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. Fröhlich 3 , H. Kersten 1 1 IEAP, Group Plasma Technology, University of Kiel 2 ITAP, University of Kiel 3 INP Greifswald 4 th Graduate Summer Institute ''Complex Plasmas'' August 5 th , 2014 Plasma Technology Plasma Technology August 5 th , 2014 1 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel outline 1. Introduction to parylene 2. The setup 3. Langmuir probe measurements 4. Electrical measurements 5. REM 6. Contact angle measurements Plasma Technology August 5 th , 2014 2 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Parylene Illustrations: SCS Specialty Coating Systems crevice penetrating low permeability to moisture and corrosive UV stable Group of polymers gases properties can be tuned by choosing substituents crevice penetrating low permeability to moisture and corrosive gases high temperature applications good temperature stability long-term UV stability Plasma Technology August 5 th , 2014 3 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Parylene properties Illustrations: SCS Specialty Coating Systems transparent hydrophobic low friction coefficient low gas permeability biostable biocompatible high chemical resistivity oxidation resistant up to 350 ° C / 662 ° F homogeneous coatings Plasma Technology August 5 th , 2014 4 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Parylene Pictures: SCS Specialty Coating Systems Plasma Technology August 5 th , 2014 5 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Parylene Group of polymers properties can be tuned by choosing substituents Plasma Technology August 5 th , 2014 6 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Conventional deposition process 1100 - 1300 ° F 600 -700 ° C the precursor - highly reactive < 194 ° F a dimer monomer < 90 ° C parylene C - a linear polymer Plasma Technology August 5 th , 2014 7 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel PECVD process 1100 - 1300 ° F 600 -700 ° C PECVD P < 194 ° F < 90 ° C Plasma Technology August 5 th , 2014 8 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel PECVD process 1100 - 1300 ° F 600 -700 ° C PECVD P Investigations: < 194 ° F < 90 ° C analyse deposited films - profilometer measurements - electron microscopy - contact angle measurements analyse plasma process - langmuir measurements - electrical measurements Plasma Technology August 5 th , 2014 9 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel ATILA capacitively coupled rf-discharge evaporator 4 vacuum gauges Plasma Technology August 5 th , 2014 10 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel ATILA - substrates silicon wafer glas plates metal plates Plasma Technology August 5 th , 2014 11 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel ATILA – silicon wafer holder Plasma Technology August 5 th , 2014 12 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel substrate positioning a b c d (outside of intense plasma glow) c b Plasma Technology August 5 th , 2014 13 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel Sublimation of the precursor too cold too warm Plasma Technology August 5 th , 2014 14 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel profilometer measurements too less precursor: too much precursor: • negative step • positive step sputtering dominates • dust formation (easily removable) Plasma Technology August 5 th , 2014 15 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel profilometer measurements temperature / coating thick- observations duration P / W ° C ness / nm / min - 43.3 ± 4.2 148…150 blocked by condensation 30 10 - 162.6 ± 45.1 200…220 dust 15 30 6430 ± 188 185…190 resublimation on substrate 10 20 before ignition, dust 72.3 ± 10.7 130…157 dust 20 20 388.8 ± 13.2 120…155 dust 110 30 process pressure of 13.6 Pa Plasma Technology August 5 th , 2014 16 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements probe box pickup-probe for passive rf-compensation ceramic / glas probe tip Plasma Technology August 5 th , 2014 17 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements U fl = 14,8 V U pl = 35,3 V argon p Baratron = 6.4 Pa P = 10 W V bias = 273 V T e = 2.63 eV = 9.6∙10 15 m -3 n e Plasma Technology August 5 th , 2014 18 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements during deposition process 20 sccm argon, P = 10W, p = 10,5Pa Plasma Technology August 5 th , 2014 19 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements during deposition process 20 sccm argon, P = 10W, p = 10,5Pa Plasma Technology August 5 th , 2014 20 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements during deposition process 20 sccm argon, P = 10W, p = 10,5Pa 212 ° F 100 ° C Plasma Technology August 5 th , 2014 21 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel langmuir probe measurements during deposition process probe tip dirty shape of drop at probe tip different kinds of coating Plasma Technology August 5 th , 2014 22 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel electrical measurements 130 ° F 161 ° F 212 ° F Plasma Technology August 5 th , 2014 23 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel electrical measurements 130 ° F 161 ° F 212 ° F coating of window increase in resistivity → inelastic collisions → decrease of n e → collisions with particles Plasma Technology August 5 th , 2014 24 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel electrical measurements 130 ° F 161 ° F 212 ° F Plasma Technology August 5 th , 2014 25 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel electrical measurements 210 ° F periodical particle formation continous particle formaiton? 196 ° F emission intensity also fluctuating resistivity increasing, when V bias decreasing Plasma Technology August 5 th , 2014 26 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel scanning electron microscopy Plasma Technology August 5 th , 2014 27 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel scanning electron microscopy Plasma Technology August 5 th , 2014 28 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel contact angle measurements parylene coating total energy σ total = 64.54 ± 23.25 mN/m dispersive energy σ d = 7.35 ± 13.30 mN/m polar energy σ p = 57.19 ± 19.07 mN/m problem: dust changes the surface energy can be used to gain superhydrophoby or superhydropholy Plasma Technology August 5 th , 2014 29 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel electrical measurements 161 ° F 212 ° F 130 ° F Plasma Technology August 5 th , 2014 30 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel summary The properties of depositing parylene are strongly dependent on the temperature at which sublimation occurs. Polymerisation took place. Low discharge power is enough to initialize polymerisation. No undesired byproducts / chemical decompounds could be found. Plasma Technology August 5 th , 2014 31 Erik v. Wahl
Institute of Experimental and Applied Physics, University of Kiel outlook 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! Plasma Technology August 5 th , 2014 32 Erik v. Wahl
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