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www.nature.com/scientificreports/ Figure 3. FT-IR spectra of (a) MNPs, (b) SMNPs, (c) ASMNPs, (d) ABF@ASMNPs and (e) Cu-ABF@ ASMNPs. surface of SMNPs was confirmed by the emergence of new peaks at 1623 cm−1 and 2926 cm−1 which are assigned to the primary amine (-NH2) group and methylene (CH2) groups respectively (Fig. 3c). By comparing the spectra of ABF@ASMNPs (Fig. 3d) with those of ASMNPs, it is observed that after the Schiff condensation reaction the characteristic peak of imine group (C=N) appears at 1655 cm–1. On metalation, it is observed that the absorption at 1655 cm−1 shifted to 1647 cm−1 which confirms that copper is successfully anchored onto the surface of ABF@ ASMNPs (Fig. 3e)71–74. Transmission electron microscopy (TEM) and field emission scanning electron microscopy analysis (FE-SEM). TEM micrograph of MNPs indicates that it is composed of tiny particles possessing the spherical morphology (Fig. 4a). Selected area electron diffraction (SAED) pattern of the MNPs is displayed as an inset in Fig. 4e. The white spots as well as the bright diffraction rings signify that the nanoparticles synthesised by the above-stated process are highly crystalline. The size distribution diagram of these nanoparticles shows that the average particle size of MNPs is in the range of 6–8 nm (see Supplementary Fig. S2). TEM image of SMNPs depicts the discrete core structure of MNPs of diameter of 6–8 nm encapsulated within the silica layer of 4–7 nm (Fig. 4b). Further, the TEM image of final Cu-ABF@ASMNPs nanocatalyst is demonstrated in Fig. 4c. The mor- phology of Cu-ABF@ASMNPs is characterized by FE-SEM as well. Fig. 4d clearly reveals that the catalyst is spherical in shape. Elemental mapping. Elemental mapping of the final Cu-ABF@ASMNPs catalyst is shown in Fig. 5a–f. The figures clearly reveal that Cu NPs dispersed uniformly on the surface of silica-based magnetite nano supports as mentioned in Fig. 1. The quantitative determination of the copper content was performed by the ICP-OES and was found to be 1.32 mmol/g in the final catalyst. X-ray photoelectron spectroscopy (XPS). The chemical loading of the copper and its chemical state of copper in final catalyst as well as reused catalyst after 5 consecutive cycles was were measured by XPS technique, the spectrum is depicted in Fig. 6a,b. In both the samples the presence of Cu2p3/2 and Cu2p1/2 having binding energies 933.4 eV and 953.6 eV respectively along with the corresponding satellite bands having binding energies 940.9 eV, 943.4 eV and 962.1 eV confirm the presence of copper having 2+ oxidation state75,76. Further the survey spectra confirm the presence of silica, carbon and oxygen on the surface proves the coating of magnetic nanopar- ticles (see Supplementary Fig. S4). Vibrating sample magnetometer (VSM). The magnetic properties of MNPs, SMNPs and Cu-ABF@ ASMNPs catalyst were thoroughly studied using vibrating sample magnetometry at room temperature (Fig. 7). The curves show decrease in the saturation magnetization (Ms) values from MNPs (58 emu/g) to SMNPs (36 emu/g) to the final Cu-ABF@ASMNPs nanocatalyst (26 emu/g). This decrease can be attributed to the pres- ence of non-magnetic silica and other functionalised groups onto the surface of MNPs. Although the Ms values have decreased sequentially, the obtained nanocatalyst can be effortlessly removed from the reaction media via an external magnet. The curves also exhibit no hysteresis loop which indicates the superparamagnetic nature of these nanoparticles. Besides, this behaviour can be confirmed from the figure given in inset which shows negligi- ble coercivity and remanence. This implies that as soon as the applied magnetic field is removed, the NPs would retain no residual magnetism, thereby making MNPs good candidates for catalytic support77. Catalytic activity of Cu-ABF@ASMNPs for cycloaddition reaction. Herein, the catalytic effi- ciency of copper-based magnetic nanocatalyst was investigated using styrene oxide as model substrate (Fig. 8). The screening of organic bases, solvents and amount of catalyst was carried out with optimised temperature and reaction time. Recently, organic bases have attracted widespread interest as CO2 activators which form the zwitterionic adduct, an activated form of CO2. We envisaged that assistance of these bases including DBU SCientifiC RepoRts | (2018) 8:1901 | DOI:10.1038/s41598-018-19551-3 4PDF Image | copper-based magnetic nanocatalyst for the fixation of carbon dioxide
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