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XXVIII Congress of the Analytical Chemistry Division Bari 22 – 26 September 2019 O6 AS2 ELECTRODECORATION AND ANALYTICAL CHARACTERIZATION OF IRON OXIDE NANOPARTICLES WITH BIOACTIVE NANOPHASES FOR TARGETED ANTIMICROBIAL MATERIALS N. Ditaranto 1 , M. Salvador 2,3 , A. Moyano 4 , V. Marchianò 1 , M. Sportella 1 , J.C. Martínez- García 2 , M. Rivas 2 , M.C. Blanco-López 4 , N. Cioffi 1 1 Dipartimento di Chimica, Università degli Studi di Bari Aldo Moro, Bari, Italy 2 Department of Physics, IUTA, University of Oviedo, Spain 3 Istituto di Struttura della Materia-CNR, Monterotondo Scalo (RM), Italy 4 Department of Physical and Analytical Chemistry, University of Oviedo, Oviedo, Spain Magnetic iron oxide nanoparticles Fe₃O₄ (MNPs) are well known in the oncology field, being used for diagnostic and therapeutic purposes. Indeed, their superparamagnetic properties are exploited to cause the death of cancer cells due to hyperthermia [1,2]. In our work, aiming at exploiting the characteristics of MNPs in a synergistic way with the antibacterial action provided by copper nanoparticles (CuNPs), we have investigated the electrodecoration of iron oxide MNPs by CuNPs [3]. All the magnetic nanoparticles were synthetized via co-precipitation of Fe 2+ and Fe 3+ salts in aqueous media, either naked or capped in-situ by polyacrylic acid (PAA) or polyethylenimine (PEI) [4,5]. The Sacrificial Anode Electrolysis (SAE) method [6] has been used to electrodecorate these MNPs in an electrochemical cell, using tetrabutyl ammonium chloride (TBAC) or benzyl dimethyl hexadecyl ammonium chloride (BDHAC) as electrolytes. All the nanomaterials were characterized by UV-visible Spectrophotometry, Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). Magnetite nanoparticles Fe₃O₄ are a mixture of ferric and ferrous anions in a 2:1 ratio. A detailed surface chemical investigation was performed to identify the Fe 2+ and Fe 3+ features present in the XPS peaks. Since the main XP photoelectron Fe2p peak is well known to be a very complex system, a combined study of both secondary peaks (Fe3p) and valence band region (VB) was performed. In particular, the VB shape is considered a kind of “fingerprint” of magnetite composition. Moreover, in many studies the peak position of Fe2p 3/2 with respect to the satellite peak [7] along with the shape of valence band [8] are accounted for differentiating Fe oxidation state, that is ferrous and ferric oxide. According to the literature, MNPs low stability in air led to maghemite (γ-Fe 2 O 3 ) formation, ending up with a Fe 3 O 4 -Fe 2 O 3 core−shell structure. Moreover, surface spectroscopy and morphological analyses demonstrated that interactions between the different nanophases occurred in composite materials, since the resulting nanomaterials both retain the MNPs magnetic properties and reveal new spectroscopic features in the valence band region of modified magnetite compared to the bare sample (Figs. 1a, 1b).
Transcript of K ò ^ î > dZK KZ d/KE E E >zd/ > , Z d Z/ d/KE K& /ZKE Ky ...barianalitica2019.it/doc/O6...
![Page 1: K ò ^ î > dZK KZ d/KE E E >zd/ > , Z d Z/ d/KE K& /ZKE Ky ...barianalitica2019.it/doc/O6 AS2_Ditaranto_Nicoletta.pdf · D ] o Æ U î ì í ñ U ñ U í ó í X ó ' }](https://reader034.fdocuments.us/reader034/viewer/2022042208/5eab5c51b2e42008766625ac/html5/thumbnails/1.jpg)
XXVIII Congress of the Analytical Chemistry Division Bari 22 – 26 September 2019
O6 AS2
ELECTRODECORATION AND ANALYTICAL CHARACTERIZATION OF IRON OXIDE NANOPARTICLES WITH BIOACTIVE NANOPHASES FOR TARGETED ANTIMICROBIAL MATERIALS
N. Ditaranto1, M. Salvador2,3, A. Moyano4, V. Marchianò1, M. Sportella1, J.C. Martínez-García2, M. Rivas2, M.C. Blanco-López4, N. Cioffi1 1Dipartimento di Chimica, Università degli Studi di Bari Aldo Moro, Bari, Italy 2Department of Physics, IUTA, University of Oviedo, Spain 3Istituto di Struttura della Materia-CNR, Monterotondo Scalo (RM), Italy 4Department of Physical and Analytical Chemistry, University of Oviedo, Oviedo, Spain
Magnetic iron oxide nanoparticles Fe₃O₄ (MNPs) are well known in the oncology field, being used for diagnostic and therapeutic purposes. Indeed, their superparamagnetic properties are exploited to cause the death of cancer cells due to hyperthermia [1,2]. In our work, aiming at exploiting the characteristics of MNPs in a synergistic way with the antibacterial action provided by copper nanoparticles (CuNPs), we have investigated the electrodecoration of iron oxide MNPs by CuNPs [3]. All the magnetic nanoparticles were synthetized via co-precipitation of Fe2+ and Fe3+ salts in aqueous media, either naked or capped in-situ by polyacrylic acid (PAA) or polyethylenimine (PEI) [4,5]. The Sacrificial Anode Electrolysis (SAE) method [6] has been used to electrodecorate these MNPs in an electrochemical cell, using tetrabutyl ammonium chloride (TBAC) or benzyl dimethyl hexadecyl ammonium chloride (BDHAC) as electrolytes. All the nanomaterials were characterized by UV-visible Spectrophotometry, Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). Magnetite nanoparticles Fe₃O₄ are a mixture of ferric and ferrous anions in a 2:1 ratio. A detailed surface chemical investigation was performed to identify the Fe2+ and Fe3+ features present in the XPS peaks. Since the main XP photoelectron Fe2p peak is well known to be a very complex system, a combined study of both secondary peaks (Fe3p) and valence band region (VB) was performed. In particular, the VB shape is considered a kind of “fingerprint” of magnetite composition. Moreover, in many studies the peak position of Fe2p3/2 with respect to the satellite peak [7] along with the shape of valence band [8] are accounted for differentiating Fe oxidation state, that is ferrous and ferric oxide. According to the literature, MNPs low stability in air led to maghemite (γ-Fe2O3) formation, ending up with a Fe3O4-Fe2O3
core−shell structure. Moreover, surface spectroscopy and morphological analyses demonstrated that interactions between the different nanophases occurred in composite materials, since the resulting nanomaterials both retain the MNPs magnetic properties and reveal new spectroscopic features in the valence band region of modified magnetite compared to the bare sample (Figs. 1a, 1b).
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XXVIII Congress of the Analytical Chemistry Division Bari 22 – 26 September 2019
O6 AS2
UV-vis and magnetic measurements are in progress, as well as the assessment of the antibacterial effects of the nanocomposite materials.
Figure 1. TEM images at different magnifications of BDHAC stabilised CuNPs@Fe₃O₄ (a) and XP valence band spectra comparison of naked and CuNPs@Fe₃O₄ samples (b).
References [1] Deatsch A.E., Evans B.A., Journal of Magnetism and Magnetic Materials, 2014, 354, 163. [2] Céspedes, E., Byrne, J. M., Farrow, N., Moise, S., Coker, V. S., Bencsik, M., Telling, N. D. Nanoscale, 2014, 6, 12958. [3] Cioffi N., Torsi L., Ditaranto N., Tantillo G., Ghibelli L., Sabbatini L., Bleve-Zacheo T., D'Alessio M., Zambonin P. G., Traversa E., Chemistry of Materials, 2005, 17, 5255. [4] Ahn, T., Kim, J. H., Yang, H. M., Lee, J. W., & Kim, J. D., Journal of Physical Chemistry C, 2012, 116, 6069. [5] Wu W., Wu Z., Yu T., Jiang C., Kim W.S., Science and Technology of Advanced Materials, 2015, 16, 023501. [6] Afzal A., Di Franco C., Mesto E., Ditaranto N., Cioffi N., Scordari F., Scamarcio G., Torsi L., Materials Express, 2015, 5, 171. [7] Grosvenor, A. P., Kobe, B. A., Biesinger, M. C., McIntyre, N. S., Surface and Interface Analysis, 2004, 36, 1564. [8] McIntyre N.S., Zetaruk D.G., Anaytical Chemistry, 1977, 49, 1521.
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