The electronic structure and chemistry of interfaces between tris-(8-hydroxyquinoline) aluminum (Alq3) and representative group IA and IIA metals, Al, and Al/LiF have been studied by x-ray and ultraviolet photoelectron spectroscopies. Quantum-chemical calculations at the density functional theory level predict that the Alq3 radical anion is formed upon reaction with the alkali metals. In this case, up to three metal atoms can react with a given Alq3 molecule to form the trivalent anion. The anion formation results in a splitting of the N 1s core level and formation of a new feature in the previously forbidden energy gap. Virtually identical spectra are observed in the Al/LiF/Alq3 system, leading to the conclusion that the radical anion is also formed when all three of these constituents are present. This is support by a simple thermodynamic model based on bulk heats of formation. In the absence of LiF or similar material, the reaction of Al with Alq3 appears to be destructive, with the deposited Al reacting directly with the quinolate oxygen. We proposed that in those circumstances where the radical anion is formed, it and not the cathode metal are responsible for the electron injection properties. This is borne out by producing excellent injecting contacts when Ag and Au are used as the metallic component of the cathode structure.
We report on the chemical adsorption of acids and bases on indium tin oxide (ITO). Ultraviolet photoelectron spectroscopy was used to measure the work function of the treated ITO and atomic surface concentrations were determined by x-ray photoelectron spectroscopy. The acid treatments yield work-function shifts as high as 0.7 eV compared to the nontreated ITO. Huge shifts in the work function are also obtained for the treatments with bases and are opposite to those obtained with the acids. These dramatic shifts are indicative of a double ionic surface layer. The importance of an appropriate plasma treatment prior to the chemical adsorption of acids or bases is discussed in terms of surface acido-basicity.
The influence of the indium tin oxide (ITO) electrode surface acido basicity on organic electroluminescent device characteristics is studied. As measured by photoelectron spectroscopy, acid and base treatments produce large work function shifts of the oxide compared to standard ITO treated by an oxygen plasma or water. The current onsets for triphenyldiamine (TPD) single layer diodes sandwiched between ITO and a silver electrode are in qualitative agreement with the work function of the hole injecting oxide electrode. However, saturated photovoltage measurements on single layer diodes built on acid and water treated ITO disagree with the work function obtained from photoelectron experiments. This is explained by protonation of the diamine layer close to the electrode surface producing a charged double layer. It suggests that even acidic surface hydroxyl groups of the oxide electrode are able to protonate the diamine layer, explaining the importance of plasma cleaning to remove surface hydroxyls. The same ITO treatments are investigated in tris(8-hydroxyquinoline) (Alq) aluminum single layer diodes as well as hybrid TPD/Alq light emitting devices. Implications of metal–oxide surface acido basicity on electrode treatment and molecular material design are discussed.
As an interconnect material, copper has the disadvantage of not forming self-limiting oxides, which can negatively affect device performance and reliability. Undesired oxide layers need to be removed by in situ cleaning, before the copper is subjected to subsequent depositions. We have used ethyl alcohol (C 2 H 5 OH) as a vapor phase reducing agent to remove copper oxides formed on electroplated copper films upon exposure to the ambient. Spectroscopic ellipsometry has been used to monitor the reduction process in situ. Ex situ characterization using X-ray photoelectron spectroscopy and atomic force microscopy support in situ measurements. While oxide removal can be achieved at temperatures as low as 130°C, independent of oxide layer thickness and composition, it occurred more efficiently at 200°C, showing compatibility with the low temperature (Ͻ400°C) processing requirements of low dielectric constant materials. The initial reaction involves the reduction of Cu 2ϩ to Cu ϩ species followed by a second phase consisting of Cu ϩ conversion to elemental copper, producing a clean metal surface. Reduction of Cu 2ϩ to Cu ϩ species is the rate-limiting step as evidenced by enhanced sensitivity to the reaction temperature.
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