Template-assisted synthesis of magnetic wireless micro- and nanoagents
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1 Research Collection Doctoral Thesis Template-assisted synthesis of magnetic wireless micro- and nanoagents Author(s): Zeeshan, Muhammad Arif Publication Date: 2013 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 Template-Assisted Synthesis of Magnetic Wireless Micro- and Nanoagents A dissertation submitted to ETH ZÜRICH for the degree of Doctor of Sciences presented by Muhammad Arif Zeeshan MSc., University of Neuchâtel Born on January 23, 1978 citizen of Switzerland accepted on the recommendation of Prof. Dr. Bradley J. Nelson, examiner Prof. Dr. Antoine Ferreira, co-examiner Prof. Dr. Lixin Dong, co-examiner Dr. Salvador Pané i Vidal, co-examiner 2013
3 Zusammenfassung Das enorme Interesse an der Herstellung von Mikro-und Nanostrukturen begründet sich aus ihren potenziellen Anwendungen in Bereichen wie Biomedizin und Materialwissenschaften, Elektronik, Magnetismus und Energiespeicherung. Diese kleineren Bausteine besitzen verbesserte mechanische, optische, magnetische und elektronische Eigenschaften im Vergleich zu Makrostrukturen. Ferngesteuerte Mikro- und Nanoroboter sind vielversprechende Kandidaten für die minimal-invasive, gezielte Verabreichung von Medikamenten. Diese Dissertation fokusiert auf die Herstellung von magnetischen Mikround Nanoroboters mit dem Vorlagen-Ansatz. Vorlagen-gestützte Fertigung erlaubt es, gewünschte Materialien innerhalb von vorgegebnen Negativ-Strukturen wie Kanälen zu deponieren. Hauptsächlich werden elektrolytische Abscheidung, chemische Polymerisation und chemische Gasphasenabscheidung (CVD) für die Vorlagen-gestützte Fabrikation verwendet. Die Verwendung poröser anodischer Aluminiumoxid (PAA) Vorlagen ermöglicht sowohl die Serienfertigung von Nanodrähten (NWS) durch galvanische Abscheidung und deren anschließende konforme Verkapselung in Graphit durch chemische Gasphasenabscheidung. Eindimensionale PAA-Vorlagen auf Silizium (Si) wurden geschaffen, indem eine aufgedampfte Aluminiumschicht anodisiert wurde. Nach der Anodisierung in Oxalsäure und Schwefelsäure wurden PAA-Vorlagen mit Porendurchmessern im Bereich von 13 nm nm gefertigt. Um Nanodrähte zu erhalten, wurden die Poren der PAA-Vorlagen dur galvanische Abscheidung mit ferromagnetischen Materialien (Fe, Ni) gefüllt. Die in der PAA-Vorlage eingebetteten ferromagnetischen Nanodrähte wurden in eine CVD-Kammer platziert und konform mit Graphit beschichtet. Diese beschichteten Fe Nanodrähte wurden entgegen eines Wasserflusses (0.1 mm s -1 ) magnetisch gesteuert (bei einer magnetischen Feldstärke von 350 Oe und einem magnetischen Gradienten von 50 k Oe m -1 ). Unser Ansatz öffnet neue Wege für das Gestalten und die Synthese von funktionellen graphitbeschichteten Nanodrähte, die für vielversprechende nanorobotischen Anwendungen eingesetzt werden können. v
4 Die Herstellung von Mikrorobotern durch herkömmliche 2D Photolithographie oder durch Zwei-Photonen-Polymerisation, welche bei der 3D-Laser-Lithographie ausgelöst wird, sowie das ferngesteuerte magnetische Antreiben der Mikrorobotern sind jüngst schon erforscht und etabliert worden. Allerdings stehen diesen Herstellungsverfahren nur eine begrenzte Auswahl an Materialien zur Verfügung, was das Funktionalisieren der Mikroroboter einschränkt. In dieser Dissertation wird ein Herstellungsprozess vorgestellt, der auf der galvanischen Abscheidung in 3D-Vorlagen beruht, und damit die Auswahl and möglichen verwendbaren Materialien vergrössert. In einem ersten Schritt wurden diese 3D-Vorlagen durch das Aufbringen einer transparenten Elektrodenschicht (Indium-Zinn-Oxid, ITO) auf einem Glasssubstrat hergestellt. Darauf wurde in einem zweiten Fabrikationsschritt ein positiver Fotolack (AZ 9260) durch Rotationsbeschichtung aufgetragen. Danach wurde mit einem 3D- Laser-Lithographie-System von Nanoscribe GmbH das gewünschte dreidimensionale Muster in den Fotolack geschrieben. In einem vierten Schritt wurden die belichteten Bereiche mit dem AZ 400K Entwickler aufgelöst. Die freigelegten spiralförmigen Kanäle wurden als 3D- Vorlage für die Mikroroboterherstellung benutzt. Die eigentlichen Roboter wurden durch galvanische Abscheidung von Kobalt-Nickel (CoNi) und Polypyrrol (PPy) in die vorgeformten Kanäle hergestellt. Nach dem letzten Fabrikationsschritt, in welchem der Fotolack der 3D-Vorlage aufgelöst wird, bleiben Reihen von dreidimensionalen hybrid Mikrorobotern, mit einer Gesamtlänge von 20!m und einer Filamentdicke von 650 nm, stehen. Die Strukturen wurden im Wasser mit einem schwachen rotierenden Magnetfeld erfolgreich angetrieben. Wegen seiner Formanisotropie wurde der ferromagnetische Kopf orthogonal zur Spiralenachse magnetisiert, was die magnetische Rotation um die Spiralenachse erlaubt. Mit dieser kontrollierten schraubenförmigen Bewegung konnte der Mikroroboter bei einer Rotationsfrequenz von 100 Hz mit einer Geschwindigkeit von 50!m s -1 forwärtsschwimmen. vi
5 Abstract The enormous interest in the fabrication of micro- and nanostructures arises from their potential applications in the areas such as biomedical and material sciences, electronics, magnetism and energy storage. These smaller building blocks posses enhanced mechanical, optical, magnetic and electronic properties compared to their bulk counterparts. Wirelessmanipulated micro and nanoagents are promising candidates for minimally invasive targeted drug delivery. This dissertation focuses on the fabrication of magnetic micro- and nanoagents based on the template-assisted approach. Template-assisted fabrication allows one to obtain desired materials within the channels of templates. Electrodeposition, chemical polymerization and chemical vapor deposition (CVD) are used as major template-assisted strategies. The use of porous anodic alumina (PAA) templates enables both the batch production of nanowires (NWs) by electrodeposition and their subsequent conformal encapsulation in graphite using chemical vapor deposition (CVD). The one-dimensional PAA templates on Si were developed by anodizing an evaporated layer of aluminum. The PAA templates with diameters in the range of 13 nm nm were obtained after carrying out anodization in oxalic and sulfuric acids. Afterwards, electrodeposition was used to fill the pores of the PAA templates with ferromagnetic (Fe, Ni) materials to obtain NWs. Ferromagnetic NWs embedded into the PAA templates were placed inside a CVD chamber and NWs were conformally coated with graphite. The graphite coated Fe NWs were precisely manipulated against a water flow (0.1 mm s -1 using a magnetic field of 350 Oe and a gradient of 50 koe m -1 in a 5-DOF magnetic manipulation system. Our approach opens new avenues for the design and synthesis of functional graphite coated NWs that are promising for nanorobotics applications. Fabrication of microagents either by the conventional 2D photolithography or by two-photon polymerization triggered by 3D laser lithography and successful wireless magnetic actuation are recently well established. However, these fabrication methods provide only a limited selection of materials that severely restricts functionalization of microagents. This work reports a fabrication process based on 3D template-assisted electrodeposition that overcomes vii
6 these limitations. Templates were produced by depositing a transparent electrode layer (indium tin oxide, ITO) on a bare glass substrate as a first step. On top of the electrode, a positive-tone photoresist (AZ 9260) was spin coated and patterned by a 3D laser lithography system provided by Nanoscribe GmbH. Three-dimensional structures were written by laser exposure. The exposed regions were dissolved by AZ 400K developer providing helical channels in the resist layer partially uncovering the electrode. The actual microagents were then deposited into these channels by means of electrodeposition with a cobalt-nickel (CoNi) and a polypyrrole (PPy) helical tail. After dissolving the photoresist, arrays of hybrid threedimensional microagents with a length of 20!m and a filament thickness of 650 nm were obtained. Actuation experiments were conducted in water by applying weak rotating magnetic fields. Due to its shape anisotropy, the ferromagnetic head was magnetized perpendicularly to the longitudinal axis of the microagent, thus causing it to rotate around the helical axis. This stable and controlled rotation similar to a cork-screw motion propelled the micro-agents resulting in a maximal swimming velocity of 50 µm s -1 at a rotating frequency of 100 Hz. viii
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