Magnetic core/shell structures: A case study on the synthesis and phototoxicity/cytotoxicity tests of multilayer graphene encapsulated Fe/Fe3C nanoparticles

Sıddıka Mertdinç-Ülküseven; Kubra Onbasli; Ece Çakır; Yağız Morova; Özge Balcı-Çağıran; Havva Yagci Acar; Alphan Sennaroğlu; M. Lütfi Öveçoğlu; Duygu Ağaoğulları

doi:10.1016/j.jallcom.2023.172145

Magnetic core/shell structures: A case study on the synthesis and phototoxicity/cytotoxicity tests of multilayer graphene encapsulated Fe/Fe₃C nanoparticles

Sıddıka Mertdinç-Ülküseven^*, Kubra Onbasli, Ece Çakır, Yağız Morova, Özge Balcı-Çağıran, Havva Yagci Acar, Alphan Sennaroğlu, M. Lütfi Öveçoğlu, Duygu Ağaoğulları

^*Corresponding author for this work

Department of Metallurgical and Materials Engineering

Research output: Contribution to journal › Article › peer-review

4 Citations (Scopus)

Abstract

This study reports on a novel and optimized synthesis procedure of multilayer graphene (MLG) encapsulated Fe/Fe₃C nanoparticles using a combined method of spray drying, chemical vapor deposition (CVD) and leaching from FeCl₃.6 H₂O based precursor, in addition to phototoxicity/cytotoxicity tests for their potential use in biomedical applications. CVD studies were employed at various temperature/time and gas flow rate values. Based on the X-ray diffractometry (XRD), Raman spectroscopy, vibrating sample magnetometry (VSM), transmission electron microscopy/energy-dispersive spectroscopy (TEM/EDS) and differential thermal analysis/thermogravimetry (DTA/TG), CVD parameters of 900 °C, 60 min, 50 mbar and CH₄/H₂:1/1 were determined as optimum conditions. MLG encapsulated (D-spacing: 0.34 nm) nanoparticles consisting BCC Fe, FCC (Fe, C) and orthorhombic Fe₃C phases were obtained with average core diameter of ∼45 nm and average shell thickness of ∼6 nm (8–50 layers). MLG encapsulated Fe/Fe₃C nanoparticles were achieved with soft ferromagnetic (M_s: ∼64 emu/g; H_c: ∼276 Oe) property. MLG coated Fe/Fe₃C nanoparticles were suspended in an aqueous media using poly/acrylic acid as a post-synthetic treatment. They were found cytocompatible even at 200 µg/mL and 75 µg/mL after 24 and 48 h exposure, respectively. Dose dependent cytotoxicity was studied on both MCF7 and HeLa cells after 72 h incubation. Light-to-heat conversion efficiency of these nanoparticles at 795 nm irradiation in water was calculated as 37.60 %. After laser irradiation, with an increased concentration of nanoparticles (75–200 µg/mL), more than 80 % cell death was observed on both MCF7 and HeLa cells lines via late apoptotic cell death as a result of photothermal effect.

Original language	English
Article number	172145
Journal	Journal of Alloys and Compounds
Volume	968
DOIs	https://doi.org/10.1016/j.jallcom.2023.172145
Publication status	Published - 15 Dec 2023

Bibliographical note

Publisher Copyright:
© 2023 Elsevier B.V.

Funding

This study was financially supported by The Scientific and Technological Research Council of Turkey (TUBITAK) with the grant number: 118F430. This study was also partially financed by Istanbul Technical University Scientific Research Projects (ITU-BAP) with the grant number: MDK-2019-41863. The authors thank to Sedat Kurnaz from Kastamonu University for VSM analyses and to Sabancı University (SUNUM) for TEM analyses. Also, the authors thank to Dr. Gülsu Şimşek Franci (from KUYTAM) for her help in Raman analyses and to M.Sc. Aybike Paksoy (from KUBAM) for her help in DTA/TG analyses. This study was financially supported by The Scientific and Technological Research Council of Turkey (TUBITAK) with the grant number: 118F430 . This study was also partially financed by Istanbul Technical University Scientific Research Projects (ITU-BAP) with the grant number: MDK-2019-41863 . The authors thank to Sedat Kurnaz from Kastamonu University for VSM analyses and to Sabancı University (SUNUM) for TEM analyses. Also, the authors thank to Dr. Gülsu Şimşek Franci (from KUYTAM) for her help in Raman analyses and to M.Sc. Aybike Paksoy (from KUBAM) for her help in DTA/TG analyses.

Funders	Funder number
SUNUM
Türkiye Bilimsel ve Teknolojik Araştırma Kurumu	118F430
Istanbul Teknik Üniversitesi
Kastamonu Üniversitesi
Sabancı Üniversitesi
Bilimsel Araştırma Projeleri Birimi, İstanbul Teknik Üniversitesi	MDK-2019-41863

Keywords

Chemical vapor deposition
Core/shell magnetic nanoparticles
Magnetic/Thermal properties
Microstructure-final
Multilayer graphene
Phototoxicity/cytotoxicity

Access to Document

10.1016/j.jallcom.2023.172145

Cite this

Mertdinç-Ülküseven, S., Onbasli, K., Çakır, E., Morova, Y., Balcı-Çağıran, Ö., Acar, H. Y., Sennaroğlu, A., Lütfi Öveçoğlu, M., & Ağaoğulları, D. (2023). Magnetic core/shell structures: A case study on the synthesis and phototoxicity/cytotoxicity tests of multilayer graphene encapsulated Fe/Fe₃C nanoparticles. Journal of Alloys and Compounds, 968, Article 172145. https://doi.org/10.1016/j.jallcom.2023.172145

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abstract = "This study reports on a novel and optimized synthesis procedure of multilayer graphene (MLG) encapsulated Fe/Fe3C nanoparticles using a combined method of spray drying, chemical vapor deposition (CVD) and leaching from FeCl3.6 H2O based precursor, in addition to phototoxicity/cytotoxicity tests for their potential use in biomedical applications. CVD studies were employed at various temperature/time and gas flow rate values. Based on the X-ray diffractometry (XRD), Raman spectroscopy, vibrating sample magnetometry (VSM), transmission electron microscopy/energy-dispersive spectroscopy (TEM/EDS) and differential thermal analysis/thermogravimetry (DTA/TG), CVD parameters of 900 °C, 60 min, 50 mbar and CH4/H2:1/1 were determined as optimum conditions. MLG encapsulated (D-spacing: 0.34 nm) nanoparticles consisting BCC Fe, FCC (Fe, C) and orthorhombic Fe3C phases were obtained with average core diameter of ∼45 nm and average shell thickness of ∼6 nm (8–50 layers). MLG encapsulated Fe/Fe3C nanoparticles were achieved with soft ferromagnetic (Ms: ∼64 emu/g; Hc: ∼276 Oe) property. MLG coated Fe/Fe3C nanoparticles were suspended in an aqueous media using poly/acrylic acid as a post-synthetic treatment. They were found cytocompatible even at 200 µg/mL and 75 µg/mL after 24 and 48 h exposure, respectively. Dose dependent cytotoxicity was studied on both MCF7 and HeLa cells after 72 h incubation. Light-to-heat conversion efficiency of these nanoparticles at 795 nm irradiation in water was calculated as 37.60 %. After laser irradiation, with an increased concentration of nanoparticles (75–200 µg/mL), more than 80 % cell death was observed on both MCF7 and HeLa cells lines via late apoptotic cell death as a result of photothermal effect.",

keywords = "Chemical vapor deposition, Core/shell magnetic nanoparticles, Magnetic/Thermal properties, Microstructure-final, Multilayer graphene, Phototoxicity/cytotoxicity",

author = "Sıddıka Mertdin{\c c}-{\"U}lk{\"u}seven and Kubra Onbasli and Ece {\c C}akır and Yağız Morova and {\"O}zge Balcı-{\c C}ağıran and Acar, {Havva Yagci} and Alphan Sennaroğlu and {L{\"u}tfi {\"O}ve{\c c}oğlu}, M. and Duygu Ağaoğulları",

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Mertdinç-Ülküseven, S, Onbasli, K, Çakır, E, Morova, Y, Balcı-Çağıran, Ö, Acar, HY, Sennaroğlu, A, Lütfi Öveçoğlu, M & Ağaoğulları, D 2023, 'Magnetic core/shell structures: A case study on the synthesis and phototoxicity/cytotoxicity tests of multilayer graphene encapsulated Fe/Fe₃C nanoparticles', Journal of Alloys and Compounds, vol. 968, 172145. https://doi.org/10.1016/j.jallcom.2023.172145

TY - JOUR

T1 - Magnetic core/shell structures

T2 - A case study on the synthesis and phototoxicity/cytotoxicity tests of multilayer graphene encapsulated Fe/Fe3C nanoparticles

AU - Mertdinç-Ülküseven, Sıddıka

AU - Onbasli, Kubra

AU - Çakır, Ece

AU - Morova, Yağız

AU - Balcı-Çağıran, Özge

AU - Acar, Havva Yagci

AU - Sennaroğlu, Alphan

AU - Lütfi Öveçoğlu, M.

AU - Ağaoğulları, Duygu

PY - 2023/12/15

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N2 - This study reports on a novel and optimized synthesis procedure of multilayer graphene (MLG) encapsulated Fe/Fe3C nanoparticles using a combined method of spray drying, chemical vapor deposition (CVD) and leaching from FeCl3.6 H2O based precursor, in addition to phototoxicity/cytotoxicity tests for their potential use in biomedical applications. CVD studies were employed at various temperature/time and gas flow rate values. Based on the X-ray diffractometry (XRD), Raman spectroscopy, vibrating sample magnetometry (VSM), transmission electron microscopy/energy-dispersive spectroscopy (TEM/EDS) and differential thermal analysis/thermogravimetry (DTA/TG), CVD parameters of 900 °C, 60 min, 50 mbar and CH4/H2:1/1 were determined as optimum conditions. MLG encapsulated (D-spacing: 0.34 nm) nanoparticles consisting BCC Fe, FCC (Fe, C) and orthorhombic Fe3C phases were obtained with average core diameter of ∼45 nm and average shell thickness of ∼6 nm (8–50 layers). MLG encapsulated Fe/Fe3C nanoparticles were achieved with soft ferromagnetic (Ms: ∼64 emu/g; Hc: ∼276 Oe) property. MLG coated Fe/Fe3C nanoparticles were suspended in an aqueous media using poly/acrylic acid as a post-synthetic treatment. They were found cytocompatible even at 200 µg/mL and 75 µg/mL after 24 and 48 h exposure, respectively. Dose dependent cytotoxicity was studied on both MCF7 and HeLa cells after 72 h incubation. Light-to-heat conversion efficiency of these nanoparticles at 795 nm irradiation in water was calculated as 37.60 %. After laser irradiation, with an increased concentration of nanoparticles (75–200 µg/mL), more than 80 % cell death was observed on both MCF7 and HeLa cells lines via late apoptotic cell death as a result of photothermal effect.

AB - This study reports on a novel and optimized synthesis procedure of multilayer graphene (MLG) encapsulated Fe/Fe3C nanoparticles using a combined method of spray drying, chemical vapor deposition (CVD) and leaching from FeCl3.6 H2O based precursor, in addition to phototoxicity/cytotoxicity tests for their potential use in biomedical applications. CVD studies were employed at various temperature/time and gas flow rate values. Based on the X-ray diffractometry (XRD), Raman spectroscopy, vibrating sample magnetometry (VSM), transmission electron microscopy/energy-dispersive spectroscopy (TEM/EDS) and differential thermal analysis/thermogravimetry (DTA/TG), CVD parameters of 900 °C, 60 min, 50 mbar and CH4/H2:1/1 were determined as optimum conditions. MLG encapsulated (D-spacing: 0.34 nm) nanoparticles consisting BCC Fe, FCC (Fe, C) and orthorhombic Fe3C phases were obtained with average core diameter of ∼45 nm and average shell thickness of ∼6 nm (8–50 layers). MLG encapsulated Fe/Fe3C nanoparticles were achieved with soft ferromagnetic (Ms: ∼64 emu/g; Hc: ∼276 Oe) property. MLG coated Fe/Fe3C nanoparticles were suspended in an aqueous media using poly/acrylic acid as a post-synthetic treatment. They were found cytocompatible even at 200 µg/mL and 75 µg/mL after 24 and 48 h exposure, respectively. Dose dependent cytotoxicity was studied on both MCF7 and HeLa cells after 72 h incubation. Light-to-heat conversion efficiency of these nanoparticles at 795 nm irradiation in water was calculated as 37.60 %. After laser irradiation, with an increased concentration of nanoparticles (75–200 µg/mL), more than 80 % cell death was observed on both MCF7 and HeLa cells lines via late apoptotic cell death as a result of photothermal effect.

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KW - Core/shell magnetic nanoparticles

KW - Magnetic/Thermal properties

KW - Microstructure-final

KW - Multilayer graphene

KW - Phototoxicity/cytotoxicity

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