Graphene membranes synthesis and mass transport across atomic thickness porous membranes
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1 Research Collection Doctoral Thesis Graphene membranes synthesis and mass transport across atomic thickness porous membranes Author(s): Buchheim, Jakob Publication Date: 2016 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. ETH NO GRAPHENE MEMBRANES SYNTHESIS AND MASS TRANSPORT ACROSS ATOMIC THICKNESS POROUS MEMBRANES A thesis submitted to attain the degree of DOCTOR OF SCIENCES of ETH ZURICH (Dr. sc. ETH Zurich) presented by JAKOB KILIAN BUCHHEIM MSc. ETH in Mechanical Engineering ETH Zürich born on citizen of Germany accepted on the recommendation of Prof. Dr. Hyung Gyu Park, supervisor Prof. Dr. Dimos Poulikakos, co-examinor Prof. Dr. Nicolas Noiray, co-examinor 2016
3 ABSTRACT The discovery of 2D materials like graphene has introduced a paradigm in a variety of research fields. Its outstanding electrical, thermal and mechanical properties enable new advances in science and engineering. Among other fields, membrane technology could greatly benefit from such an ultrathin material. Graphene displays extraordinary mechanical strength and molecular tightness in its pristine state, which render the material a perfect choice as a basis for subsequent pore formation. Due to the atomic thickness such membranes out of porous graphene are expected to impose minimal flow resistance. A successful transformation of graphene into a membrane, therefore, would be a change of paradigm in membrane science, since it would define the ultimate permeation limit. Here, the laboratory scale synthesis and first macroscopic mass transport characterization of such porous graphene membranes are described. Graphene is synthesized at a centimeter scale by chemical vapor deposition. Two monolayers of graphene are transferred onto a porous support subsequently, which isolates the leak tight, freestanding graphene double layer. The freestanding graphene is then punctured with pores. In order to allow detailed analyses of the transport phenomena across porous graphene, the precise knowledge about created pore sizes and the membrane area is necessary. Therefore, the potential of pattern formation by the vii
4 versatile nanopatterning technique of focused ion beam milling is investigated in detail. High energetic focused ion hit the freestanding graphene lattice and can remove a single C atom, a mechanism that can be well described by the binary collision theory of the incident ions with the C lattice atom. Precise control of the exposure dose leads to the formation of pore arrays up to in number, having controlled sizes ranging from ~3.7 nm to 1 μm. Gas flow measurements through these synthesized graphene membranes exhibit ultimate permeation. For membrane pore sizes smaller than ~50 nm transport can be described by a free molecular flow at atmospheric pressures, and large pores display viscosity dominated flow following continuum theory for flow through infinitely thin orifices. Small sub-10-nmpored graphene membranes display gas separation performance based on Graham s law. Water flow measurements through graphene with pores between 5.7 nm to 1 μm show that the flow can be described by a continuum theory for flow through infinitely thin orifices which is also an upper limit of permeation through pores of a given size. The present thesis experimentally confirms the great potential of porous graphene as an ultimately permeable membrane with defining an upper limit for mass transport across membrane materials. viii
5 ZUSAMMENFASSUNG Die Entdeckung zweidimensionaler Kristalle wie Graphen führte zu einem Paradigmenwechsel in einer Vielzahl von Forschungsfeldern. Die herausragenden elektrischen, thermischen und mechanischen Eigenschaften des Graphens ermöglichen neue Entwicklungen in der Forschung und in den angewandten Ingenieurswissenschaften. Die Membran-Technologie kann, wie viele andere Bereiche, von diesem ultra-dünnen Material profitieren. In unmodifiziertem Zustand hat Graphen eine außergewöhnliche mechanische Festigkeit und ist eine perfekte Diffusionsbarriere für Moleküle. Beide Eigenschaften bezeichnen ein Material, welches ideal zur gezielten Perforation und somit Herstellung einer porösen Membran geeignet ist. Es ist zu erwarten, dass aufgrund der atomaren Dicke einer solchen Membran der Durchflusswiderstand von Fluiden minimal ist. Die erfolgreiche Herstellung einer ebensolchen Membran minimalen Widerstands bedeutet einen Durchbruch in den Membranwissenschaften, da diese Membran die Obergrenze der maximal möglichen Permeation definieren würde. In vorliegender Forschungsarbeit wird in einem ersten Schritt die Synthese einer porösen Graphen-Membran auf Labormaßstab beschrieben. Im Folgenden werden erstmalig die makroskopischen Transporteigenschaften dieser Membrane bestimmt. Durch chemische Gasphasenabscheidung wird Graphen großflächig auf Zentimeter-Skala synthetisiert. Anschließend werden zwei Graphen-Monolagen auf ein löchriges Substrat xi
6 übertragen. Sie überspannen nun freistehend/-schwebend, aber leckfrei die Löcher in dem darunterliegenden Trägermaterial. Das freistehende Graphen wird nun perforiert. Um eine detaillierte Analyse der Transportphänomene von porösem Graphen zu ermöglichen, muss die genaue Größe der Poren sowie der gesamten Membranfläche bekannt sein. Daher wurden die Eigenschaften von fokussierten Ionenstrahlen, einer breit genutzten Oberflächenstrukturierungstechnologie, für die Strukturierung von freistehendem Graphen im Detail untersucht. Hochenergetische Ionen treffen auf den zweidimensional Graphen-Kristall und können einzelne Kohlenstoffatome herauslösen. Diese Interaktion zwischen dem eintreffenden, energetischen Ion und den Kohlenstoffgitteratomen wird mit Hilfe der binären Kollisionstheorie von Atomen beschrieben werden. Durch genaue Kontrolle der Menge an Ionen, die das Graphen trifft, können Felder mit bis zu Löchern mit genau definiertem Durchmesser zwischen 3.7 nm und 1 μm hergestellt werden. Die Messung von Gasfluss durch diese hergestellten Membranen weist einen maximalen Durchfluss an der Obergrenze der möglichen Permeation auf. Der Gasfluss durch Membranen, deren Poren kleiner als ~50 nm sind, kann mittels freier Molekularströmung durch Öffnungen bei atmosphärischem Druck beschrieben werden. Für Membranen mit größeren Poren folgt der Durchfluss der klassischen Kontinuumstheorie für Strömung durch unendlich dünne Öffnungen, die von der Viskosität des Gases bestimmt wird. Membranen mit Poren, die kleiner als 10 nm sind, xii
7 ermöglichen zusätzlich die Filtration von Gasen auf Basis des Graham schen Gesetzes. Der Wassertransport durch Graphenporen im Größenbereich zwischen 5.7 nm und 1 μm wird ebenso durch die Kontinuumstheorie für Strömung durch unendlich dünne Öffnungen charakterisiert und definiert daher eine Obergrenze für den maximal möglichen Durchfluss bei festgelegter Porengröße. Damit bestätigt die vorliegende Arbeit experimentell das große Potential von porösen Graphen-Membranen, als maximal permeables Membranmaterial. xiii
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