Research Collection. Doctoral Thesis. ETH Library. Author(s): Baettig, Julia. Publication Date: 2014
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1 Research Collection Doctoral Thesis Sequential Coating of Nanopores with Charged Polymers: A General Approach for Controlling Pore Properties of Self- Assembled Block Copolymer Membranes Author(s): Baettig, Julia Publication Date: 2014 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 DISS.-NO. ETH Sequential Coating of Nanopores with Charged Polymers: A General Approach for Controlling Pore Properties of Self-Assembled Block Copolymer Membranes A dissertation submitted to the ETH ZÜRICH for the degree of Doctor of Sciences presented by Julia Baettig M. A., State University of New York at Buffalo, U.S.A. born May 14 th, 1980 citizen of the United States of America accepted on the recommendation of Prof. Dr. Dieter A. Schlüter, examiner Prof. Dr. Anders Egede Daugaard, co-examiner Prof. Dr. Lucio Isa, co-examiner Dr. Anzar Khan, co-examiner 2014
3 Summary R ecent advances in membrane technology have led to the development of block copolymer membranes with an ordered isoporous structure formed by selfassembly. The functionalization of such membranes imparts them with huge potential in the fields of catalysis, water treatment, enzyme immobilization, and chemical separations. Membranes can be functionalized by covalent modification or by the addition of polymers that bind to the outermost membrane material, through ionic interactions, hydrogen bonding, or hydrophobic interactions. In this thesis, progress was made towards the development of a general strategy for the functionalization of block copolymer membranes. Constructed from poly(styrene)-b-poly(4- vinylpyridine) (PS-b-P4VP), these polymeric phase-inversion membranes possess a polystyrene core and a surface entirely coated with P4VP. The initial functionalization of this membrane was performed by using poly(acrylic acid), which has the unique property of being able to both hydrogen bond with the 4-vinylpyridine groups and also simultaneously present negatively charged carboxylate groups to the interior of the nanopore. Therefore, PAA was used for a base layer from which to begin layer-by-layer assembly. This was then followed by the layering of oppositely charged polyelectrolyte chains onto the pore wall by pushing polyelectrolyte solutions in sequence through the membrane. A method was developed for depositing polyelectrolyte multilayers onto and in the pores of a polystyrene-b-poly(4- vinylpyridine) membrane. By using a strong and a weak polyelectrolyte, poly(styrene sulfonate) and protonated poly(ethylene imine), we looked at layer development as it relates to ph, and correspondingly charge of the poly(ethyleneimine). Weak-weak and strong-strong polyelectrolyte combinations were also explored. A pressure sensor was used to monitor the change in pore size during the layer deposition, providing valuable insight into the layer-bylayer process inside of the nanopore. Using charged polyelectrolytes we made inroads to control the pore size and chemistry. The pore size and chemistry was then explored with dye separation and sieving curve analyses. ii
4 Zusammenfassung S eit kurzem ist es möglich, Copolymermembranen herzustellen, bei denen eine geordnete isopore Struktur durch Selbstorganisation erzielt wird. Werden diese Membranen zusätzlich noch funktionalisiert, können sie in den Bereichen Katalyse, Wasserbehandlung, Enzymimmobilisierung oder chemischer Trennung eingesetzt werden. Diese Funktionalisierung geschieht entweder durch kovalente Verknüpfung oder durch das Hinzufügen von Polymeren an die äusserste Membranschicht, wobei die Polymere entweder durch ionische oder hydrophobe Wechselwirkungen oder durch Wasserstoffbrücken gebunden werden. Diese Dissertation dokumentiert die Fortschritte, die bei der Entwicklung einer allgemeinen Strategie zur Funktionalisierung von Blockcopolymermembranen erzielt wurden. Ausgehend von Polystyrol-b-poly(4-vinylpyridin) (PS-b-P4VP), besitzen diese durch Phasenumkehr hergestellten Membranen einen Polystyrol-Kern und eine vollständig mit P4VP bedeckte Oberfläche. Die erste Funktionalisierung dieser Membran wurde mit Polyacrylsäure (PAA) durchgeführt. Diese hat die einzigartige Eigenschaft, einerseits Wasserstoffbrücken mit den 4-Vinylpyridin-Gruppen zu bilden und andererseits im Inneren der Nanoporen negativ geladene Carboxylatgruppen zur Verfügung zu stellen. Aus diesen Gründen ist PAA ein idealer Unterbau, um eine schichtweise Selbstorganisation zu beginnen. Auf die PAA folgen mehrere Lagen von entgegengesetzt geladenen Polyelektrolytketten, die durch abwechselndes Spülen der Membran mit Polyelektrolytlösungen an die Porenwände angebracht wurden. Es wurde eine Methode entwickelt, um mehrlagige Polyelektrolyte auf und in die Poren einer Polystyrol-b-poly(4-vinylpyridin)-Membran anzubringen. Ein starkes und ein schwaches Polyelektrolyt wurden eingesetzt, d.h. Natriumpoly(styrolsulfonat) und protoniertes Polyethylenimin, und der Schichtaufbau und seine ph-abhängigkeit und damit die Ladung des Polyethylenimins wurden untersucht. Darüber hiraus galt es schwach-schwache und stark-starke Polyelektrolytkombinationen zu untersuchen. Mittels eines Drucksensors konnte die Veränderung der Porengrösse während der Ablagerung der Schichten untersucht werden. Dies ergab wertvolle Erkenntnisse über den schichtweisen Aufbau im Inneren der iii
5 Nanoporen. Durch die Verwendung von geladenen Polyelektrolyten erzielten wir Fortschritte in der Steuerung der Porengrösse und Porenchemie. Mit den so erhaltenen Membranen wurden dann Trennungsexperimente an Farbstoffmischungen sowie Siebkurvenanalysen durchgeführt. iv
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