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Ion-Track Technology Based Synthesis and Characterization of Gold and Gold Alloys Nanowires and Nanocones

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Ion-Track Technology Based Synthesis and Characterization of Gold and Gold Alloys Nanowires and Nanocones Ion-track technology based synthesis and characterization of gold and gold alloys nanowires and nanocones Vom Fachbereich Material- und Geowissenschaften der Technischen Universität Darmstadt zur Erklärung des akademischen Grades eines Doktors der Naturwissenschaften (Dr. rer. nat.) genehmigte Dissertation von Dipl. Ing. M.Sc. Loïc Burr aus Colmar (Frankreich) June 2016 - Darmstadt – D17 Ion-track technology based synthesis and characterization of gold and gold alloys nanowires and nanocones genehmigte Disseration von Dipl. Ing. M.Sc. Loïc Burr aus Colmar (Frankreich) 1. Gutachten: Prof. Dr. Christina Trautmann 2. Gutachten: Prof. Dr. Ralph Krupke Tag der Einreichung: 21.04.2016 Tag der mündlichen Prüfung: 21.04.2016 Darmstadt – 2016 D17 II | P a g e The work described in this thesis was carried out between November 2012 and June 2013 under the supervision of Prof. Dr. Trautmann at the Materials Research group of the GSI Helmholtz Centre for Heavy Ion Reseach, Plackstraße 1, D- 64291 Darmstadt, Germany Top cover image: colorized SEM image of Au nanowires standing on their Au backelectrode fabricated by electrodeposition in etched ion track templates as presented in this thesis Back cover image: modified SEM image of Au nanocones with their caps overlaying a nanocone array III | P a g e Erklärung zur Dissertation Hiermit versichere ich, die vorliegende Dissertation ohne Hilfe Dritter und nur mit den angegebenen Quellen und Hilfsmitteln angefertigt zu haben. Alle Stellen, die aus den Quellen entnommen wurden, sind als solche kenntlich gemacht worden. Diese Arbeit hat in dieser oder ähnlicher Form noch keiner Prüfungsbehörde vorgelegen. Darmstadt, den 19.04.2016 _________________________________ (Loïc Burr) Loïc Burr Ion-track technology based synthesis and characterization of gold and gold alloys nanowires and nanocones PhD Thesis, Technische Universität Darmstadt, Darmstadt, Germany URN: urn:nbn:de:tuda-tuprints-55410 URI: http://tuprints.ulb.tu-darmstadt.de/id/eprint/5541 Copyright © 2016 by L. Burr IV | P a g e “Go back to work” B.S. V | P a g e Zusammenfassung Metallische Nanostrukturen sind äußerst attraktiv für Anwendungen in Batterien, Solarzellen oder Arzneimitteln. In dieser Doktorarbeit wurden folgende Gold- Nanostrukturen durch elektrochemische Abscheidung in geätzten Ionenspurmembranen synthetisiert: (1) zylindrische Nanodrähte bestehend aus Gold oder Gold-Silber-Legierungen, (2) poröse, zylindrische Gold-Nanodrähte hergestellt durch selektives Auflösen des Silberanteils und (3) konische Gold- Nanodrähte (auch Nanokegel genannt). Durch Kontrolle der Prozessparameter wurden zylindrische Nanodrähte unterschiedlicher Zusammensetzung (Au; Au60Ag40; Au40Ag60; Ag) und mit vorgegebenen Durchmessern abgeschieden. Für Au40Ag60-Nanodrähte führte chemisches Auflösen des Silbers zu porösen Au-Nanodrähten mit stark vergrößerter Oberfläche. Morphologie und Zusammensetzung dieser Strukturen wurden mit energiedispersiver Röntgenspektroskopie (EDX) und Transmissions- elektronmikroskopie (TEM) untersucht. Die Analyse der elementaren Zusammensetzung der Au-Ag-legierten Drähte gibt klare Hinweise auf Oberflächensegregation. Au60Ag40-Drähte zeigen ungleichmäßig goldreiche Oberflächen, Au40Ag60 Nanodrähte hingegen zeigen Silberanreicherungen. Nach der selektiven Auflösung des Silbers bestehen die porösen goldreichen Nanodrähte aus 5 bis 30 nm breiten Ligamenten. Diese porösen Nanodrähte könnten künftig als Sensoren benutzt werden. Hierfür müssen allerdings der elektrische und thermische Wiederstand ermittelt werden. Um diese Messungen zu ermöglichen, wurden geeignete Kontaktierungsverfahren für AuAg- Nanodrähten mittels Laserlithographie getestet. Freistehende Gold-Nanokegel mit Mikrometer großen Basen und ca. 50 nm breiten Spitzen wurden elektrochemisch in Ionenspurmembranen mit asymmetrisch geätzten konischen Kanälen hergestellt. Stabile Nanokegel sind für Anwendungen interessant z.B. als hydrophobe Deckschicht oder als kalte Feldemitter. Die in dieser Arbeit hergestellten Gold-Nanokegel wurden VI | P a g e elektrochemisch von der Spitze zur Basis abgeschieden, um die mechanische Stabilität zu verbessern und einen soliden elektrischen und thermischen Kontakt zum Substrat sicherzustellen. Ein Test an geordneten Nanokegel-Arrays zeigt kalte Feldemission mit Feldüberhöhungen zwischen 200 und 1000 sowie maximalen Emissionsströmen zwischen 1 und 100 µA. Die Ergebnisse diese Promotionsarbeit verdeutlichen die große Flexibilität und unterschiedlichen Möglichkeiten der Ionenspur-Nanotechnologie. VII | P a g e Abstract Metallic nanostructures are attracting growing interest because of their potential application in various devices such as batteries, solar cells, or drug delivery systems. This thesis focuses on the synthesis and characterization of three different nanostructures: (1) solid cylindrical AuAg nanowires with controlled composition and size, fabricated by electrodeposition in etched ion-track membranes with cylindrical channels, (2) porous cylindrical Au nanowires attained by selective dealloying of AuAg nanowires, and (3) Au nanocones synthesized by electrodeposition in conical channels. AuAg nanowires with controlled diameter and composition, namely Au, Au40Ag60, Au60Ag40, and Ag were synthesized and characterized. By dealloying these nanowires were converted into porous Au-based nanowires with diameters above and below 100 nm possessing an enhanced surface area. Surface morphology and composition of the nanostructures before and after dealloying were studied by means of high spatial resolution energy-dispersive X-ray spectroscopy (EDX) in a high-resolution transmission electron microscope (TEM). The results demonstrate surface segregation effects in solid AuAg nanowires that strongly vary with the initial composition. Surface segregation occurs on a time scale of days (< 3 days) independently of the wire dimensions. After dealloying of Au40Ag60 nanowires, the porous nanowires have a silver content below 10% and ligament size from 5 to 30 nm. Solid and porous wires are particularly attractive for future applications, e.g., in sensorics. The characterization of such small nanostructures regarding, e.g. electrical transport properties, requires suitable contacts. Special designs to contact nanowires by laser lithography as well as by using pre-patterned templates were developed. Gold nanocones with sharp tips down to 50 nm diameter and several microns large bases were fabricated. Given by this special geometry, the nanostructures exhibit a high mechanical stability and are freestanding with an aspect ratio of 500 and above. Stable gold nanocone arrays are attractive for a large range of VIII | P a g e applications including field emission and as coating for hydrophobic surfaces. In this work, the standard wire deposition process from base to tip was inverted in order to improve the electrical and thermal contact of the nanocones to the substrate. After selective removal of the template, 30 µm long gold nanocones with ~ 50 nm sharp tips were freestanding and vertically aligned. Such structures are highly tunable in terms of cone dimensions and number density. The field emission properties of patterned nanocone arrays, investigated in collaboration with the Bergische Universität Wuppertal, exhibit field enhancement factors between 200 and 1000 as well as a maximum emission current ranging from ~ 1 to 100 μA. The results presented in this thesis emphasize the variety of possibilities that ion- track technology offers in order to tailor dimensions and characteristics of nanostructures. IX | P a g e Résumé L’intérêt croissant pour les nanotechnologies et plus particulièrement les nanostructures métalliques provient des besoins de nouveaux développements technologiques dans le domaine des batteries, des panneaux solaires ou en médecine. Cette thèse aborde la fabrication et la caractérisation de trois différentes structures à base d’or: (1) des nano-fils en alliage or et argent (AuAg), (2) des nano-fils poreux obtenus par la dissolution sélective de l’argent contenu dans des fils AuAg, et (3) des nano-cônes en or. Ces structures ont été synthétisées par électrodéposition dans des pores calibrés de membranes polymères. Elles ont été obtenues par révélation chimique des traces latentes laissées dans le matériau après irradiation par des ions lourds accélérés (plus connus sous le nom anglais « ion-track technology »). Cette technique permet de contrôler précisément le diamètre et la composition des nano-fils d’alliage or-argent. La dissolution de l’argent contenu dans des fils de composition Au40Ag60 par corrosion sélective rend possible l’obtention de nano- fils poreux. L’évolution de la morphologie et de la composition de ces nano-fils a été étudiée par microscopie électronique en transmission couplée à une analyse dispersive en énergie (EDX) avant et après traitement corrosif. Avant la dissolution de l’argent, les nano-fils sont cylindriques, mais leur composition n’est pas homogène. Une ségrégation de surface se produit au bout de quelques jours (< 3 jours). Les nano-fils de composition Au60Ag40 voient leur surface enrichie en or et, à l’inverse, celle des fils Au40Ag60 s’enrichie en argent. Après le traitement corrosif, seuls les fils comportant le plus d’argent (Au40Ag60) permettent la fabrication de nano-fils poreux, donnant lieu à une augmentation de leur surface. De tels fils sont particulièrement intéressants pour le développement de détecteurs ultra-sensibles. A cette fin, leurs propriétés électriques et thermiques doivent
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