CoFe2O4-Fe3O4 Bimagnetic Heterostructure A Versati

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CoFe2O4-Fe3O4 bimagnetic heterostructure: A versatile core-shell

nanoparticle with magnetically recoverable photocatalytic and self heating
properties
Article in Materials Research Express · January 2020

DOI: 10.1088/2053-1591/ab6493
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Chandan Borgohain Jyoti Prasad borah

Indian Institute of Technology Guwahati National Institute of Technology Nagaland
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CoFe2O4-Fe3O4
bimagnetic heterostructure: A versatile core-shell nanoparticle with
magnetically recoverable photocatalytic and self heating properties
To cite this article before publication: Chandan Borgohain et al 2019 Mater. Res. Express in press https://doi.org/10.1088/2053-1591/ab6493
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Page 1 of 25 AUTHOR SUBMITTED MANUSCRIPT - MRX-119272.R2
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4 CoFe2O4-Fe3O4 bimagnetic heterostructure: A versatile core-shell
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6 nanoparticle with magnetically recoverable photocatalytic and self heating
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8 properties
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10 C. Borgohaina*, J. P. Borahb ,*
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12 a
Central Instrumentation Facility (CIF), Indian Institute of Technology Guwahati, Guwahati, 781039,
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14 India
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Department of physics, National Institute of Technology Nagaland, Chumukedima, 797103, India
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17 email: acbgohain@rediffmail.com, bjpborah @rediffmail.com
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22 ABSTRACT
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CoFe2O4-Fe3O4 (Fe/Co = 2.3, 2.75 & 3.5) core-shell magnetic nanocomposite (MNC) was successfully
prepared by combined sonochemical and reverse co-precipitation method using cost effective and readily
available precursor. The structure, morphology, thermal, optical and magnetic properties of the MNC was
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extensively studied and the product was found suitable for use as an environmentally safe recyclable
30 photocatalyst for pollution control. The self-heating properties of the MNC was also investigated for
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32 magnetic hyperthermia application. The studies of Infrared (IR) and Ultraviolet-visible (UV-Vis)
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34 spectroscopy confirmed the synthesis and formation of the bimagnetic heterostructure. The X-ray
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Diffraction studies and Transmission Electron Microscopy (TEM) analysis confirmed the formation of
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37 subnanometer clusters (<10 nm) in the asprepared samples. The results of Differential Scanning
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39 Calorimetry (DSC)/Thermo-Gravimetric Analysis (TGA) analysis of the as prepared samples showed

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41 transformation of intermediate Fe-phases to Fe3O4 during sample heating at 420oC. This transformation
42 accompanied structural changes in the asprepared sample that led to the formation of the coreshell
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44 structure which was observed in the TEM images of the annealed sample with Fe/Co ratio (x= 3.5). The
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46 magnetization-hysteresis (M-H) studies was done on the asprepared and annealed samples using the
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Vibrating Sample Magnetometer (VSM). The VSM studies showed significant improvement of
49 magnetization and coercivity in the annealed samples making it suitable for re-usability in photocatalytic
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51 reaction and magnetic hyperthermia application. The degradation of phenolphthalein (a non-
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53 biodegradable organic chemical) in the presence of UV light irradiation was used as a reference reaction
54 to confirm the photocatalytic properties of the CoFe2O4-Fe3O4 MNC, which could be well isolated from
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56 the media at the end of degradation, by applying an external magnetic field and reused. The
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AUTHOR SUBMITTED MANUSCRIPT - MRX-119272.R2 Page 2 of 25
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3 nanocomposite was also investigated for magnetic hyperthermia using induction heating properties and
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5 the result infer that it is also a promising material for hyperthermia application.
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KEYWORDS
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10 Sonochemical, co-precipitation, core-shell, exchanged-coupled, photocatalytic, magnetic hyperthermia
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12 1. Introduction:
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14 Nanoscale magnetism of a magnetic nanoparticle system composed of a magnetically hard and soft
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phases has stimulated great interest in the recent years due to their importance in many technological
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17 applications [1-2]. Compared to traditional single-phase material, such two-phase systems have high
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19 magnetization and coercivity [3], which are the most important parameters describing a permanent
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21 magnet. However, a bimagnetic core/shell nanoparticle system, where the shell in addition to being
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magnetic (ferro- or ferri-magnetic) also show good optical property has been less studied. The study of
such nanoparticle system is interesting due to their potential in magneto-optical, electromagnetic,
biomedical, photocatalytic and permanent magnetic applications. Therefore, it is tempting to consider
composites of material consisting of bi-magnetic phases, one of which provides a high nucleation field for
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29 irreversible magnetization reversal at the core and the other material with high magnetization saturation,
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31 Ms and good optical property at the shell. Here, we report the fabrication of core-shell MNC of CoFe2O4
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33 (core) and Fe3O4 (shell), using reverse co-precipitation technique under the assistance of ultrasonic
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irradiation [4, 5]. CoFe2O4 nano-particle is a well-known hard magnetic material [5, 6, 7], which has been
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36 studied in detail due to its high coercivity, moderate magnetic saturation, remarkable chemical stability
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38 and mechanical hardness. On the other hand, Fe3O4 (magnetite) with large saturation magnetic moment
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40 and low coercivity nanoparticles could serve as an ideal soft magnetic material for the nanocomposite [8].
41 Moreover, due to the well-known optical properties, biocompatibility and excellent ferrimagnetic
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43 properties exhibited by the Fe3O4 nanoparticles, their applications could also be explored in several areas
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45 of science and technology. These areas include magnetic recording technology, pigments, catalysis and
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photo-catalysis [9-13], as well as the medical uses with emphasis on the cell separation [14], biological
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48 sensing and probing [15,16], Magnetic hyperthermia [17,18] making it a truly multifunctional
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50 nanocomposite. Erikson et al. [19] has studied the nonstoichometry, cation distribution and electrical
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52 properties of CoFe2O4-Fe3O4 nanocomposite prepared by resin intermediate method (P. PECHINI, U.S.
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53 Patent 3,330,697, July 11, 1967) at high temperature. So far no elaborate application oriented study on
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55 magnetic and optical properties of such core-shell CoFe2O4-Fe3O4 nanocomposite system prepared by
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3 sonochemically assisted reverse co-precipitation technique has been done. A study of these conjugates
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5 may provide an insight into developing nanostructured material with enhanced magnetic and optical
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7 properties for possible use as an effective photo-catalyst in environmentally safe cost effective pollution
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control and hyperthermia applications. There are different technologically important methods such as
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10 acqueous coprecipitation, [20, 21] sonochemical reactions, [22, 23] hydrolysis of precursor, [24, 25]
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12 mechano-chemical synthesis, [26, 27] hydrothermal process, [28, 29] microwave synthesis, [30] micelle
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14 microemulsion, [31] and others [32-33]. Chemical routes are commonly used to fabricate ultra-fine
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powder having high volume of crystalline structure and uniform size distribution [34, 35]. Among
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17 numerous chemical methods, co-precipitation is considered to be the simplest, cost-effective and most
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19 efficient pathway to obtain magnetic nanoparticles [36-38]. In our approach, both CoFe2O4 and Fe3O4 are
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21 incorporated as nanometer scale building blocks in a single step reaction by the reverse co-precipitation
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technique under the assistance of ultrasonic irradiation [4-5]. The reverse co-precipitation technique is a
simple fast and inexpensive approach to synthesize these nanocomposites since it does not involve any
intermediate steps. In addition, it is also easy to control the stoichiometric composition and crystallite
sizes, which have many important effects on the magnetic and optical properties. The Fe/Co ratio (2.3 to
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29 3.5) in CoxFe3-xO4 (where x=0.67 to 0.91) can be easily varied to obtain a nano-composite of desired
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31 properties by tuning the composition of the individual building blocks. In this paper, we have prepared
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33 highly stable cobalt ferrite/ferric oxide nanocomposite by combined sonochemical and reverse co-
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precipitation method. This is achieved by adding off-stoichiometric ratios of mixed acidic solution of
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36 metal salts (FeCl3 and CoCl2.6H2O) to a large amount of basic solution, which maintains the solution pH
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38 until all the components gets precipitated completely [39]. The main aim of the present work is to
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40 investigate the influence of Fe/Co ratio on the structural, magnetic and optical properties of the
41 nanocomposite. We also emphasize on the development of an effective tool for the degradation of
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43 environmental pollutants such as phenolphthalein (a non-biodegradable organic chemical). The
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45 investigation also analyses the application prospects of the nanocomposite for magnetic hyperthermia
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applications.
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48 2. Experimental:
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50 The raw material used in the synthesis of CoFe2O4-Fe3O4, was obtained from Merck and used as
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52 purchased. The raw materials are cobalt chloride hexahydrate CoCl2.6H2O (purity 98%), Iron chloride
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53 FeCl3 (purity 97%) and sodium hydroxide NaOH (purity 96%).

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3 2.1 Synthesis of CoFe2O4-Fe3O4 nanocomposite:
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5 The CoFe2O4-Fe3O4 MNC was synthesized by taking two aqueous solutions of FeCl3 (2.399g, 14.7 mmol,
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7 50 ml) and CoCl2.6H2O (1g, 4.2 mmol, 50 ml) mixed in a 200 ml flat bottom flask. The mixed acidic
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solution was added drop-wise to an aqueous NaOH solution (4 g, 250 mmol, 25 ml) in a 500ml beaker.
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10 The reaction was done under argon atmosphere with continuous ultrasonic irradiation using a JEIOTECH,
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12 Lab Companion Ultrasonic bath (Model: 1505), operating at a frequency 40 KHz and a power of 40 KW.
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14 Prior to mixing, all these three solutions were sonicated for 30 min to remove any dissolved oxygen.
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During mixing, the pH of the solution was continuously monitored and maintained in a range of 13-14.
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17 After the completion of the mixing, the temperature of the sonicator bath was raised up to 330 K and was
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19 further sonicated for 30 minutes in air atmosphere. The black precipitate formation was observed and the
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21 reaction mixture was then centrifuged at 14000 rpm at ambient temperature for 15 minutes. The black
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precipitate was separated from supernatant liquid and washed off with copious amount of distilled water
and ethanol. A sample of the precipitate formed was analyzed in TEM-EDX and the formation of
CoFe2O4-Fe3O4 nanocomposite was confirmed from the Fe and Co ratio (Fe/Co = 3.5). We have repeated
the above steps by taking two more concentration of FeCl3 as 1.8812 g (11.6 mmol) and 1.5702 g (9.68
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29 mmol) in 50ml water to obtain the desired ratios of Fe and Co (Fe/Co = 2.3 and 2.75). To study the
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31 microstructural and magnetic properties of the nano-crystalline particles, the material was annealed in
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33 nitrogen atmosphere for 12 hours using a custom made tubular muffle furnace at temperature of 500 oC
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and was quenched using compressed nitrogen gas at room temperature.
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36 2.2 Characterization:
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38 The crystalline nature of the synthesized CoFe2O4-Fe3O4 sample was investigated by XRD pattern
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40 recorded on a Bruker AXS D8 using Cu-K radiation ( = 1.54178 A). The crystallite size of the
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CoFe2O4-Fe3O4 nanoparticles was obtained from the XRD pattern using Scherer's formula. The IR studies
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43 were recorded using a PerkinElmer RXI FT-IR spectrometer in KBr pellets. The crystallinity and particle-
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45 size of the CoFe2O4-Fe3O4 nanoparticles were examined by TEM (JEOL JEM2100). The sample for TEM
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analysis was prepared by taking a micro drop of dilute ethanol solution of the dispersed nano-particles,
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48 deposited on a carbon-coated copper grid (400 mesh size). The nanoparticle was observed in bright field
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50 TEM imaging at a maximum resolution of 20 nm with a magnification range of 50–200KX. The magnetic
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52 properties were observed under the application of a magnetic field upto 20 kOe, for the various samples
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using a VSM (Lakeshore 7410). UV-Vis spectra of the nanoparticles as well as the photocatalytic
55 degradation were recorded in a Varian Cary 50 bio UV-Vis spectrophotometer.
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3 The specific surface area was measured by the application of Brunauer–Emmett–Teller (BET) equation
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5 and Barrett–Joyner–Halanda (BJH) method. The sample was first degassed for 2h at 200◦C and then
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7 analyzed by a Backman Coulter (SA 3100) surface area and pore-size Analyzer. Induction heating
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variations were analyzed by using Easy Heat AMBRELL 8310.
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10 2.3 Photocatalytic degradation of phenolphthalein by CoFe2O4-Fe3O4 nanocomposite:
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12 The evaluation of photocatalytic activity for the prepared samples was measured by degrading
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14 phenolphthalein in aqueous solution at ambient temperature. The experiment was carried out in a 200 ml
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quartz glass vessel. The core-shell CoFe2O4-Fe3O4 MNC (0.02 g) was placed into the tubular quartz
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17 vessel containing 100 ml of 1x10-5 M phenolphthalein aqueous solution. Then the mixture was stirred in
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19 dark to obtain absorption/desorption equilibrium until a uniform concentration of phenolphthalein was
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21 obtained. The mixture was then illuminated with a 12 mW UV lamp (wavelength of 400 nm) with
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continuous stirring. After the reaction began, the mixture was sampled at different times and separated by
a magnet to discard any sediment. The absorption spectra was obtained through a wavelength scan from
220-350 nm with aid of quartz cells (10 mm optical path length) on a UV–Vis spectrophotometer.
3. Results and discussion:
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29 3.1 Structural and Morphological analysis:
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31 In the present study, we report the microstructural, magnetic and optical properties of a series of
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33 nanocomposites of CoFe2O4-Fe3O4 with Fe/Co ranging from 2.3 to 3.5 synthesized by the sonochemically
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assisted reverse co-precipitation method. The TEM observation of the as prepared samples shown in
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36 figure 1a-1b and figure 1c-1d indicate the formation of clusters of approximately 4-8 nm in diameter with
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38 particle-particle contact surrounding the CoFe2O4 nanoparticle. It is highly possible that subnanometer
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40 phases such as FeOOH (akagenite), Fe5HO8.H2O (Ferrihydrite), Fe(OH)3, etc along with CoFe2O4
41 nanoparticle may be formed due to off- stoichiometric ratios of NaOH and FeCl3 in the reaction [40].
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43 These intermediate phases are more prominently observed in the TEM images of the as prepared samples
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45 with Fe/Co equal to 3.5.
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Figure 1(a). Bright field TEM images and (b) HRTEM images of CoFe2O4-Fe3O4 as prepared
nanocomposite for Fe/Co=2.3.
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45 Figure 1(c). Bright field TEM images and (d) HRTEM images of CoFe2O4-Fe3O4 as prepared
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nanocomposite for Fe/Co=3.5
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3 Table 1. Vibrational band frequencies (ν1) and (ν2) of CoFe2O4-Fe3O4.
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5 Observed Fe/Co (x) ν 1 (cm-1) ν 2 (cm-1)
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7 2.3 581 400
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9 2.75 586 405
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10 3.5 591 410
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13 The IR spectra of the as prepared samples in figure 2 have been used to locate the band positions in the
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15 region between 350 cm-1 and 4000 cm-1 and their values are given in table1. The higher frequency band
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17 observed at around 600 cm-1 (ν1) and the lower frequency at around 400 cm-1 (ν 2) are an indication of
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formation of CoFe2O4 spinel structure [41]. These bands are assigned to intrinsic vibration in the
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20 tetrahedral and octahedral interstices [42]. In the present system we have also observed prominent peaks
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22 around 1623 cm-1 and 3410 cm-1 which also suggest the formation of the intermediate Fe-phases and the
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hydroxyl ions that were entrapped on the surface of the nanoparticle during the sonication process. Figure
3 shows the DSC/TGA curves of the sample with Fe/Co ratios (x= 3.5) recorded on a NETZSCH 449 F3
Jupiter under nitrogen atmosphere at a heating rate of 10oC/minute. The DSC-TGA curves showed a
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29 complicated behavior arising from the simultaneous dehydration and oxidation of the Fe-phase. The TGA
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curve showed an initial weight loss of ~17 % upto 200oC due to de-absorption of OH ions. Further, a
32 close examination of the DSC curve also showed peaks which is attributed to transformation of the
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34 intermediate Fe-phase to Fe2O3 at 269.3oC and finally to Fe3O4 at 420oC [40]. This transformation
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36 accompanied structural changes in the asprepared sample that led to the formation of the coreshell
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structure. Therefore, to form highly crystalline and well defined nanocomposites of CoFe2O4 and Fe3O4,
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39 all the samples were annealed at 500 oC for 12 hours under nitrogen atmosphere.
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Figure 2. IR spectra of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x) varying from to 2.3 to 3.5.
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52 The UV-Vis analysis of the annealed samples in figure 3 showed absorption bands around 400nm. The
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direct band gap corresponding to these absorption bands was observed between 2.19 eV - 2.57 eV which
55 was calculated by plotting (αhν)2 vs hν (Figure 3b) using Equation 1[43].
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4 h = Const(h − Eh )n ------------------------ (1)
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6 The value of α is obtained from Equation 2. [42]
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= 2.3026 ------------------------------------ (2)
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11 Where A is absorption and t is the thickness of the sample.
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13 The CoFe2O4 nanoparticle is identified by a charge transfer band around 350nm [45]. In CoFe2O4-Fe3O4
14 nanocomposite we have observed this band at 400 nm. This shift in the charge transfer band indicates the
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16 formation of CoFe2O4-Fe3O4 NP. Compared to traditional Fe3O4 [46], these bands showed a red shift with
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18 a prominent absorption in the near-ultraviolet spectral region suggesting its suitability for photo-catalytic
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activity [47]. Figure 5 shows the XRD of annealed CoFe2O4-Fe3O4 nanocomposite. The diffraction peaks
21 and relative intensities of all patterns matched well with a cubic spinel structure of CoFe2O4 and Fe3O4
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(JCPDS–International center diffraction data, PDF cards 22-1086 and 1-1111). However, the small
difference in the lattice parameter of both compounds makes it difficult to differentiate them. Further, no
other impurity phase other than CoFe2O4 and Fe3O4 was found in all the patterns. The profile of the SAED
patterns in figure 7b & 7c also showed peaks which matched well with the cubic spinel structure of
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30 CoFe2O4 and Fe3O4 and is consistent with the XRD analysis. The crystallite size as calculated by
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32 Scherer’s broadening analysis [48] of the spinel 311 reflection, are shown in table 2.
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Figure 4(a). Absorption spectra’s of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x) varying from to
2.3 to 3.5. Inset: 4(b) Band gap measurement of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x)
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30 varying from to 2.3 to 3.5
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3 The nanostructure of the heat-treated samples (Figure 6a-6d) was also investigated using TEM. Again,
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5 because of the similarities in the crystal structures it was difficult to distinguish between the CoFe2O4 and
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7 Fe3O4 phases in the TEM images. High resolution TEM (HRTEM) has been done to clearly distinguish
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the phases. The HRTEM image of the annealed sample (Fe/Co = 2.3) in figure 6b showed some
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10 coalescence but, the phases in the sample (Fe/Co = 3.5) in figure 6d remained isolated with the formation
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12 of a core-shell structure. The particle size distribution of the TEM images shown in figure 7a & 7d and
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14 table 2 showed an increase in average particle size for higher Fe ratio. This may be due to the
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coalescences of the Fe-phase upon annealing that lead to the formation of a Fe3O4 shell and was more
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17 prominently observed for the sample Fe/Co = 3.5. However, the CoFe2O4 MNP at the core showed good
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19 structural stability [22]. The formation of the cobalt ferrite/ferric oxide core-shell hetrostructure has been
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Figure 6(a). Bright field TEM images and (b) HRTEM images of CoFe2O4-Fe3O4 annealed
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Figure 6(c). Bright field TEM images and (d) HRTEM images of CoFe2O4-Fe3O4 annealed
nanocomposite for Fe/Co=3.5
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50 Figure 7(a). Particle size distribution and (b) SAED pattern of annealed CoFe2O4-Fe3O4 nanocomposite
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with Fe/Co=3.5
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Figure 7(c). SAED pattern and (d) Particle size distribution of annealed CoFe2O4-Fe3O4 nanocomposite
with Fe/Co=2.3
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Figure 8. Schematic illustration of formation of the cobalt ferrite/ferric oxide core-shell hetrostructure.
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3 Table 2. Some physical parameters of CoFe2O4-Fe3O4 nanocomposite prepared by combined
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7 Observed Crystallite Particle size (nm) Coercivity Hc (Oe) Magnetization
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9 Fe/Co (x) size (nm) Annealed (300K) MS (emu/g)
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12 2.3 22.75 24 812 63
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14 2.75 30.44 - 865 69
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3.5 44.32 50 867 73
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19 3.2 Magnetic Analysis:
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21 The magnetic behavior of the asprepared and annealed samples has been explained on the basis of the
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magnetization curves measured at room temperature and at 80 K and are shown in fig.9 and fig.10. The
inset in the figure 9 and figure 10 shows the expanded region around the origin to make the coercivity
more visible at various temperatures. The magnetization and coercivity values were extracted from the
magnetization curves are shown in Table 2. The development of coercivity differed greatly between the
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29 single phase and two phase Co-Fe structure. Our previous studies on single phase CoFe2O4 structure
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31 prepared by this method have given a moderate coercivity which transformed to a hard magnetic structure
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33 after appropriate heat treatment [22, 39, and 49]. In the present study we have observed a clear hysteresis
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for the annealed samples with Fe/Co ratio at 2.3 with a coercivity of 812 Oe which reached a maximum
36 of 4KOe at 80K for the sample Fe/Co = 3.5. Moreover, the hysteresis loops of the sample (Fe/Co = 3.5)
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38 measured at 80K in figure 10 also showed a non-saturating behavior which may be attributed to strong
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40 magnetocrystalline anisotropy. As the field approached zero a prominent hump appeared in the
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demagnetization curve particularly for the sample Fe/Co = 3.5 and was more prominent in the hysteresis
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43 loops measured below 150 K. A similar feature has been observed in the magnetization-demagnetization
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45 curves of CoFe2O4-ZnFe2O4 core-shell structure reported by Ombretta Masala et al [50] and has been
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attributed to magnetic exchange coupling between the hard CoFe2O4 phase and soft ZnFe2O4 phase.
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48 Similarly in our case the magnetic interaction across the grain boundaries of the hard CoFe 2O4 phases and
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50 soft Fe3O4 phases of the core-shell structure has given rise to exchange coupling between the phases [51].
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52 The evidence of core-shell structure in the annealed samples is also observed from the temperature
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dependence of the field-cooled (FC) and zero-field cooled (ZFC) magnetization curves of the annealed
55 samples under an applied field of 100 Oe. Below the blocking temperature TB, the FC and ZFC curves in
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3 figure 11 diverge and the ZFC values approach zero as the temperature approaches 10K. From the figure
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5 11 we also observed that the blocking temperature is independent of the sample composition and is same
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7 for the samples with Fe/Co = 2.3 and 3.5. We may conclude that the magnetization of both the phases in
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the core-shell type structure are correlated due to spin coupling at the interface and one value of blocking
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31 Figure 9. M-H curves of annealed CoFe2O4-Fe3O4 nanocomposite with Co/Fe ratios (x) varying from to
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33 2.3 to 3.5 measured at room temperature
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56 temperature (80K to 300K)
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Figure 11. Temperature dependence of Field-cooled (FC) and Zero-field cooled (ZFC) magnetization
curves of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x = 2.3 and3.5) measured at 100Oe
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29 3.3 Photocatalytic degradation of phenolphthalein:
30 The excellent magnetic and optical properties shown by this nanocomposite has prompted its use as an
31
32 effective photocatalyst in environmentally safe and cost-effective pollution control which is an important
33
34 area of research and needs immediate attention. Although there are several approaches for environmental
35
36 cleanup such as adsorption, reverse-osmosis, chlorination, ozonisation etc, photocatalysis is an
37 environmental friendly process that utilizes the radiation energy to perform catalytic reactions under
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39 ambient conditions. This technology has been widely investigated for eradication of pollutants that are
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41 present in the environment. Reduction of phenolic (phenolphthalein) compounds to their corresponding
42
derivatives in the presence of UV light irradiation has been chosen as a standard reaction for monitoring
43
44 the catalytic activity of the nanocomposite. The UV-VIS spectra of phenolphthalein during the UV
45
46 irradiation are illustrated in figure 12. It can be seen that the maximum absorbance of 227 nm and 277 nm
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47
48 disappears completely after irradiation for about 5 h. A blank experiment in the absence of irradiation but
49 with CoFe2O4-Fe3O4 MNC with Fe/Co ratios (x= 3.5) catalyst demonstrates that no degradation occurs as
50
51 shown in the spectra. Another blank experiment in the absence of the catalyst but under irradiation shows
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Figure 12. UV-VIS absorption of phenolphthalein in the presence of CoFe2O4-Fe3O4 (x=3.5) under UV
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21 Figure 13. Recovery of CoFe2O4-Fe3O4 nanoparticle by applying an external magnetic field at the end of
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the reaction
The CoFe2O4-Fe3O4 MNC is a new photocatalyst to degrade organic contaminants, such as
phenolphthalein. The photo catalytic degradation percentage of phenolphthalein was calculated using
Equation 3.
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30 AO − A
31 Degradation% = x100% -----(3)
AO
32
33
Where, Ao is the initial absorbance of phenolphthalein before degradation and A is the absorbance after
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35 time t. It was found that the degradation % of phenolphthalein is 93% in 5 hour of UV irradiation. The
36
37 observed high degradation may be attributed due to (a) high band gap energy (2.57eV) for the
38
nanocomposite [52], and (b) small particle size (30-40 nm) which is associated with remarkably high
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40 surface area (BET surface area = 133.46m2/g) as the photocatalysis occurs at the surface of the catalyst.
41
42 The high photocatalytic activity shown by this nanocomposite can also be explained on the basis of
43
44 electrical and optical properties of the sample. It is known that CoFe2O4 is a p-type semiconductor [53],
45
but it was shown by Na and Lee [54] that Fe excess cobalt ferrite exhibited n-type conduction due to
46
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47 cation redistribution in spinel lattice. As electrons have higher mobility than holes, Fe-excess cobalt
48
49 ferrite shows higher electrical conductivity [54]. To confirm the high conductivity of the sample, we have
50
51 also calculated the Urbach energy (EU) of the sample which characterizes the extent of the exponential tail
52 of the absorption edge [55]. Although, Urbach energy (EU) depend on parameters such as temperature,
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54 thermal vibrations in the lattice, induced disorder, static disorder etc., the main factor contributing to edge
55
56 broadening in our sample is exciton-phonon coupling (dynamic disorder). The urbach energy calculated
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3 for our sample (Fe/Co = 3.5) is EU ~ 0.84eV, which is higher than the Urbach energy of Fe3O4 reported by
4
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5 Ghandoor et al [56] and EI-Daisty et al [57]. These results suggest that our composite is more conducting
6
7 than CoFe2O4 or Fe3O4 [56]. Therefore, the photogenerated electrons during UV irradiation of our sample
8
9
in solution are more efficiently generated and transferred to the surface of the nanoparticle which react
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10 with the trapped O2 to produce superoxide radical anions,O2•-, which on further protonation generates
11
•
12 OH. These •OH radicals is highly reactive to degrade organic molecules and enhances the photocatalytic
13
14 activity of the sample.The as-prepared CoFe2O4-Fe3O4 MNC with combined the catalytic and magnetic
15
properties could be isolated from the reaction mixture easily by an exterior magnet (fig. 13) at the end of
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21 3.4 Induction heating studies:
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51 Figure 14: Induction heating curves of CoFe2O4-Fe3O4 as prepared nanocomposite for Fe/Co=3.5
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Figure 15 : Histogram of SAR values of nanocomposite with Fe/Co ratios 3.5
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32 The plot of self heating capabilities of the nanocomposite with Fe/Co ratio at 3.5 as a function of time is
33
presented in the figure 14 (Field amplitude H=8.98 kAm-1and constant frequency f =337 kHz). We have
34
35 chosen the field amplitude and frequency within the biological safety limit as suggested by Hergt [58].
36
37 However, in other systems (2.5 and 2.75) could not reach the hyperthermic temperature and therefore not
38
shown here. Heating profile conclusively shows that the nanocomposite with ratio 3.5 and optimum
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40 concentration 2mg/ml attain the hyperthermic threshold temperature limit. The possible reason to act as a
41
42 nano-heater of the nanocomposite with Fe/Co ratio 3.5 is due to the higher magnetization and coericivity
43
44 compared to other nanocomposites. To analyze the hyperthermia efficiency of the nanocomposite, a well-
45
46
known parameter, Specific Absorption Rate (SAR) has been calculated by using initial slope method [59]
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47 and is depicted in the figure 15. As can be seen, the SAR value decreases with particle concentration.
48
49 Probably, the dipolar energy exert a disordering random torque-disrupting spin relaxation process due to
50
51 competition between the interparticle interaction and interparticle anisotropy and hence SAR value
52
decreases [60].
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3 4. Conclusion:
4
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5 In conclusion, we have synthesized CoFe2O4-Fe3O4 nanocomposites using a combined sonochemical and
6
7 reverse co-precipitation technique. A two-phase core-shell structure of CoFe2O4 and Fe3O4 was formed
8
9
after annealing the asprepared sample at 500oC which showed excellent magnetic and optical properties.
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10 Our approach suggests that this method can be used for the controlled synthesis of core-shell CoFe2O4-
11
12 Fe3O4 nanocomposites using off- stoichiometric ratios of Co and Fe which may find potential application
13
14 in the field of permanent magnet with excellent optical properties. The core–shell NPs also showed good
15
magnetic recoverable photo-catalytic activity towards reduction of phenolphthalein under UV light
16
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17 irradiation and was magnetically recoverable and reusable. Also, the nanocomposite was demonstrated to
18
19 be an efficient nano heater for hyperthermia application with moderate SAR value.
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5. Acknowledgements: Financial support from DST (India) for TEM facility at CIF, IIT Guwahati (Grant
No. SR/S5/NM-01/2005) is gratefully acknowledged. The authors would also like to acknowledge the
support from IITGuwahati and NIT Nagaland for the analytical facilities during the course of
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29 investigations.
30
31
32
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29 Figure Caption:
30
31 1. Figure 1(a). Bright field TEM images and (b) HRTEM images of CoFe2O4-Fe3O4 asprepared
32
33 nanocomposite for Fe/Co=2.3.
34
2. Figure 1(c). Bright field TEM images and (d) HRTEM images of CoFe2O4-Fe3O4 asprepared
35
37
38 3. Figure 2. IR spectra of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x) varying from to 2.3 to
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40 3.5.
41 4. Figure 3. DSC/TGA analysis of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios ( x = 3.5).
42
43 5. Figure 4(a). Absorption spectra of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x) varying
44
45 from to 2.3 to 3.5. Inset: 4(b) Band gap measurement of CoFe2O4-Fe3O4 nanocomposite with
46
Fe/Co ratios (x) varying from to 2.3 to 3.5.
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48 6. Figure 5. XRD pattern of CoFe2O4-Fe3O4 nanocomposite.
49
50 7. Figure 6(a). Bright field TEM images and 6(b) HRTEM images of CoFe2O4-Fe3O4 annealed
51
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53 8. Figure 6(c). Bright field TEM images and 6(d) HRTEM images of CoFe2O4-Fe3O4 annealed
54
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3 9. Figure 7(a). Particle size distribution and 7(b) SAED pattern of annealed CoFe2O4-Fe3O4
4
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5 nanocomposite with Fe/Co=3.5.
6
7 10. Figure 7(c). SAED pattern and 7(d) Particle size distribution of annealed CoFe2O4-Fe3O4
8
9
nanocomposite with Fe/Co=2.3.
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10 11. Figure 8. Schematic illustration of formation of the cobalt ferrite/ferric oxide core-shell
11
12 hetrostructure.
13
14 12. Figure 9. M-H curves of annealed CoFe2O4-Fe3O4 nanocomposite with Co/Fe ratios (x) varying
15
from to 2.3 to 3.5 measured at room temperature.
16
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17 13. Figure 10. M-H curves of annealed CoFe2O4-Fe3O4 nanocomposite with Co/Fe = 3.5 measured at
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19 low temperature (80K to 300K).
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21 14. Figure 11. Temperature dependence of Field-cooled (FC) and Zero-field cooled (ZFC)
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measured at 100Oe.
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magnetization curves of CoFe2O4-Fe3O4 nanocomposite with Fe/Co ratios (x = 2.3 and3.5)
15. Figure 12. UV-VIS absorption of phenolphthalein in the presence of CoFe2O4-Fe3O4 (x=3.5) under
uv irradiation at different time intervals.
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29 16. Figure 13. Recovery of CoFe2O4-Fe3O4 nanoparticle by applying an external magnetic field at the
30
31 end of the reaction.
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33 17. Figure 14: Induction heating curves of CoFe2O4-Fe3O4 as prepared nanocomposite for Fe/Co=3.5
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18. Figure 15 : Histogram of SAR values of nanocomposite with Fe/Co ratios 3.5
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40 1. Table 1. Vibrational band frequencies (ν1) and (ν2) of CoFe2O4-Fe3O4.
41 2. Table 2. Some physical parameters of CoFe2O4-Fe3O4 nanocomposite prepared by combined
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43 sonochemical and reverse co-precipitation method.
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CoFe2O4-Fe3O4 bimagnetic heterostructure: A versatile core-shell

Article in Materials Research Express · January 2020

Chandan Borgohain Jyoti Prasad borah

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39 Calorimetry (DSC)/Thermo-Gravimetric Analysis (TGA) analysis of the as prepared samples showed

53 FeCl3 (purity 97%) and sodium hydroxide NaOH (purity 96%).

53 Figure 5. XRD pattern of CoFe2O4-Fe3O4 nanocomposite

53 that phenolphthalein cannot be degraded under the present experimental condition.

39 irradiation at different time intervals

47 [6] K. V. P. M. Shafi, A. Gedanken, R. Prozorov, J. Balogh, Chem. Mater. 10 (1998) 3445.

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