Structural and spectroscopic studies of bromofullerene P. Anto Christy a , A. Milton Franklin Benial b , A. John Peter a, * , Chang Woo Lee c, ** a P.G and Research Dept. of Physics, Government Arts College, Melur, 625106, Madurai, India b PG and Research Department of Physics, N.M.S.S.V.N College, Madurai, 625 019, India c Department of Chemical Engineering, College of Engineering, Kyung Hee University,1732 Deogyeong-daero, Gihung, Yongin, Gyeonggi 446-701, South Korea article info Article history: Received 9 June 2018 Received in revised form 5 November 2018 Accepted 25 November 2018 Available online 28 November 2018 Keywords: Fullerene Bromination Structure properties HRTEM abstract Structural and spectroscopic studies on fullerene and bromofullerene molecules were investigated. The reaction with liquid bromine was used to prepare bromofullerene and it was characterized by using X-ray diffraction, ultravioletevisible, Fourier transform infrared, Fourier transform Raman, electron para- magnetic resonance, scanning electron microscopy, high resolution transmission electron and energy dispersive X-ray techniques. The XRD pattern of bromofullerene confirms the attachment of bromine to fullerene. FT-IR and FT-Raman characterization reveal the C-Br vibrations in the brominated fullerene which confirms the bromination. UVeVis spectral analysis endorses shifting of absorption peak. EPR line width, with g-factor values, indicates the magnetic ion sites in the samples. Scanning electron micro- scope and high resolution transmission electron microscope signify the changes in surface and particle size of the molecule. The particle size was calculated from Debey-Sherrer's formula and corroborated by TEM images. Energy dispersive X-ray elemental micro analysis confirms the presence of bromine element in the molecule. The enhanced reactivity by substitution of bromine paves the way for designing the bioactive molecules which will be useful in the field of carbon nano-medicine and targeted drug delivery applications. © 2018 Elsevier B.V. All rights reserved. 1. Introduction The development of versatile functionalization chemistry allowed for a large varieties of organic reactions has been carried out with fullerene such as arylation, halogenation, hydroxylation, and alkoxylation ever since the discovery of fullerene and pro- duction in wide range [1 ,2]. C 60 fullerenes can be easily function- alized due to their high reactivity with unique physical and electrical properties. Halogenation was one such functionalization which has been carried out by various research groups. Hal- ofullerenes have been intensively studied as versatile synthetic intermediates in fullerene chemistry. Synthesis of halogenated fullerenes which were among the first reported fullerene de- rivatives exposing a new field with the reactivity of nucleophiles [3]. The mechanism is thought to be similar to the electrophilic aromatic substitution reaction. It has been well established that halogenated fullerene C 60 X n , (X ¼ Br,F,Cl) derivatives act as synthetic intermediates for further substitution via replacement with nucleophiles [4]. The reaction of C 60 with fluorine, chlorine, and bromine are important because the resulting halide products can be useful precursors to a variety of substituted derivatives [5]. Since fullerene is highly symmetrical in nature, any derivatives of it would have novel spectrum due to reduction of symmetry [6e10]. It is well known that halogen atoms are typical electron- withdrawing ones with the small size. Earlier, the reaction of C 60 with liquid bromine has been found to afford bromofullerene. Bromination of fullerene in organic solvents gave C 60 Br 6 and C 60 Br 8 . It was difficult to reproduce the synthesis of bromofullerene because the experimental procedures were virtually lacking in the publications. Bromination of fullerene by neat bromine was re- ported earlier with two or four bromines attached based on weight uptake were confirmed [11e 14]. It has been shown that bromina- tion of fullerene with neat bromine gives bromo derivatives. Hence, the extensive investigation was carried out followed by the convenient procedures for the synthesis of bromofullerene and obtained reliable data on the molecular and crystal structures of bromides of fullerene [15]. Fullerene and its derivatives have a lot of applications in the field * Corresponding author. ** Corresponding author. E-mail address: a.john.peter@gmail.com (A. John Peter). Contents lists available at ScienceDirect Journal of Alloys and Compounds journal homepage: http://www.elsevier.com/locate/jalcom https://doi.org/10.1016/j.jallcom.2018.11.336 0925-8388/© 2018 Elsevier B.V. All rights reserved. Journal of Alloys and Compounds 780 (2019) 202e211