Abstract
In the present study, we have synthesised and characterised newly copper(II) complexes with the general formula [Cu2(NH2(NH=)CC2F5)2(µ–O2CRF)4], where RF = CF3, C2F5, C3F7, C4F9. Infrared spectroscopy, mass spectrometry with electron ionisation (EI MS), and density-functional theory (DFT) calculations were used to confirm compounds’ composition and structure. The volatility of the compounds was studied using thermal analysis (TGA), EI MS mass spectrometry, variable temperature infrared spectroscopy (VT IR), and sublimation experiments. Research has revealed that these compounds are the source of metal carriers in the gas phase. The thermal decomposition mechanism over reduced pressure was proposed. TGA studies demonstrated that copper transfer to the gaseous phase occurs even at atmospheric pressure. Two selected complexes [Cu2(NH2(NH=)CC2F5)2(µ–O2CC2F5)4] and [Cu2(NH2(NH=)CC2F5)2(µ–O2CC3F7)4] were successful used as chemical vapour deposition precursors. Copper films were deposited with an evaporation temperature of 393 K and 453 K, respectively, and a decomposition temperature in the range of 573–633 K without the use of hydrogen. The microscopic observations made to investigate the interaction of the [Cu2(NH2(NH=)CC2F5)2(µ–O2CC2F5)4] with the electron beam showed that the ligands are completely lost under transmission electron microscopy analysis conditions (200 keV), and the final product is copper(II) fluoride. In contrast, the beam energy in scanning electron microscopy (20 keV) was insufficient to break all coordination bonds. It was shown that the Cu-O bond is more sensitive to the electron beam than the Cu-N bond.
Highlights
Nowadays, copper compounds are used, for example, to design hybrid organicinorganic materials [1,2,3], anticancer agents [4,5], and sensors [6,7]
Copper nanostructures are used, for example, in electronics [11,12,13], plasmonics [14,15], catalysis [16,17,18], and as antibacterial agents [19,20]. These structures can be obtained by gas-assisted methods such as chemical vapour deposition (CVD) [21,22,23]
In focused electron beam induced deposition (FEBID), the precursor is supplied without the use of carrier gas, the adsorbed compound is dissociated in the focus of an electron beam provided by a scanning or transmission electron microscope (SEM/transmissionelectron electronmicroscope microscope (TEM)) [28]
Summary
Copper compounds are used, for example, to design hybrid organicinorganic materials [1,2,3], anticancer agents [4,5], and sensors [6,7]. Copper nanostructures are used, for example, in electronics [11,12,13], plasmonics [14,15], catalysis [16,17,18], and as antibacterial agents [19,20] These structures can be obtained by gas-assisted methods such as chemical vapour deposition (CVD) [21,22,23]. CVD is a process where one or more volatile precursors are transported in the vapour carrier gas to the reactor chamber, where they decompose on a heated substrate and deposit a solid material [27].
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