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Efficient electron-induced removal of oxalate ions and formation of copper nanoparticles from copper(II) oxalate precursor layers

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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.

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XP spectra in the ranges Cu 2p, O 1s, and C 1s recorded before (pristine) and after (irradiated) an electron exposure of 16000 μC/cm2 at 50 eV of surface grown copper(II) oxalate prepared by performing four deposition cycles. The sample was grown on a MUA-coated gold substrate.
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Figure 8: XP spectra in the ranges Cu 2p, O 1s, and C 1s recorded before (pristine) and after (irradiated) an electron exposure of 16000 μC/cm2 at 50 eV of surface grown copper(II) oxalate prepared by performing four deposition cycles. The sample was grown on a MUA-coated gold substrate.

Mentions: Fig. 8 shows the XPS spectra in the Cu 2p, O 1s, and C 1s ranges recorded prior to and after electron exposure. The XPS data are summarized and compared to literature values in Table 1. The as-prepared sample reveals two C 1s peaks at 284.5 eV, attributed to the aliphatic carbon chain of the underlying MUA SAM, and at 289.1 eV characteristic of carboxylic carbon [34] and thus assigned to the oxalate linker and to minor contributions of the MUA SAM. After irradiation, the peak at 289.1 eV nearly disappears confirming the decomposition of the oxalate linker and possibly also the decomposition of the terminal group of the underlying MUA SAM. The other signal shows a minor shift to a higher binding energy, which may relate to the overlap of the original signal with some amount of alcoholic or ether-type molecular units [35] formed by oxidation of the alkane chains in the underlying SAM.


Efficient electron-induced removal of oxalate ions and formation of copper nanoparticles from copper(II) oxalate precursor layers
XP spectra in the ranges Cu 2p, O 1s, and C 1s recorded before (pristine) and after (irradiated) an electron exposure of 16000 μC/cm2 at 50 eV of surface grown copper(II) oxalate prepared by performing four deposition cycles. The sample was grown on a MUA-coated gold substrate.
© Copyright Policy - Beilstein
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC4979688&req=5

Figure 8: XP spectra in the ranges Cu 2p, O 1s, and C 1s recorded before (pristine) and after (irradiated) an electron exposure of 16000 μC/cm2 at 50 eV of surface grown copper(II) oxalate prepared by performing four deposition cycles. The sample was grown on a MUA-coated gold substrate.
Mentions: Fig. 8 shows the XPS spectra in the Cu 2p, O 1s, and C 1s ranges recorded prior to and after electron exposure. The XPS data are summarized and compared to literature values in Table 1. The as-prepared sample reveals two C 1s peaks at 284.5 eV, attributed to the aliphatic carbon chain of the underlying MUA SAM, and at 289.1 eV characteristic of carboxylic carbon [34] and thus assigned to the oxalate linker and to minor contributions of the MUA SAM. After irradiation, the peak at 289.1 eV nearly disappears confirming the decomposition of the oxalate linker and possibly also the decomposition of the terminal group of the underlying MUA SAM. The other signal shows a minor shift to a higher binding energy, which may relate to the overlap of the original signal with some amount of alcoholic or ether-type molecular units [35] formed by oxidation of the alkane chains in the underlying SAM.

View Article: PubMed Central - HTML - PubMed

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.

No MeSH data available.


Related in: MedlinePlus