polyparylene deposition in a PECVD reactor E. v. Wahl 1 , C Kirchberg 2 , M. Frhlich 3 , H. Kersten 1 1 IEAP,


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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 1

Institute of Experimental and Applied Physics

Plasma Technology

Feasibility study on polyparylene deposition in a PECVD reactor

  • E. v. Wahl1, C Kirchberg2, M. Fröhlich3, H. Kersten1

4th Graduate Summer Institute ''Complex Plasmas'' August 5th, 2014

1 IEAP, Group Plasma Technology, University of Kiel 2 ITAP, University of Kiel 3 INP Greifswald

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 2

  • utline
  • 1. Introduction to parylene
  • 2. The setup
  • 3. Langmuir probe measurements
  • 4. Electrical measurements
  • 5. REM
  • 6. Contact angle measurements
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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 3

Parylene

Group of polymers

properties can be tuned by choosing substituents

Illustrations: SCS Specialty Coating Systems

crevice penetrating UV stable low permeability to moisture and corrosive gases crevice penetrating high temperature applications long-term UV stability low permeability to moisture and corrosive gases good temperature stability

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 4

Parylene properties

Illustrations: SCS Specialty Coating Systems

transparent hydrophobic low friction coefficient low gas permeability biostable biocompatible high chemical resistivity

  • xidation resistant up to 350 °C / 662 °F

homogeneous coatings

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 5

Parylene

Pictures: SCS Specialty Coating Systems

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 6

Parylene

Group of polymers

properties can be tuned by choosing substituents

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 7

Conventional deposition process 1100 - 1300 °F 600 -700 °C < 194 °F < 90 °C the precursor - a dimer highly reactive monomer parylene C - a linear polymer

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 8

PECVD process P PECVD 1100 - 1300 °F 600 -700 °C < 194 °F < 90 °C

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 9

PECVD process P PECVD Investigations:

analyse deposited films

  • profilometer measurements
  • electron microscopy
  • contact angle measurements

analyse plasma process

  • langmuir measurements
  • electrical measurements

1100 - 1300 °F 600 -700 °C < 194 °F < 90 °C

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 10

ATILA capacitively coupled rf-discharge evaporator 4 vacuum gauges

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 11

ATILA - substrates silicon wafer glas plates metal plates

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 12

ATILA – silicon wafer holder

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 13

substrate positioning a b c d (outside of intense plasma glow) b c

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 14

Sublimation of the precursor too cold too warm

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 15

profilometer measurements too less precursor:

  • negative step
  • sputtering dominates

too much precursor:

  • positive step
  • dust formation (easily

removable)

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 16

profilometer measurements

temperature / °C coating thick- ness / nm

  • bservations

duration / min P / W 148…150

  • 43.3 ± 4.2

blocked by condensation 30 10 200…220

  • 162.6 ± 45.1

dust 15 30 185…190 6430 ± 188 resublimation on substrate before ignition, dust 10 20 130…157 72.3 ± 10.7 dust 20 20 120…155 388.8 ± 13.2 dust 110 30

process pressure of 13.6 Pa

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 17

langmuir probe measurements pickup-probe for passive rf-compensation probe tip ceramic / glas probe box

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 18

langmuir probe measurements argon pBaratron = 6.4 Pa P = 10 W Vbias = 273 V T

e

= 2.63 eV ne = 9.6∙1015 m-3 Ufl = 14,8 V Upl = 35,3 V

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 19

langmuir probe measurements during deposition process 20 sccm argon, P = 10W, p = 10,5Pa

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 20

langmuir probe measurements during deposition process 20 sccm argon, P = 10W, p = 10,5Pa

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 21

20 sccm argon, P = 10W, p = 10,5Pa langmuir probe measurements during deposition process 212 °F 100 °C

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 22

langmuir probe measurements during deposition process probe tip dirty shape of drop at probe tip different kinds of coating

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 23

electrical measurements

161 °F 212 °F 130 °F

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 24

electrical measurements coating of window

increase in resistivity → inelastic collisions → decrease of ne → collisions with particles

161 °F 212 °F 130 °F

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 25

electrical measurements

161 °F 212 °F 130 °F

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 26

electrical measurements

continous particle formaiton? periodical particle formation emission intensity also fluctuating resistivity increasing, when Vbias decreasing

210 °F 196 °F

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 27

scanning electron microscopy

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 28

scanning electron microscopy

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 29

contact angle measurements problem: dust changes the surface energy can be used to gain superhydrophoby or superhydropholy parylene coating total energy σtotal = 64.54 ± 23.25 mN/m dispersive energy σd = 7.35 ± 13.30 mN/m polar energy σp = 57.19 ± 19.07 mN/m

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 30

electrical measurements

161 °F 212 °F 130 °F

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 31

summary The properties of depositing parylene are strongly dependent on the temperature at which sublimation

  • ccurs.

Polymerisation took place. Low discharge power is enough to initialize polymerisation. No undesired byproducts / chemical decompounds could be found.

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 32

  • utlook

More deposition trials are needed in order to obtain a clean thin film deposition. Contact angle measurements have to be done on samples without dust. Mass spectrometry could give an insight into the chemical reactions. Thank you very much for your attention!

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 33

literature

[1] Phil Morten Hundt, Diplomarbeit, Spektroskopische Diagnostik an Prozessplasmen, CAU 2009 [2] J. Berndt, E. Kovacevic, I. Stefanovic, O. Stepanovic, S. H. Hong, L. Boufendi and J. Winter, Some Aspects of Reactive Complex Plasmas. Contrib. Plasma Phys., vol. 49, 107–133 (2009). [3] S. A. Khrapak et al., Phys. Rev. E 72, 016406 (2005) [4] Hollenstein, Ch.: The physics and chemistry of dusty plasmas. Plasma Physics and Controlled Fusion, 42:R93–R104, 2000 [5] Bouchoule, A. (Herausgeber): Dusty Plasmas - Physics, Chemistry and Technological Impacts in Plasma Processing. Wiley-VCH Verlag, 1999 [6] Cui, C. und J. Goree: Fluctuations of the charge on a dust grain in a plasma. IEEE Transactions on Plasma Science, 22:151–158, 1994 [7] Patrick Sadler, Diplomarbeit, Partikelbildung in reaktiven Plasmen unter Verwendung kohlenwasserstoffhaltiger bzw. siliziumorganischer Precursoren, CAU 2010 [8] Kortshagen, U. und U. Bhandarkar: Modeling of particulate coagulation in low pressure plasmas. Physical Review E, 60:887–898, 1999 [9] H. Ketelsen, Diplomarbeit, Mie-Ellipsometrie an staubigen Plasmen, CAU 2009 [10]

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 34

deposition of parylene in ATILA

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 35

langmuir probe measurements – power dependence Argon p = 6,4Pa

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 36

Argon P = 10W langmuir probe measurements – pressure dependence

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 37

Die Selfbias-Spannung Precursor wird „verbraucht“, Druck sinkt Plasma zünden Wände werden beschichtet

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Institute of Experimental and Applied Physics, University of Kiel

Erik v. Wahl

Plasma Technology

August 5th, 2014 38

Die Selfbias-Spannung

aus [A. Keudell, Vorlesungsskript, 2012]

Vbias ist empfindlicher Indikator für eine Beschichtung der Wände mit einem Dielektrikum