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Outgassing Rates of PEEK, Kapton® and Vespel® Polymers Sergio Giacomo Sammartano

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Outgassing Rates of PEEK, Kapton® and Vespel® Polymers Sergio Giacomo Sammartano Outgassing Rates of PEEK, Kapton® and Vespel® Polymers Sergio Giacomo Sammartano Degree Thesis Materials Processing Technology 2020 Sergio Giacomo Sammartano DEGREE THESIS Arcada Degree Programme: Materials Processing Technology Identification number: 18727 Author: Sergio Giacomo Sammartano Title: Outgassing rates of PEEK, Kapton® and Vespel® polymers Supervisor (Arcada): Mariann Holmberg Supervisor (CERN): Ivo Wevers Examiner (Arcada): Stewart Makkonen-Craig Commissioned by: CERN Abstract: In this study commissioned by CERN, the outgassing behaviour of PEEK, Kapton® and Vespel® polymers has been investigated for potential use in the vacuum systems of parti- cle accelerators. Polymeric materials are in general avoided in high vacuum (HV) and ultra-high vacuum (UHV) applications due to their high outgassing rates, which cannot be effectively reduced via bakeout procedures typically used with metals because of their usually low melting points and loss of mechanical performance above the glass transition temperature. The selected polymers have greater usability potential due to their superior thermal resistance and relatively low outgassing rates compared to most other polymers. Pump-down measurements were conducted on at least 5 samples of different thicknesses for each material, exposed to normal levels of moisture in the air (30-60% R.H.) prior to the tests. The data collected allowed to establish that diffusion of H2O molecules from the bulk to the surface of these materials represents their main source of outgassing when un- der vacuum; the concurrent release of other atmospheric species such as N2, O2, CO and Ar above normal levels, detected through spectrometric analysis of the residual gases, suggested that PEEK and Vespel® can also trap relevant amounts of air simply upon ex- posure. The decay of the outgassing rates of all three polymers, initially proportional to the inverse of the square root of time, was characterized by a time constant 휏 that depend- ed on the diffusion coefficient of water inside the material and the square of its thickness; the diffusive process exhibited Fickian characteristics during pumping times up to 3휏, but diverged considerably from the expected behaviour when extending the pumping beyond this limit, indicating the occurrence of a secondary diffusive mechanism becoming mani- fest at low concentrations of the diffusing species in the bulk. An empirical model con- sisting of a 3-step equation was obtained through regression analysis of the data and the values of diffusion coefficients D and initial moisture contents c0 of each material were estimated by optimizing the parameters in the equations during the fitting procedure. The computed diffusion coefficients were 4.2∙10-9 cm2 s-1 for PEEK, 1.7∙10-9 cm2 s-1 for Kap- ton® and 1.8∙10-9 cm2 s-1 for Vespel®, while the initial moisture content was estimated to be ca 0.3% in PEEK and ca. 1% in the other two materials. These values were found in good agreement with the information retrieved from the available sources. Keywords: Outgassing, vacuum, polymers, PEEK, polyimides, diffusion, CERN Number of pages: 95 Language: English Date of acceptance: 29 May 2020 2 AKNOWLEDGMENTS First and foremost, I would like to deeply thank my CERN supervisor, Ivo Wevers, for providing me with his invaluable advice throughout my whole experience as a technical student at the laboratory. This research project would have not been possible without his guidance, his thoughtful insights and troubleshooting skills, and I am sincerely grateful to have been given the chance to learn so much while working under his supervision. My sincere thanks also go to all the members of the VSC group, whom it has been an honour and pleasure to work with, and in particular to Giuseppe Bregliozzi, leader of the BVO section, for his constructive suggestions and constant support during the exe- cution of the experiments. I wish to express my most sincere appreciation to my university supervisor, Mariann Holmberg, who has inspired and encouraged me not only during the writing of this doc- ument, but also throughout the time I spent at Arcada as a student: her enthusiasm for the discipline of materials science has truly been an invaluable source of motivation during my entire academic career, and it will continue to be so in the future. Last, but not least, I would like to thank the whole staff of the department of Energy and Materials Technology at Arcada, for giving me the opportunity to study and learn in such a friendly and stimulating environment. In particular, I thank Mirja Andersson, head of the department, for teaching me research methodology and project management skills, and Rene Herrmann, for reigniting over and over my passion for mathematical and physical disciplines throughout his courses. 3 CONTENTS LIST OF FIGURES ....................................................................................................... 6 LIST OF TABLES ......................................................................................................... 8 LIST OF SYMBOLS (IN ORDER OF APPEARANCE) ................................................. 9 LIST OF ABBREVIATIONS (IN ALPHABETIC ORDER) ........................................... 11 1 INTRODUCTION ................................................................................................. 12 1.1 Background ................................................................................................................. 13 1.1.1 The European Organization for Nuclear Research (CERN) ............................... 13 1.1.2 The Vacuum at CERN ......................................................................................... 15 1.2 Scope of the Thesis ..................................................................................................... 17 2 LITERATURE REVIEW ....................................................................................... 17 2.1 Fundamentals of Vacuum Science .............................................................................. 17 2.1.1 Units..................................................................................................................... 18 2.1.2 Number Density, Ideal Gas Law and the Kinetic Theory of Gases ..................... 18 2.1.3 Knudsen Number and Gas Flow Regimes .......................................................... 22 2.1.4 Flow Measurement: Gas Throughput, Pumping Speed, Conductance ............... 24 2.2 Sorption Phenomena ................................................................................................... 29 2.2.1 Desorption ........................................................................................................... 30 2.2.2 Diffusion ............................................................................................................... 33 2.3 Pumping Principles and Technologies ........................................................................ 37 2.3.1 The Pump-Down Process.................................................................................... 37 2.3.2 Pumps and Pumping Technologies ..................................................................... 39 2.4 Vacuum Measurements .............................................................................................. 46 2.4.1 Pressure Measurement and Vacuum Gauges .................................................... 47 2.4.2 Mass Spectrometry .............................................................................................. 50 2.5 Overview of Polymers.................................................................................................. 51 2.5.1 General Aspects .................................................................................................. 51 2.5.2 Outgassing of Polymers ...................................................................................... 55 3 MATERIALS AND EXPERIMENTAL PROCEDURES ......................................... 56 3.1 Samples Information.................................................................................................... 56 3.2 Equipment ................................................................................................................... 59 3.3 Experimental Procedures ............................................................................................ 60 4 RESULTS ............................................................................................................ 61 4.1 Pump-Down Curves and Specific Outgassing Rates .................................................. 61 4.1.1 Background Measurement .................................................................................. 61 4 4.1.2 Pump-Down Curves Obtained with the Samples ................................................ 62 4.2 Mass Spectra ............................................................................................................... 66 4.2.1 Background Measurement .................................................................................. 66 4.2.2 Mass Spectra of the Samples ............................................................................. 67 5 ANALYSIS OF THE RESULTS ........................................................................... 69 6 DISCUSSION ...................................................................................................... 73 7 CONCLUSIONS .................................................................................................. 75 REFERENCES ..........................................................................................................
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