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1.  Efficient electron-induced removal of oxalate ions and formation of copper nanoparticles from copper(II) oxalate precursor layers 
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.
PMCID: PMC4979688  PMID: 27547602
copper(II) oxalate; electron-induced reactions; layer-by-layer deposition; nanoparticle formation; thin film
2.  Focused particle beam-induced processing 
PMCID: PMC4660902  PMID: 26665058
3.  Imaging of carbon nanomembranes with helium ion microscopy 
Carbon nanomembranes (CNMs) prepared from aromatic self-assembled monolayers constitute a recently developed class of 2D materials. They are made by a combination of self-assembly, radiation-induced cross-linking and the detachment of the cross-linked SAM from its substrate. CNMs can be deposited on arbitrary substrates, including holey and perforated ones, as well as on metallic (transmission electron microscopy) grids. Therewith, freestanding membranes with a thickness of 1 nm and macroscopic lateral dimensions can be prepared. Although free-standing CNMs cannot be imaged by light microscopy, charged particle techniques can visualize them. However, CNMs are electrically insulating, which makes them sensitive to charging. We demonstrate that the helium ion microscope (HIM) is a good candidate for imaging freestanding CNMs due to its efficient charge compensation tool. Scanning with a beam of helium ions while recording the emitted secondary electrons generates the HIM images. The advantages of HIM are high resolution, high surface sensitivity and large depth of field. The effects of sample charging, imaging of multilayer CNMs as well as imaging artefacts are discussed.
PMCID: PMC4578422  PMID: 26425423
2D materials; carbon nanomembrane; helium ion microscopy; self-assembled monolayers
4.  Fabrication of carbon nanomembranes by helium ion beam lithography 
The irradiation-induced cross-linking of aromatic self-assembled monolayers (SAMs) is a universal method for the fabrication of ultrathin carbon nanomembranes (CNMs). Here we demonstrate the cross-linking of aromatic SAMs due to exposure to helium ions. The distinction of cross-linked from non-cross-linked regions in the SAM was facilitated by transferring the irradiated SAM to a new substrate, which allowed for an ex situ observation of the cross-linking process by helium ion microscopy (HIM). In this way, three growth regimes of cross-linked areas were identified: formation of nuclei, one-dimensional (1D) and two-dimensional (2D) growth. The evaluation of the corresponding HIM images revealed the dose-dependent coverage, i.e., the relative monolayer area, whose density of cross-links surpassed a certain threshold value, as a function of the exposure dose. A complete cross-linking of aromatic SAMs by He+ ion irradiation requires an exposure dose of about 850 µC/cm2, which is roughly 60 times smaller than the corresponding electron irradiation dose. Most likely, this is due to the energy distribution of secondary electrons shifted to lower energies, which results in a more efficient dissociative electron attachment (DEA) process.
PMCID: PMC3943867  PMID: 24605285
carbon nanomembranes; dissociative electron attachment; helium ion microscopy; ion beam-organic molecules interactions; self-assembled monolayers
5.  Mechanical characterization of carbon nanomembranes from self-assembled monolayers 
This paper reports on the mechanical characterization of carbon nanomembranes (CNMs) with a thickness of 1 nm that are fabricated by electron-induced crosslinking of aromatic self-assembled monolayers (SAMs). A novel type of in situ bulge test employing an atomic force microscope (AFM) is utilized to investigate their mechanical properties. A series of biphenyl-based molecules with different types of terminal and/or anchor groups were used to prepare the CNMs, such as 4'-[(3-trimethoxysilyl)propoxy]-[1,1'-biphenyl]-4-carbonitrile (CBPS), 1,1'-biphenyl-4-thiol (BPT) and 4-nitro-1,1'-biphenyl-4-thiol (NBPT). The elastic properties, viscoelastic behaviors and ultimate tensile strength of these biphenyl-based CNMs are investigated and discussed.
PMCID: PMC3257509  PMID: 22259767
bulge test; carbon nanomembrane; mechanical characterization; self-assembled monolayers; two-dimensional materials

Results 1-5 (5)