Abstract
Copper(II) oxalate grown on carboxy-terminated self-assembled monolayers (SAM) using a step-by-step approach was used as precursor for the electron-induced synthesis of surface-supported copper nanoparticles. The precursor material was deposited by dipping the surfaces alternately in ethanolic solutions of copper(II) acetate and oxalic acid with intermediate thorough rinsing steps. The deposition of copper(II) oxalate and the efficient electron-induced removal of the oxalate ions was monitored by reflection absorption infrared spectroscopy (RAIRS). Helium ion microscopy (HIM) reveals the formation of spherical nanoparticles with well-defined size and X-ray photoelectron spectroscopy (XPS) confirms their metallic nature. Continued irradiation after depletion of oxalate does not lead to further particle growth giving evidence that nanoparticle formation is primarily controlled by the available amount of precursor.
Highlights
Electron-induced chemistry is a versatile approach to the fabrication of nanoscale materials and devices
In close agreement with earlier results [26], spectra recorded after oxalic acid dipping steps (Figure 1a) show four bands in the range between 600 and 1800 cm−1, which can be assigned to characteristic vibrations of the oxalate anions
Between the acquisitions of spectra the samples investigated by reflection absorption infrared spectroscopy (RAIRS) were introduced in a dedicated UHV chamber with base pressure of 1 × 10−8 mbar and irradiated using an electron flood-gun (FG15/40, Specs), which generates a sufficiently divergent beam to grant a uniform irradiation of the samples
Summary
Electron-induced chemistry is a versatile approach to the fabrication of nanoscale materials and devices. Using a tightly focused beam, structures of arbitrary shape with dimensions in the nanometer regime can be directly written on surfaces. In such focused electron beam induced deposition (FEBID) [1,2] solid materials are produced on surfaces through decomposition of volatile precursor compounds under the electron beam [1,3,4]. As an alternative to deposition from the gas phase, FEBID has recently been performed in micrometer-thin films of molten metal salts [5] or in aqueous precursor solutions [6,7,8].
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