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Simple preparation and investigation of magnetic nanocomposites: Electrodeposition of polymeric aniline-barium ferrite and aniline-strontium ferrite thin films

  • Farzaneh Sharifi , Kambiz Hedayati EMAIL logo and Davood Ghanbari EMAIL logo
Published/Copyright: September 15, 2022
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Main Group Metal Chemistry
From the journal Main Group Metal Chemistry Volume 45 Issue 1

Abstract

In this work, new polymeric aniline-barium ferrite and aniline-strontium ferrite thin layers were synthesized. In the first step, hexaferrites nano-additives were prepared by applying ultra-sound and microwave irradiation. Then, hexaferrites were added to aniline electrolyte solution separately. The electrodeposition of aniline as a polymeric matrix and hexaferrite as nano-additives was performed in an electrochemical cell in the presence of various acids. Scanning electron microscopy images were applied for morphology investigation and measuring average particle size. Energy dispersive X-ray spectroscopy was applied for elemental detection and analysis, as well as presence confirmation of nanoparticles. Atomic force microscopy was applied for surface roughness analysis of thin films. Magnetic property of the nanoparticles and polymeric nanocomposites was checked and measured by vibrating sample magnetometer. The crystallinity, crystallite size, and phase of samples were confirmed by X-ray diffraction pattern analysis.

Keywords: conductive polymer; ultra-sound; microwave; magnetic properties

1 Introduction

Hexaferrite is usually a composition of divalent metals such as barium, strontium, or lead with iron oxide (general formula: MFe12O19), in terms of magnetic property they are part of ferromagnetic materials (Meng et al., 2016; Monsef and Salavati-Niasari, 2022; Xia et al., 2013). They are hard and brittle, and their color is gray or black. A natural magnet or magnetite is an example of a ferrite magnet that has been used to build a compass for centuries. They are widely used in a variety of industries for a variety of reasons, including their low price (Lahijani et al., 2018; Monsef et al., 2021). In terms of material structure, ferrites are polycrystalline materials. This means that they are composed of a large number of tiny crystals with different orientations (Ahmadian-Fard-Fini et al., 2018; Panahi-Kalamuei et al., 2015; Sadeghpour et al., 2022). In terms of crystal structure, ferrites are of different types, such as spinel, garnet, perovskite, and hexagonal ferrites. Three main families of ferrites are used to make magnets: hexagonal ferrites, spinel ferrites, and garnet ferrites. Their crystal structure is in the form of a hexagonal or hexagonal prism with a vertical axis (Hajian Karahroudi et al., 2020). The magnetization of the material along this vertical axis is easier than other axes. For this reason, these ferrites are magnetically considered to be hard magnetic materials, that is, the magnitude or direction of their magnetic field does not change easily, and they are therefore suitable for making permanent magnets. This family is also called “hexaferrite.” Hexaferrites are the main building blocks of permanent ferrite magnets (Masoumi et al., 2016; Gholami et al., 2017).

Electrodeposition is a controlled method for depositing different types of conductive and semiconductor layers. In this method, three electrodes are used, the work electrode is a local in which the target material is layered by gaining or losing electrons. A reference electrode is used to control the potential between the working electrode and the electrolyte, and a secondary electrode must be used to complete the electrical circuit (Davar et al., 2010; Sadeghi et al., 2018; Song et al., 2019; Zinatloo-Ajabshir et al., 2018).

In electrochemical polymerization technique, thickness and morphology of thin layers can be controlled by adjusting the density of current and potential. Electrochemical polymerization could be an economical and environmental technique because no toxic, complex, and expensive compounds are required (Hassanpour et al., 2017; Nautiyal and Parida, 2016; Zinatloo-Ajabshir and Salavati-Niasari, 2019). Various parameters will affect the electro-deposition, such as temperature, acidity, concentration, and crystal structure of substrate (Abdelraheem et al., 2018; Fleaca et al., 2016; He et al., 2015).

2 Results and discussion

Figure 1a illustrates scanning electron microscopy (SEM) images of barium hexaferrite that were achieved by sono-chemistry method irradiation under 200 W power for 25 min (on: 3 s, off: 3 s), as can be argued from the pictures, homogeneous nanoparticles of close size with an average diameter of 40  nm have been obtained. Figure 1b illustrates SEM images of barium ferrite synthesized with the help of microwave irradiation; as results confirm, uniform hexagonal plate of hexaferrite were achieved. Figure 1c depicts the morphology of strontium ferrite that were obtained applying ultrasound irradiation (100 W, 60 min), nano-products with an average size less than 100 nm were obtained. Figure 1d shows images of SrFe12O19 that were achieved by 600 W power microwave irradiation; it is perceived from the pictures that products with rods morphology were prepared. These images determine that all ferrites nanoparticles are in the nanoscale range.

Figure 1 FESEM images of barium ferrite by (a) sono-chemical method and (b) microwave method. FESEM images of strontium ferrite nanoparticles by (c) sono-chemical method and (d) microwave method.
Figure 1

FESEM images of barium ferrite by (a) sono-chemical method and (b) microwave method. FESEM images of strontium ferrite nanoparticles by (c) sono-chemical method and (d) microwave method.

Figure 2 shows the morphology of polymeric aniline-barium ferrite thin layer for the 5–20 cycles of electrodeposition, Figure 2a illustrates needle like surface morphology, the presence of nano-additives in all three polyaniline-barium ferrite thin layer are approved. As shown in Figure 2b and c the grain and thickness of layers enhance with increase in the number of cycles.

Figure 2 FESEM images of polyaniline-barium ferrite with (a) 5, (b) 10, and (c) 20 cycles of electrodeposition.
Figure 2

FESEM images of polyaniline-barium ferrite with (a) 5, (b) 10, and (c) 20 cycles of electrodeposition.

Figure 3a–c shows surface roughness of the polyaniline-SrFe12O19 thin layer composite for the 5–20 cycles of electrodeposition. In Figure 3, can be seen composite with more circles have more particles rather to composite. On examining the morphology, it is seen that the SrFe12O19 particles are uniform in the polyaniline films and the thicker layers have bigger grains in the polyaniline.

Figure 3 FESEM images of polyaniline-strontium ferrite with (a) 5, (b) 10, and (c) 20 cycles of electrodeposition.
Figure 3

FESEM images of polyaniline-strontium ferrite with (a) 5, (b) 10, and (c) 20 cycles of electrodeposition.

Figure 4a shows Energy dispersive X-ray (EDX) analysis for barium ferrite and Figure 4b shows strontium ferrite nano-powder. In the EDX spectra, there are related elements of each ferrite. Figure 5a shows the elemental map of polyaniline film via ten cycles of electrodeposition. The map shows the elements N, O, and C monotonic dispensation in polymer. Figure 5b shows the map of polyaniline film on copper substrate.

Figure 4 XED analysis of (a) barium ferrite and (b) strontium ferrite.
Figure 4

XED analysis of (a) barium ferrite and (b) strontium ferrite.

Figure 5 X-ray element distribution maps (MAP) analysis of (a) polyaniline/barium ferrite nanocomposite and (b) polyaniline-barium ferrite on the copper substrate.
Figure 5

X-ray element distribution maps (MAP) analysis of (a) polyaniline/barium ferrite nanocomposite and (b) polyaniline-barium ferrite on the copper substrate.

The phase structure was approved by X-ray diffraction (XRD) (Philips, X’Pert Pro), (CuKα radiation, λ = 0.154 nm). Figure 6a shows the XRD pattern of BaFe12O19 nanocrystals. The XRD diagram showing the BaFe12O19 peaks has a good appraise by BaFe12O19 standard peaks (Ebrahimi et al., 2017).

Figure 6 XRD pattern for (a) barium ferrite and (b) strontium ferrite nanoparticles.
Figure 6

XRD pattern for (a) barium ferrite and (b) strontium ferrite nanoparticles.

Figure 6b indicates the XRD peaks of SrFe12O19 nanocrystals. The XRD diagram complies with the standard samples (Hajian Karahroudi et al., 2020).

The crystallite size of ferrites calculated via Debye–Scherrer equation (Eq. 1):

(1) t = 0 . 9 λ β cos θ

where β is the width of peaks in half maximum intensity, λ is 1.54 Å, θ is the angle of diffraction, and t is the size of crystallite (Abbasi et al., 2021). The crystallite size of SrFe12O19 nanoparticles was calculated to be 34 nm and BaFe12O19 nanoparticles was calculated to be 28 nm.

The Williamson–Hall formula calculates the crystallite size and strain of the crystal lattice:

(2) β cos θ = 4 ε sin θ + 0 . 9 λ D

where ε is lattice strain and β, θ, and λ are the same as in Eq. 1 (Abbasi et al., 2021). The crystallite size of BaFe12O19 and SrFe12O19 nanoparticles using Williamson–Hall method was calculated to be 25 and 32, respectively. The lattice strain of BaFe12O19 and SrFe12O19 was calculated to be 0.011 and 0.015, respectively.

Roughness is checked on the surface of many materials and thin layers. The roughness or kinetic roughening for layers depended to time of deposition or thickness of films. The roughness (w) is indicated by Eq. 3:

(3) w = 〈 [ h − 〈 h 〉 ] 2 〉

where h is the height of different points on the sample surface. In Family-Vicsek scaling assumption, roughness is expressed during short and long scan lengths with the following relations (Eqs. 4 and 5):

(4) w ∝ l H , l ≪ l c

(5) w ∝ t β , l ≫ l c

where H, l c , and β are Hurst coefficient, crossover length, and growth exponent, respectively. The anomalous scaling systems are explained via the following relations (Eqs. 6 and 7):

(6) w ∝ l H t β loc , l ≪ l c

(7) w ∝ t β + β loc , l ≫ l c

where β loc is the local roughness exponent (Hedayati, 2015).

The roughness of polyaniline/(SrFe12O19 and BaFe12O19) films was investigated by atomic force microscopy (AFM). The AFM images of BaFe12O19 and polyaniline composites in cycles of 5, 10, and 20 are shown in Figure 7a–c.

Figure 7 AFM images of thin layer of polyaniline/barium ferrite nanocomposite with (a) 5, (b) 10, and (c) 20 cycles of deposition.
Figure 7

AFM images of thin layer of polyaniline/barium ferrite nanocomposite with (a) 5, (b) 10, and (c) 20 cycles of deposition.

Figure 8a–c show the AFM image for polyaniline-SrFe12O19 thin layer for 5,10, and 20 cycles, respectively. The logarithmic curve of roughness vs length scale of deposited BaFe12O19-polyaniline thin films with 5–20 cycles is depicted in Figure 9a.

Figure 8 AFM images of thin layer of polyaniline/strontium ferrite nanocomposite with (a) 5, (b) 10, and (c) 20 cycles of deposition.
Figure 8

AFM images of thin layer of polyaniline/strontium ferrite nanocomposite with (a) 5, (b) 10, and (c) 20 cycles of deposition.

Figure 9 The roughness-scan length diagram in logarithmic scale for thin layer of (a) polyaniline/barium ferrite and (b) polyaniline/strontium ferrite nanocomposite with 5, 10, and 20 cycles of deposition.
Figure 9

The roughness-scan length diagram in logarithmic scale for thin layer of (a) polyaniline/barium ferrite and (b) polyaniline/strontium ferrite nanocomposite with 5, 10, and 20 cycles of deposition.

Figure 9b shows logarithmic curve of the roughness and length scale deposited SrFe12O19-polyaniline layers via 5, 10, and 20 cycles. The diagrams of Figure 9a and b show that both SrFe12O19- and BaFe12O19-polyaniline layers have anomalous scaling treatment. According to these images, with increase in the deposition cycles, the roughness increases.

The magnetic hysteresis curve of composite films investigated via vibrating sample magnetometer (VSM) at room temperature. Figure 10a and b indicate the VSM loop for BaFe12O19 and SrFe12O19 nanocrystals, respectively. The remanence and saturation magnetization and coercivity of nano powders are described in Table 1. These loops demonstrate that BaFe12O19 and SrFe12O19 are ferromagnetic and BaFe12O19 is harder than SrFe12O19.

Figure 10 Hysteresis loop for (a) barium ferrite and (b) strontium ferrite nanoparticles.
Figure 10

Hysteresis loop for (a) barium ferrite and (b) strontium ferrite nanoparticles.

Table 1

Mr, Ms, and Hc for magnetic nanoparticles

Coercivity (Oe) Saturation magnetization (emu‧g−1) Remanence magnetization (emu‧g−1) Nanoparticles
2,000 64.66 33.94 Barium ferrite
1,000 51.79 25.36 Strontium ferrite
3,000 2.09 0.87 Polyaniline/barium ferrite
0 3.75 0.01 Polyaniline/strontium ferrite

Figure 11a represents magnetic loop of BaFe12O19-polyaniline (ten cycles) composite in parallel field. The hysteresis loop of SrFe12O19-polyaniline (ten cycles) is shown in Figure 11b. For polyaniline-BaFe12O19, amount of Ms and Mr decreased compared to that of BaFe12O19 but Hc increased. In comparison to SrFe12O19-polyaniline vs SrFe12O19, amount of Ms, Mr, and Hc is decreased and SrFe12O19-polyaniline have super-paramagnetic behavior.

Figure 11 Hysteresis loop for (a) polyaniline/barium ferrite and (b) polyaniline/strontium ferrite thin layer composite in parallel field.
Figure 11

Hysteresis loop for (a) polyaniline/barium ferrite and (b) polyaniline/strontium ferrite thin layer composite in parallel field.

3 Conclusion

BaFe12O19 and SrFe12O19 nanoparticles were manufactured by both microwave irradiation and sono-chemical method. The ferrites-polyaniline nanocomposite films were grown by electrodeposition technique. SEM images showed that the grain size increased via increasing the film thickness. The EDX spectra indicated related peaks of BaFe12O19- and SrFe12O19-polyaniline. XRD analysis illustrated the crystalline structure of BaFe12O19 and SrFe12O19. The strain of lattice and crystallite size of BaFe12O19 and SrFe12O19 were computed via Debye–Scherrer equation and Williamson–Hall method. The computed crystallite size of BaFe12O19 and SrFe12O19 nanoparticles is in agreement with the observed SEM grain size. Kinetic roughening of BaFe12O19- and SrFe12O19-polyaniline composite films was anomalous scaling treatment. The magnetic loop indicated that BaFe12O19, SrFe12O19, and BaFe12O19-polyaniline are ferromagnetic, but SrFe12O19-polyaniline is super-paramagnetic.

Experimental method

Preparation of hexaferrite nanoparticles

Strontium nitrate, barium nitrate, iron nitrate, aniline, and sodium hydroxide were purchased from Sigma-Aldrich and Merck (Germany) and all materials have a purity above 99%. For synthesized strontium ferrite, 0.01 mol of strontium sulfate hydrate and 0.12 mol of iron nitrate were dissolved in 200 mL of deionized water. The solution was placed under microwave irradiation (900 W, on: 30 s, off: 30 s) for 30 min. Then, the pH of the prepared solution was increased to 10 by 20 mL of sodium hydroxide (1 M) solution. After that the solution was microwave irradiated for 10 min. 0.01 mol of Ba(NO3)2 and 0.12 mol of Fe(NO3)3‧9H2O were added to 50 mL of deionized water. By adding 15 mL of 1 M NaOH solution, alkalinity was increased to 10. The solution was placed under microwave irradiation (900 W, on: 30 s, off: 30 s) for 30 min. After precipitation and washing, the product was placed at 800°C for 2 h.

For sono-chemical synthesis, all chemical precursors were used as the same as microwave irradiation with the difference that ultra sound irradiation (400 W, 30 min) was used instead of microwave irradiation.

Polyaniline/barium ferrite and strontium ferrite composites

Aniline thin layers were deposited on copper substrate by cyclic voltammetry technique in various number of cycles from 5 to 20. Sulfuric acid (0.2 M) solution and aniline (0.1 M) were used as electrolyte. The voltage applied at this stage ranged from −0.2 to 1.2 V. The substrates were prepared by two-step mechanical and electrochemical polishing. For electroporation, 0.1 g of each ferrite were added to 100 mL of electrolyte

  1. Funding information: The project was financially supported by the Ministry of Science, Research and Technology, under grant number 299901000108.

  2. Author contributions: Farzaneh Sharifi: writing – original draft, and formal analysis; Kambiz Hedayati: writing – original draft, writing – review and editing, formal analysis, visualization, and project administration; Davood Ghanbari: writing – original draft, writing – review and editing, methodology, and formal analysis.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: All relevant data are included in the article.

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Received: 2022-03-11
Revised: 2022-09-02
Accepted: 2022-07-20
Published Online: 2022-09-15

© 2022 Farzaneh Sharifi et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/mgmc-2022-0019
Keywords for this article
conductive polymer; ultra-sound; microwave; magnetic properties
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  19. Special Issue: Theoretical and computational aspects of graph-theoretic methods in modern-day chemistry (Guest Editors: Muhammad Imran and Muhammad Javaid)
  20. Computation of edge- and vertex-degree-based topological indices for tetrahedral sheets of clay minerals
  21. Structures devised by the generalizations of two graph operations and their topological descriptors
  22. On topological indices of zinc-based metal organic frameworks
  23. On computation of the reduced reverse degree and neighbourhood degree sum-based topological indices for metal-organic frameworks
  24. An estimation of HOMO–LUMO gap for a class of molecular graphs
  25. On k-regular edge connectivity of chemical graphs
  26. On arithmetic–geometric eigenvalues of graphs
  27. Mostar index of graphs associated to groups
  28. On topological polynomials and indices for metal-organic and cuboctahedral bimetallic networks
  29. Finite vertex-based resolvability of supramolecular chain in dialkyltin
  30. Expressions for Mostar and weighted Mostar invariants in a chemical structure
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