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Metal-Ion Implanted Elastomers: Analysis of Microstructures and Characterization and Modeling of Electrical and Mechanical Properties

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Metal-Ion Implanted Elastomers: Analysis of Microstructures and Characterization and Modeling of Electrical and Mechanical Properties Metal-Ion Implanted Elastomers: Analysis of Microstructures and Characterization and Modeling of Electrical and Mechanical Properties THÈSE NO 4798 (2010) PRÉSENTÉE LE 17 SEPTEMBRE 2010 À LA FACULTÉ SCIENCES ET TECHNIQUES DE L'INGÉNIEUR LABORATOIRE DES MICROSYSTÈMES POUR LES TECHNOLOGIES SPATIALES PROGRAMME DOCTORAL EN MICROSYSTÈMES ET MICROÉLECTRONIQUE ÉCOLE POLYTECHNIQUE FÉDÉRALE DE LAUSANNE POUR L'OBTENTION DU GRADE DE DOCTEUR ÈS SCIENCES PAR Muhamed NIKLAUS acceptée sur proposition du jury: Prof. H. P. Herzig, président du jury Prof. H. Shea, directeur de thèse Dr M. Dadras, rapporteur Dr A. Karimi, rapporteur Dr G. Kofod, rapporteur Suisse 2010 Thought, a brief flash in the middle of night, but a flash which means … everything. Jules Henri Poincaré Abstract This thesis reports on the microstructural analysis of metal ion implanted Polydimethylsiloxane (PDMS), and on the characterization and modeling of its electrical and mechanical properties. Low energy (below 35 keV) metal ion implantation into PDMS forms metal nanoparticles in the top 10 nm to 120 nm of the polymer, creating a metal–insulator composite. Above a certain ion dose, the percolation threshold, the particles form a conductive path. By suitable choice of the volume-ratio between the two constituents (metal atoms and PDMS), one is able to create stretchable electrodes capable of sustaining uniaxial strains of up to 175% while remaining conductive, and remaining operational after 105 cycles at 30% strain. These outstanding properties are especially required for flexible electronic and for polymer actuators and sensors. Low energy metal ion implantation into 30 μm thick PDMS was performed at 10 keV and 35 keV with Low Energy Broad Beam Implanter (LEI), and at 2.5 keV, 5 keV and 10 keV with Filtered Cathode Vacuum Arc (FCVA). The metals used for the implantation were Titanium and Gold. Doses ranged from 0.1x1016 at/cm2 to 7x1016 at/cm2, leading to surface resistivities between 100 Ω/square and 100 MΩ/square. Generally lower implantation energy and higher ion doses lead to better conductivities. However doses above the percolation threshold lead to an important increase of stiffness. The effective Young’s modulus measurements for FCVA implanted samples were in the range of 5 MPa. The samples implanted with LEI showed much important increase of the stiffness reaching 80 MPa for the gold and 170 MPa for the titanium implantations. Together the electrical and the mechanical measurements showed the best conductivity-to-compliance-ratio is obtained with FCVA implantation with Gold at 2.5 keV and doses around 1.5x1016 at/cm2. A TEM sample preparation method based on cryo-ultramicrotomy, was developed, adapted for extremely low modulus (1 MPa) elastomers with hard inclusions, allowing high-resolution TEM cross-section micrographs for microstructural analysis of the implanted layers. Gold ions penetrate PDMS by up to 30 nm (for FCVA, 60 nm for LEI) and form crystalline nanoparticles whose size increases with the dose and the energy. Titanium forms a nearly homogeneous amorphous composite with the PDMS up to 18 nm thick (for FCVA) and 120 nm thick for LEI). The penetration depths were confirmed with computer simulations. Using TEM micrographs the metal volume fraction of the composite was accurately determined, allowing conductivity and the Young’s modulus to be plotted vs. the volume fraction. The graphs showed different scalings dependant on the microstructure and on the ion species, allowing for the first time quantitative use of the percolation theory for ion implanted thin films. This allowed linking the composite’s Young’s modulus and conductivity directly to the implantation parameters and volume fraction. Both electrical and mechanical properties were measured on the same samples, and different percolation thresholds and exponents were found, showing that while percolation explains very well both conduction and stiffness of the composite, the interaction between metal nanoparticles occurs differently for determining mechanical and electrical properties. Flexible electrodes fabricated by this ion implantation technique were used to fabricate small arrays of 1 to 3 mm diameter tunable lenses, consisting of electroactive polymer actuators bonded to a socket that provides fluidic coupling between devices. The focal length was electrically tuned from 4 mm to 8 mm by applying a voltage from 0 kV to 1.7 kV. Keywords: Metal ion implantation, Conductivity, Elastic properties, Percolation, microstructure, Electroactive polymers. Abstrakt Die vorliegende Dissertation berichtet über Analysen der Mikrostruktur von Metall- Ionen implantiertem Polydimethylsiloxan (PDMS) und über Charakterisierung und Modellierung der elektrischen und mechanischen Eigenschaften. Niederenergie- Metall-Ionen-Implantation (kleiner als 35 keV) des PDMS bildet Metall-Nanopartikel in obersten 10 nm bis 120 nm dicken Schichten des Polymers. Dadurch entsteht ein Metall-Isolator-Verbundwerkstoff. Ab einer bestimmten Ionenkonzentration, bekannt als die Perkolationsschwelle, formen die Partikel ein für den elektrischen Strom leitendes Netzwerk. Durch ein geeignetes Volumenverhältniss der beiden Komponenten, der Metallionen und des PDMS, werden flexible Elektroden entwickelt, die uniaxiale mechanische Spannungen von bis zu 175% ertragen, ohne dabei die elektrische Leitfähigkeit zu verlieren. Die Elektroden bleiben nach 105 Zyklen bei 30% mechanischer Spannung operationsfähig. Diese herausragenden Eigenschaften sind besonders interessant für flexible Elektronik, für Polymer- Aktoren und Sensoren. Die Implantationen der 30 μm dünnen Schicht des PDMS wurden für 10 keV und 35 keV mit einem Niederenergie-Breitstrahl-Implanter (LEI), und für 2,5 keV, 5 keV und 10 keV mit einem Filter-Kathode-Vakuum-Elektrobogen-Implanter (FCVA) durchgeführt. Für die Implantation verwendete Metalle waren Titanium und Gold. Die implantierte Ionendosis reichte von 0.1x1016 at/cm2 bis 7x1016 at/cm2, was zu spezifischen Flächenwiderständen zwischen 100 Ω/Quadrat und 100 MΩ/Quadrat führte. Generell folgt aus höherer Ionendosis und niedrigerer Energie bessere elektrische Leitfähigkeiten. Allerdings führen die Konzentrationen oberhalb der Perkolationsschwelle zu einer bedeutenden Steigerung der Steifigkeit. Der Elastizitätsmodulmessungen für die von FCVA implantierten Proben lagen im Bereich von 5 MPa. Die Proben, die mit LEI implantiert wurden, zeigten eine bedeutend grössere Zunahme der Steifigkeit, die 80 MPa für die Gold- und 170 MPa für die Titaniumimplantate ergab. Die elektrischen und mechanischen Messungen zigten zusammen das beste Verhältniss zwischen der elektrischen Leitfähigkeit und der Elastizität für die FCVA-Goldimplantation mit 2.5 keV und einer Dosis von 1.5x1016 at/cm2. Eine Probenvorbereitungsmethode für die Transmissionelektronenmikroskopie (TEM) wurde entwickelt. Sie basiert auf der Kryo-Ultramikrotomie und ist für extrem niedrige Elastizitätsmodule (1 MPa) geeignet. Die Methode erlaubt mikrostrukturelle Analysen der implantierten Schichten dank hochauflösenden TEM-Querschnittsbilder. Goldione dringen bis zu 30 nm tief in PDMS ein (für FCVA, 60 nm für LEI) und bilden danach kristalline Nanopartikel, deren Größe mit der Implantationsenergie und der Ionendosis steigt. Titaniumionen bilden mit PDMS eine fast homogene, 18 nm dicke (für FCVA, 120 nm für LEI), amorphe Schicht. Die Eingangstiefen der implantierten Ionen wurden mit Computer simuliert und bestätigt. Dank den TEM-Querschittsbilder wurde die Volumenfraktion (Konzentration) der Metallpartikel innerhalb der implantierten PDMS-Schicht determiniert, so dass die elektrische Leitfähigkeit und das Elastizitätsmodul als Funktion der Volumenfraktion graphisch dargestellt werden konnten. Zum ersten Mal wurde die Perkolationstheorie an implantierten dünnen Schichten angewendet und quantitativ ausgewertet. Die Graphiken zeigten diverse Skalierungen abhängig von der Mikrostruktur und dem implantierten Element. Dies ermöglichte eine Beziehung zwischen dem Elastizitätsmodul (oder der Leitfähigkeit) und den Implantationsparametern zu etablieren, und zeigte unterschiedliche elektrische und mechanische Perkolationsparameter, die zum ersten mal gleichzeitig an denselben Proben gemessen wurden. Flexible Elektroden angefertigt durch Ionenimplantation wurden für die Herrstellung von in Matrizen geordneten, abstimmbaren, kleinen (1-3 mm Durchmesser) Linsen verwendet. Sie bestanden aus elektroaktiven Polymer-Aktoren und PDMS-Membranen (Linsen) verbunden durch mit Flüssigkeit gefüllten Kanälen. Die Brennweite wurde elektrisch, durch das Anlegen einer Spannung von 0 kV bis 1,7 kV, von 4 mm bis 8 mm abgestimmt. Stichwörter: Metall-Ionen-Implantation, elektrische Leitfähigkeit, Elastizität, Perkolation, Mikrostruktur, Elektroaktive Polymere. Contents INTRODUCTION 1 CHAPTER 1 5 1. ELECTROACTIVE POLYMERS 5 1.1. Electromechanical mechanism for DEAP 6 1.2. Performance of field-activated Electroactive Polymers 7 1.3. Field-activated DEAP fabricated in “Microsystems for Space Technologies Laboratory” (LMTS-EPFL) 8 CHAPTER 2 13 2. METAL IMPLANTATION IN POLYMERS 13 2.1. Polymers 14 2.2. PDMS 14 2.3. Physical interactions between polymer and energetic ion 15 2.3.1 Energy-loss processes of ions in matter 16 2.3.2 Range and damage distributions 18 2.4. Simulation 20 2.4.1 Simulation of implantation in compounds 21 2.5. Physical and chemical changes of polymers after ion implantation or irradiation 22 2.5.1 Hardness 23 2.5.2 Metal-polymer interface formation and adhesion 24 2.5.3 Increasing of
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