Solution-processed transparent electrodes from metal oxide nanocrystals for thin film optoelectronics
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1 Research Collection Doctoral Thesis Solution-processed transparent electrodes from metal oxide nanocrystals for thin film optoelectronics Author(s): Luo, Li 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 Solution-processed Transparent Electrodes from Metal Oxide Nanocrystals for Thin Film Optoelectronics A dissertation submitted to ETH ZURICH for the degree of Doctor of Sciences presented by LI LUO MSc. ETH ZURICH born January 21, 1983 citizen of China accepted on the recommendation of Prof. Dr. Markus Niederberger, examiner Prof. Dr. Vanessa Wood, co-examiner Prof. Dr. Maksym Kovalenko, co-examiner 2013
3 Abstract The aim of this PhD work is to use metal oxide nanocrystals, including aluminum doped zinc oxide (AZO), tin doped zinc oxide (TZO), antimony doped tin oxide (ATO) and indium tin oxide (ITO), as building blocks to form high performance transparent conducting oxide (TCO) films which can be applied to optoelectronic devices by solution processes. AZO nanoparticles with different doping levels are synthesized by a microwave-assisted non-aqueous sol-gel route in benzyl alcohol and subsequently processed into transparent conducting films. The crystal structure, crystal size, shape and doping level of the nanoparticles are analyzed in detail by Rietveld refinement from powder X-ray diffraction (PXRD) data and transmission electron microscopy (TEM). Study of the thermal stability gives evidence that the material is thermally stable up to 600 C. Films are prepared on fused silica substrates by dipcoating from AZO nanoparticle dispersions, followed by a microwave-assisted densification step. According to scanning electron microscopy (SEM) and atomic force microscopy (AFM) measurements, the films are homogeneous over large areas with a root mean square roughness of about 10 nm. A minimum resistivity of Ω cm is achieved for a 357 nm thick AZO film with an initial Al-to-Zn mol ratio of 1:9 after post-annealing under N 2. The changes of the electrical properties of the films could be well explained on the basis of varying initial doping levels and crystal sizes of the nanoparticle building blocks. The average transmittance of the films in the visible light range is higher than 90 %, and especially for green light it reaches up to 95 %. TZO nanoparticles and films are synthesized by the same method used for AZO. Similar to AZO, the concentration of Sn has a great impact on the electrical properties of the films. A minimum resistivity of 20.3 Ω cm is obtained for a porous TZO film with initial Sn concentration of 7.5 mol% after annealing in air and post-annealing in N 2 at 600 C. The resistivity of this porous film could further be reduced to 2.6 Ω cm and 0.6 Ω cm after densification in TZO and AZO reaction solution, respectively. The average optical transmittance of a 400-nm-thick TZO film densified with TZO after the two annealing steps is 91 %. 3 nm diameter ATO nanocrystals with narrow size distrubituon, synthesized by an efficient microwave-assisted nonaqueous sol-gel method as well, are dispersed in tetrahydrofuran (THF) without any additives and processed into films by spin-coating on glass substrates. After thermal v
4 Abstract treatment, uniform and crack-free films with a low surface roughness of 1.6 nm and tunable thickness of 30 to 800 nm are obtained. A resistivity of Ω cm is achieved for a 480 nm thick ATO film with a high transparency of 90 % in the visible light range ( nm). To demonstrate that these films are indeed viable as transparent electrodes, an organic light emitting diode (OLED) is fabricated on this nanocrystal-based ATO electrode, and it exhibits an electrical and optical performance comparable to an OLED on a commercially available 150 nm thick indium tin oxide (ITO) film. ITO nanocrystals with sizes of 10 nm, also synthesized by microwave-assisted nonaqueous sol-gel route, are directly processed into a highly stable dispersion in toluene. Spin-coating of this dispersion results in ITO films with a surface roughness of 2.9 nm. After annealing at a low temperature (300 C for 3 h) in Ar mixed with 5 % of H 2, a resistivity of Ω cm is obtained for a 140 nm thick ITO film, and the average transmittance is up to 96 % in the visible light range. By increasing the temperature to 400 C, the resistivity reduces to Ω cm. Multiple stacking layers consisting of ITO and ATO nanocrystal films are obtained by alternating spin-coating of ITO and ATO dispersions. The microstructure and surface roughness of the individual layer maintains the same as the single composition films. The electrical properties of the multilayers depends on the individual layer of ITO and ATO, while the optical transmittance is tuned by different number of stacks, i.e. the transmittance of IAI in green light range is 98 %, and the transmittance of IAIAI in blue light range is over 99 %. The average transmittance in visible light range is still over 95 % when the number of stacks is up to seven layers (IAIAIAI). Simultaneous syntheses of metal oxide nanocrystals and deposition of their thin films by microwave-assisted nonaqueous sol-gel method are also tested. The influence of precursor concentration, type of substrates and reaction conditions on film formation are investigated. Continuous AZO films are obtained on Si(100) substrates, but it is rather difficult to get homogeneous films in a large area on glass substrates. Further improvement of this method is needed for TCO film deposition. vi
5 Zusammenfassung Ziel dieser Dissertation ist es, Metalloxid-Nanokristalle wie Aluminium-dotiertes Zinkoxid (AZO), Zinn-dotiertes Zinkoxid (TZO), Antimon-Zinnoxid (ATO) und Indium-Zinn-Oxid (ITO) als Bausteine zur Herstellung von hochleistungsfähigen, transparenten und leitfähigen Oxidfilmen (TCO) zu verwenden, welche wiederum für optoelektronische Bauteile in einem Flüssigphasenprozess verwendet werden können. AZO Nanopartikel mit unterschiedlicher Dotierung wurden durch eine Mikrowellen-unterstützte, nichtwässrige Sol-Gel-Methode in Benzylalkohol hergestellt und anschliessend zu transparenten, leitenden Filmen verarbeitet. Die Kristallstruktur, Kristallgrösse, Form und Dotierung der Nanopartikel wurde durch die Rietveld-Methode an Pulver-röntgenbeugungsdaten (PXRD) und Transmissionselektronenmikroskopie (TEM) detailliert untersucht. Die Untersuchung der thermischen Stabilität hat gezeigt, dass das Material bis 600 C stabil bleibt. Die Filme wurden durch Tauchbeschichtung von AZO Nanopartikel Dispersionen auf Quarzglassubstraten mit einem Mikrowellen-unterstützten Verdichtungsschritt hergestellt.gemäss Messungen mit dem Rasterelektronenmikroskop (REM) und dem Rasterkraftmikroskop (AFM) weisen die Filme über grosse Flächen eine quadratische Rauheit von etwa 10 nm auf. Ein minimaler Widerstand von Ω cm wurde für 357 nm dicke AZO Filme mit einem anfänglichen Al-zu-Zn mol Verhältnis von 1:9 erreicht, nachdem die Proben zusätzlich in einer N 2 Atmosphäre geglüht wurden. Die Änderungen der elektrischen Eigenschaften der Filme kann auch auf Grundlage der unterschiedlichen anfänglichen Dotierungen und Kristallgrössen der Nanopartikel-Bausteine erklärt werden. Die mittlere Transmission der Filme im Bereich des sichtbaren Lichts war grösser als 90 % und insbesondere für grünes Licht wurden bis zu 95 % erreicht. TZO Nanopartikel und Filme wurden durch das gleiche Verfahren wie für AZO synthetisiert. Ähnlich wie bei AZO hat die Konzentration von Sn einen grossen Einfluss auf die elektrischen Eigenschaften der Filme. Ein minimaler Widerstand von 20.3 Ω cm wurde für einen porösen TZO Film mit anfänglicher Sn-Konzentration von 7.5 mol% nach dem Glühen in Luft und anschliessend unter N 2 Atmosphäre bei 600 C erreicht. Der Widerstand dieses porösen Films konnte weiter auf 2.6 Ω cm und 0.6 Ω cm reduziert werden, nachdem die Proben in TZO und AZO Reaktionslösungen verdichtet wurden. Die durchschnittliche Transmission eines 400 nm dicken, mit TZO verdichtetentzp Films nach den beiden Glühbehandlungen beträgt 91 %. vii
6 Zusammenfassung 3 nm grosse ATO Nanokristalle mit enger Grössenverteilung wurden durch ein effizientes Mikrowellen-unterstütztes Sol-Gel-Verfahren synthetisiert, in Tetrahydrofuran (THF) ohne Additive dispergiert und anschliessend durch Rotationsbeschichtung auf Glassubstraten aufgetragen. Nach der thermischen Behandlung wurden gleichmässige und rissfreie Filme mit einer geringen Oberflächenrauhigkeit von 1.6 nm und mit einer gut kontrollierbaren Dicke von 30 bis 800 nm erhalten. Bei einem Widerstand von Ω cm für eine 480 nm dicken ATO Film wurde eine hohe Transmission von 90 % im Bereich des sichtbaren Lichts ( nm) erreicht. Um zu zeigen, dass sich diese Filme tatsächlich als transparente Elektroden eignen, wurde eine organische lichtemittierende Diode (OLED) aus diesen nanokristallinen ATO Elektroden hergestellt. Die elektrischen und optischen Eigenschaften dieser OLED waren mit jener 150 nm dicker, handelsüblicher Indium Zinn Oxid (ITO) Filmen vergleichbar. ITO Nanokristalle mit einem Durchmesser 10 nm wurden ebenfalls durch Mikro-wellenunterstützte nichtwässrige Sol-Gel-Synthese hergestellt und direkt zu stabilen Dispersionen in Toluol verarbeitet. Rotationsbeschichtung dieser Dispersionen führt zu ITO-Schichten mit einer Oberflächenrauheit von 2.9 nm. Nach dem Glühen bei niedriger Temperatur (300 C für 3 h) in Ar mit 5 % H 2, wurde ein spezifischer Widerstand von Ω cm für eine 140 nm dicke ITO Schicht gemessen. Die durchschnittliche Transmission im sichtbaren Bereich betrug bis zu 96 %. Durch Erhöhung der Temperatur auf 400 C reduziert sich der spezifische Widerstand auf Ω cm. Durch abwechselndes Rotationsbeschichten der ITO und ATO Dispersionen wurden mehrere Filme aus gestapelten Schichten aus nanokristallinem ITO und ATO produziert. Die Mikrostruktur und die Oberflächenrauhigkeit der einzelnen Schichten waren mit jenen einzelner Schichten vergleichbar. Die elektrischen Eigenschaften der Mehrfachschichten hängen von der individuellen Schicht aus ITO und ATO ab, während die optische Transmission durch die unterschiedliche Anzahl von Stapeln bestimmt ist, d.h. die Transmission von IAI im Bereich des grünen Lichts betrug 98 % und die Transmission von IAIAI im Bereich des blauen Lichts betrug über 99 %. Die durchschnittliche Transmission im sichtbaren Lichtbereich ist immer noch höher als 95 %, auch bei Stapeln von bis zu sieben Schichten (IAIAIAI). Simultane Synthesen von Metalloxid Nanokristallen und deren Abscheidung in dünne Schichten durch Mikrowellen-unterstützte Sol-Gel-Verfahren wurde ebenfalls untersucht. Der Einfluss der Precursorkonzentration, Substrattypen und Reaktionsbedingungen auf die Filmherstellung wurden untersucht. Kontinuierliche AZO Filme wurden auf Si(100) Substraten produziert, aber homogene Filme über grössere Flächen sind sehr schwierig herzustellen. Für die Abscheidung von TCO Schichten sind dazu weitere Fortschritte nötig. viii
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