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Morphology and plasmonic properties of self-organized arrays of ...

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40 CHAPTER 2. EXPERIMENTAL METHODSturbomolecularpumpsample holderAu crucible60° 60°LiF effusion cellFigure 2.1: Sketch <strong>of</strong> the experimental chamber (front view). The LiF effusion cell <strong>and</strong>the Au crucible are visible. The sample holder can rotate <strong>and</strong> translate in the plane <strong>of</strong>the figure for the fine positioning during the MBE depositions.The deposition <strong>of</strong> insulating or metallic films is performed by means <strong>of</strong> the molecularbeam epitaxy (MBE) technique, which allows the formation <strong>of</strong> high quality crystallinefilms <strong>and</strong> nanostructures.The LiF source is composed by a boron nitride (h-BN) crucible, in which LiF lumpmaterial to be deposited is loaded. h-BN is a ceramic material with the same layeredstructure <strong>of</strong> graphite, from which it is sometimes called white graphite; it has a lowerelectric conductance with respect to graphite, but its thermal <strong>and</strong> chemical stability aremuch superior. The crucible is supported by a W filament, that also serves to its heatingbyJouleeffect. Itreachesatemperature<strong>of</strong>≈ 700 ◦ C,sufficienttopromotethesublimation<strong>of</strong> the lump LiF crystals (the melting point <strong>of</strong> LiF is at 845 ◦ C). A screen <strong>of</strong> tantalum isused as collimator for the molecular beam <strong>and</strong> to prevent the chamber contamination <strong>and</strong>selectively expose the sample to the beam. The LiF source can achieve deposition ratesup to at least 6 nm/min, at base pressure in the 10 −7 mbar range. For this thesis, typicalrates <strong>of</strong> 1 nm/min were chosen, as explained in more detail in the next chapter. Thethickness <strong>of</strong> the deposited LiF layer was calibrated by ex-situ optical characterization.The Au source requires instead a different configuration, because <strong>of</strong> the higher Aumelting point (1068 ◦ C) <strong>and</strong> relatively low vapour pressure. In this case short sections<strong>of</strong> pure gold wires (99.99%, MaTecK) are stored in a crucible <strong>of</strong> molybdenum, which isthen heated by electron bombardment applying an high voltage with respect to a hotW filament. The crucible is supported by an alumina rod, which grants a good thermalinsulation, <strong>and</strong> an additional copper screen is used both as collimator <strong>and</strong> thermal shield.The Au evaporator allowed to achieve evaporation rates in the 0.4÷0.7 nm/min range,applying an overall power <strong>of</strong> ≈ 40 W to the Mo crucible. Typical pressures during growthwere in the 10 −7 mbar range, that, though high, were perfectly acceptable due to the lowreactivity <strong>of</strong> the involved material.Although the characterization <strong>of</strong> the samples is typically performed mostly ex-situ,it is possible to perform reflectivity measurements by means <strong>of</strong> an optical setup. The

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