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Vol. 9. Issue 2.
Pages 2513-2521 (March - April 2020)
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Vol. 9. Issue 2.
Pages 2513-2521 (March - April 2020)
Original Article
DOI: 10.1016/j.jmrt.2019.12.082
Open Access
Facile preparation and enhanced electromagnetic wave absorption properties of Fe3O4 @PVDF nanocomposite
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Lawal Lanre Adebayoa,
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adebayolawallanre@yahoo.com

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, Hassan Soleimania,
Corresponding author
hassan.soleimani@utp.edu.my

Corresponding authors.
, Noorhana Yahyaa, Zulkifly Abbasb, Maziyar Sabetc, Fatai Adisa Wahaaba, Ridwan Tobi Ayinlaa
a Fundamental and Applied Science Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, Perak Darul Ridzuan, 32610, Malaysia
b Department of Physics, Faculty of Science, Universiti Pultra Malaysia, UPM Serdang, Selangor Darul Ehsan, 43400, Malaysia
c Petroleum and Chemical Engineering, Universiti Teknologi Brunei (UTB), Bandar Seri Begawan, BE1410, Brunei Darussalam
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Abstract

Fabrication and investigation of microwave absorbing materials have been widely explored to mitigate the emerging EM pollution. In this study, we prepared magnetite (Fe3O4) nanoparticles via a rare facile sol–gel method followed by a calcination process. Then, Fe3O4 and polyvinylidene fluoride (Fe3O4@PVDF) nanocomposite were prepared and the electromagnetic wave absorption (EMWA) properties were studied using the finite element method. Characterization techniques employed in this study include; X-ray diffraction, Fourier-transform infrared spectroscopy (FTIR), vibrating sample magnetometer (VSM), Field emission scanning electron microscopy (FESEM) and Transmission electron microscopy (TEM). The microwave absorption properties of Fe3O4@PVDF were studied at the X-band (8.2–12.4 GHz) and Ku-band (12.4–18 GHz) frequency range. The Fe3O4@PVDF nanocomposite displayed minimum reflection loss of −62.7 dB at 16.9 GHz for 3.5 mm thick sample. These outstanding EMWA coefficients could be attributed to favorable impedance match from outstanding dielectric and magnetic loss mechanisms.

Keywords:
Microwave absorption property
Magnetite nanoparticles
PVDF
Reflection loss
Full Text
1Introduction

The recent advances and massive utilization of wireless devices that function at microwave frequency range is a major factor leading to the incessant growth in electromagnetic (EM) pollution that endangers human health [1,2]. Another emerging issue is the EM interference with precise electronic equipment operating at the super-high frequency [3–5]. Therefore, it is pertinent to develop technologies to tackle this problem, among which fabrication of novel materials with high electromagnetic wave absorption (EMWA) properties has been proposed as one effective way [6–8]. Features of an ideal EM wave absorbing materials include strong absorption, thin thickness, light-weight, low cost and wide absorption bandwidth [9–11]. Conventional EM wave absorbing materials such as ceramics, natural graphite, ferrites, and their alloys have been extensively explored [12–14]. However, an efficient absorptive material is anticipated to dissipate the EM wave via magnetic and dielectric dissipation. To achieve strong magnetic dissipation, a typical representative of ferrites, magnetite (Fe3O4) has attracted much interest as a result of its outstanding permeability and permittivity which promotes high EM wave absorption. Furthermore, it has proper saturation magnetization (Ms), easy processability and low cost of production [15–17]. Nonetheless, the rapid drop in permeability at high frequency, mismatch of impedance, easy oxidation, large absorber thickness, and high density are limiting factors affecting efficiency of Fe3O4 as an ideal absorptive material [3,18].

To improve the EM wave absorption performance of Fe3O4, concerted research efforts have been explored and reported. According to literature, widely employed optimizing strategies can be divided into four. First, fabrication of hierarchical nanostructure with core-shell/yolk-shell structures such as core-shell Fe3O4/C microspheres [19], PAN@ Fe3O4[20], Fe3O4@SiO2@PPy [21], yolk-shell Fe3O4@mSiO2 and octahedral Fe3O4 nanostructure [22]. This method typically involves coating Fe3O4 with organic or inorganic shells, resulting in a heterogeneous interface and unique structure which enhances the EMWA. The second approach involves size reduction of the Fe3O4 to nanoscale [23,24]. In this technique, the prepared Fe3O4 nanoparticles usually occur in single domain, hence, the ferromagnetic resonance increases absorption which promotes EMWA. The third method entails fabrication of porous Fe3O4 nanostructure [25] to promote multiple scattering and attenuation of EM wave resulting in improved microwave absorption performance. The last technique involves composite formation of Fe3O4 and a dielectric material such as carbon-based materials. Also, composite formation of Fe3O4 with conductive polymers such as Polypyrrole [26], Poly (3,4 ethylenedioxythiophene) [27], Polyaniline [28], etc. presents numerous merits beyond strong absorption, low density, and environmental stability. Among the conductive polymers with properties favorable for practical EMWA applications, polyvinylidene fluoride (PVDF) have unique properties which include flexibility, low density, and resistance to heat and chemical corrosion [29]. Due to these advantages, PVDF has been used to prepare composites in the field of EMWA [30–32].

In this study, Fe3O4 nanoparticles prepared by the facile sol–gel method were combined with PVDF via in-situ solvent mixing method. Several characterization technique was used to study the physiochemical properties of the sample. The effect of the morphology and nanostructure of the sample on the EMWA performance was analyzed and presented. In fact, the Fe3O4 nanoparticles prepared in this study posseses low dimensions which help reduce the eddy current loss and enhance the EMWA performance. The Fe3O4@PVDF nanocomposites display superior microwave absorption performance at Ku band frequency range exhibiting a minimum reflection loss (RL) value of −62.7 dB at 16.9 GHz, with an optimal absorber thickness of 3.5 mm. This high EMWA performance by the sample can be accredited to outstanding dielectric and magnetic loss mechanism, and good impedance matching. The synergistic effect between Fe3O4 as a strong magnetic material and PVDF as a dielectric matrix was beneficial for enhancing the microwave absorption performance of the resultant composite.

2Methodology2.1Synthesis of Fe3O4

Iron (III) nitrate nonahydrate (Fe3(NO3)3.9H2O), citric acid monohydrate (C6H8O7.H2O) were purchased from R & M chemicals. The chemicals were analytical grade and used as collected without further purification. The Fe3O4 was prepared by a facile sol–gel method and high temperature calcination. Typically, 1 mol of Fe3(NO3)3.9H2O was dissolved in double distilled water and the solution was stirred at 500 rpm for 30 min at 80 °C. Then, 1 mol of C6H8O7.H2O was added dropwise to the solution under the same temperature and stirring rate. The solution was allowed to stir continuously until gel formation. The resulting gel was dried in an oven at 90 °C for 2 h. The product was crushed into powder and calcinated at 200 °C for 2 h in a tube furnace.

2.2Preparation of Fe3O4@PVDF nanocomposites

5g of PVDF pellets were poured into 20 mL NMP solution and stirred vigorously at 150 °C for 90 min to make the PVDF solution. Then Fe3O4 nanoparticles were subsequently dispersed in the prepared solution with a mass ratio of 50 wt %. For homogenous dispersion, the mixture was vigorously stirred for 45 min using an electric stirrer. Afterward, the composite was poured in a bath of clean water and allowed to solidify and finally dried in an oven.

2.3Characterizations

The crystallinity and phase composition was studied using X-ray diffraction (XRD) spectrometer with Cu Kα radiation (λ = 0.15406 nm, 40 mA and 45 kV). The morphology and nanostructure images were obtained using field emission scanning electron microscopy (FESEM) with an accelerating voltage of 15 KV. To investigate structural properties, transmission electron microscopy (TEM) was performed on a JEOL JEM 2010 F at 200 kV.Vibrating sample magnetometer (VSM, Lakeshore Model 648 series) was used to study the magnetic properties of the Fe3O4 nanoparticles at room temperature. The chemical bonds were investigated using Fourier-transform infrared spectroscopy (FTIR) to further confirm the formation of Fe3O4. To measure the EM parameters, the Fe3O4@PVDF nanocomposite was compressed by hot pressing at 200 °C into a rectangular form with dimensions 10.16 × 22.86 mm3 for measurements at X-band frequency and 7.90 × 15.80 mm3 for Ku-band frequency. The samples were snugly fitted into the WR-90 and WR62 waveguides of Keysite E5071C vector network analyzer (VNA) for measurement. The VNA calibration was implemented using a typical two-port calibration procedure for equally spaced frequency points.

2.4EMWA simulation

The EMWA properties of the Fe3O4@PVDF sample placed in a rectangular waveguide was studied with COMSOL multiphysics. In setting up the geometry, a cross-section of the WR90 and WR62 rectangular waveguides was built in two dimensions (2D). Then, the 2D geometry was extruded into depth with a finite number of layers in 3D. The 3D rectangular waveguide was divided into three domains. Domains 1 and 3 were filled with air, as the rectangular waveguide is a hollow structure. Then, the synthesized Fe3O4@PVDF nanocomposite of known relative permittivity and permeability values was filled in domain 2. All boundaries of the waveguides were modeled as a perfect electric conductor apart from two boundaries marked as port 1 and port 2 for wave excitation. So a mesh consisting of tetrahedral elements was generated using a user-controlled mesh. The fundamental TE10 mode with the least cut-off frequency that can propagate through a rectangular waveguide was used in this study, employing two-port wave excitation. Applying this module and two-port boundary conditions, the scattering parameters and reflection loss were computed. The EM field distribution within the rectangular waveguide was obtained using FEM formulation.

3Results and discussion3.1Structural and morphological analysis

The XRD pattern shown in Fig. 1a presents the crystal structure of the synthesized Fe3O4 nanoparticles. The XRD spectrum exhibit diffraction which corresponds to the (111), (220), (311), (400), (422), (511), (440), and (533) crystal planes of Fe3O4. These peaks match with an earlier report (JCPDS file no. 19-0629) in the crystallographic database. The fitted image shows that no other diffraction peak is present in the sample which confirms the pure crystalline phase of the prepared Fe3O4. From the XRD pattern, the average crystal size of the Fe3O4 nanoparticles was calculated as 7.5 nm using Scherrer equation. FTIR analysis presented in Fig. 1b shows a strong peak at 631.26 cm−1, 566.20 cm−1 and a weak one at 448.31 cm−1 which can be ascribed to the stretching of FeO stretching [33]. The broad peak around 3400.96 cm−1 is the vibrational characteristics of the hydroxyl functional group (−OH) [34]. These analyses confirm the sample as Fe3O4.

Fig. 1.

(a) XRD pattern and (b) FT-IR spectra of Fe3O4 nanoparticles.

(0.17MB).

The morphology and nanostructure of the Fe3O4 nanoparticles were studied using FESEM as presented in Fig. 2. The FESEM image shows the compacted nature of the Fe3O4 nanoparticles having spherical nanostructure and highly agglomerated. A possible explanation for the agglomeration could be the strong magnetic attraction among the Fe3O4 nanoparticles. Also, it may be due to strong inter-particle Van der Waals force among the Fe3O4 nanoparticles. The FESEM image of the Fe3O4@PVDF nanocomposite presented in Fig. 2b confirms firm attachment of the Fe3O4 nanoparticles to the PVDF matrix. This favorable attachment could provide interfacial polarization at the interface of Fe3O4 and PVDF and therefore favor the attenuation of the EM wave. To obtain detail structural information, TEM and HR-TEM were used to further characterize the sample. Fig. 2c and d reveals that the Fe3O4 nanoparticles are highly compacted and composed of small crystals with spherical morphology. The HR-TEM image shown in Fig. 2e reveals an interplanar spacing of 0.261 nm which could be attributed to the (311) plane of Fe3O4. Fig. 2f shows the selected area electron diffraction (SAED) of the sample. The rings in the SAED pattern can be well assigned to the (220), (311), (400), (422), and (440) planes of Fe3O4, which aligns with the XRD results.

Fig. 2.

FESEM image of (a) Fe3O4 nanoparticles, (b) Fe3O4@PVDF nanocomposite, (c,d) TEM image of Fe3O4 nanoparticles, (e) HR-TEM image, and (f) SAED pattern of Fe3O4 nanoparticles.

(0.76MB).
3.2Magnetic properties of Fe3O4 nanoparticles

Fig. 3 presents the room temperature magnetic properties of the Fe3O4 nanoparticles. The measured saturation magnetization (Ms) value of the synthesized Fe3O4 is 44.85 emu/g at room temperature. While the coercivity (Hc) was measured as 26.66 Oe which can be observed in the enlarged hysteresis curve inserted in Fig. 3. It is reported that the particle size and shape can strongly influence the Hc value [3]. Therefore, the low Ms and Hc values can be linked to the small particle size of the synthesized Fe3O4[35]. Nevertheless, this magnetic moment confirms the ferromagnetic nature of the Fe3O4 nanoparticles with the ability to attenuate EM waves [36].

Fig. 3.

Hysteresis loop of the Fe3O4 nanoparticles inset is the magnified low field hysteresis curve.

(0.12MB).
3.3EM wave absorption properties

The complex relative permittivity  (εr=ε׳-jε׳׳) and permeability (μr=μ׳-jμ׳׳) were measured from 8.2 to 18 GHz. Using the measured EM properties, the EMWA properties represented by reflection loss (RL) of the Fe3O4@PVDF nanocomposite were calculated from Eqs. (1) and (2) below based on the transmission line theory [37].

where εr, µr, c, f, d, Zo, and Zin are the relative complex permittivity and permeability, the velocity of EM wave in vacuum, microwave frequency, absorber thickness, impedance of free space, and characteristic impedance of the absorptive material, respectively. Generally, when RL values are below −10 dB or −20 dB, 90% or 99% of EM wave could be absorbed respectively [38]. The operating bandwidth of the absorptive material is the frequency range corresponding to this reflection loss (RL<-10 dB) in a fixed absorber thickness [39]. The frequency dependence RL curves for the Fe3O4@PVDF nanocomposite at thicknesses of 3.0–6.0 mm in a frequency range 8.2−18 GHz are presented in Fig. 4. Within X-band frequency, a minimum RL value of −43.3 dB was achieved at 9.7 GHz with a thickness of 6.0 mm. Also, a minimum RL value of −43.7 dB was achieved at 10.8 GHz with a thickness of 5.5 mm and a minimum RL value of −67.3 dB was achieved at 11.8 GHz with a relatively large absorber thickness of 5.0 mm. At Ku-band frequency, the minimum RL values at an absorber thickness of 3.5, 4.0, and 4.5 mm are −63.7, −45.9, and −51.66 dB at frequencies 16.6, 14.7, and 13.2 GHz, respectively, which corresponds to above 99 % EM wave absorption. The operating bandwidth can cover 9.2−18 GHz by tuning the absorber thickness from 3.5 to 6 mm. This result agrees with the quarter-wavelength regulation that the peak frequency shifts to higher frequencies as thickness reduces [19].

Fig. 4.

Frequency dependence reflection loss curve of Fe3O4@PVDF nanocomposites with varying thickness in the range of 8.2−18 GHz.

(0.18MB).

To investigate the likely mechanism for the outstanding MAP of Fe3O4@PVDF, the EM parameters were studied. The real parts of permeability and permittivity (µ׳and ε׳) denote the magnetic and electric energy storage ability, while the imaginary parts (µ׳׳and ε׳׳) represent the dissipative abilities of both energies [39]. Fig. 5a presents the real (ε׳) and imaginary (ε׳׳) parts of complex permittivities of Fe3O4@PVDF nanocomposite and Fe3O4 nanoparticles over the 8.2–18 GHz frequency range. The ε׳ and ε׳׳ values of Fe3O4 nanoparticles are in the range of 1.1–3.8 and 0.14–0.7, respectively, which show poor dielectric loss properties. The ε׳ and ε׳׳ of the Fe3O4@PVDF increases with the Fe3O4 filled in the PVDF matrix. This improvement could be linked with improved conductivities, and this also shows consistency with the effective medium theory [40] The ε׳ and ε׳׳ decreased slowly as frequency increases displaying a unique frequency dispersion reported in some Fe3O4 based composites [41–43]. This behavior ensues due to lack of dipoles to quickly respond and align with the high frequency alternating EM Field, thereby resulting to decrease in ε׳ and ε׳׳ [44]. Interestingly, the ε׳ and ε׳׳ value of Fe3O4@PVDF nanocomposite vary with several resonance peaks as frequency increases. This can be attributed to the interfacial polarization mechanism between Fe3O4 nanoparticles and PVDF matrix. The degree of polarization of the composite increases due to the synergistic effect of Fe3O4 and PVDF, resulting in enhanced dielectric loss. Fig. 5b shows the µ׳ and µ׳׳ values of the Fe3O4@PVDF nanocomposite and Fe3O4 nanoparticles. The values of µ׳ and µ׳׳ of Fe3O4 are approximately unity and zero, respectively. While, for the composite, the µ׳ and µ׳׳ are in the range of 0.9–1.25 and 0.7–1.1, respectively. These findings reveal that the PVDF matrix does not contribute to the magnetic loss. As the µ׳ and µ׳׳ values of the composites tend to remain constant over the studied frequency range. This reveals that the composite of Fe3O4 and PVDF reported in this work could effectively overcome the traditional Snoek’s limit of Fe3O4.

Fig. 5.

(a) Complex permittivities and (b) permeabilities of Fe3O4@PVDF composite and Fe3O4 nanoparticles.

(0.23MB).

The dielectric and magnetic losses can be evaluated by the dielectric loss tangent (tanδε) and magnetic loss tangent (tanδµ). Fig. 6 presents the dielectric and magnetic loss ( tanδε and  tanδμ ) tangents of Fe3O4@PVDF. It can be seen that the magnitude of  tanδε in the range of 0.34–0.9 are much higher than that of  tanδμ over the whole studied frequency range. To investigate the dielectric loss mechanism of the Fe3O4@PVDF, Debye dipolar relaxation model was utilized. The correlation between ε׳ and ε׳׳ according to this model can be expressed as follows:

where  εs, τ, ω = 2πf, and  ε∞ denotes the static permittivity, relaxation time, angular frequency, and relative permittivity at the high-frequency limit. According to this model, the plot of ε׳׳ against ε׳ (Cole-Cole plots) will show a semi-circle which denotes a polarization process [45]. As shown in Fig. 7a, the Cole-Cole plots of Fe3O4@PVDF nanocomposite show quite a few semi-circles. These findings may be ascribed to the small crystallite size of the Fe3O4 nanoparticles. The enormous heterogeneous interfaces between Fe3O4 and PVDF can also induce strong interfacial and multiple polarization loss mechanisms [32]. In addition, as the semicircles are several distorted, this suggests the presence of a different loss mechanism asides polarization e.g. conduction loss, promoting the dielectric loss mechanism [46].

Fig. 6.

The loss tangents of Fe3O4@PVDF.

(0.12MB).
Fig. 7.

(a) Cole-Cole plot and (b) Frequency dependence of Co=μιιμι-2f-1 values of Fe3O4@PVDF.

(0.12MB).

The magnetic loss (tan⁡δμ) dissipation occurs due to relaxation processes during magnetization, such as domain wall resonance, natural resonance, hysteresis loss, and eddy current resonance [3]. The domain wall resonates and hysteresis loss can be excluded in the microwave frequency range as the former often occurs at low-frequency, and the latter is mostly negligible in a weak magnetization field [47]. Hence, ferromagnetic resonance and eddy current may be responsible for the attenuation of EM wave by magnetic loss mechanism at X-band and Ku-band frequency range. Magnetic loss from eddy current is often investigated by analyzing the variation of Co=μ׳׳μ׳-2f-1 with frequency. If the variation of Co remains constant with increase in frequency, then the magnetic loss mechanism originates from eddy current resonance [48]. As presented in Fig. 7b, the Co values of the of Fe3O4@PVDF nanocomposite tend to remain constant at X-band frequency but vary significantly at Ku-band frequency range. Hence, this analysis suggests that attenuation of EM wave by magnetic loss is from natural ferromagnetic resonance and not from eddy current resonance. The presence of resonance peaks in the tan⁡δμ curve presented in Fig. 6 also suggests that the magnetic loss originates from ferromagnetic resonance.

3.4EM energy density analysis

Fig. 8 presents the three-dimensional (3D) volume plot of the simulated rectangular waveguide with COMSOL multiphysics.

Fig. 8.

3D plot illustrating ((a) and (b )) simulated EM energy density of rectangular waveguide comprising 3.5 mm thick sample at selected frequencies (8.2 GHz and 16.9 GHz), and ((a)׳ and (b׳)) corresponding magnified view of waveguide region filled with samples.

(0.37MB).

The distribution of the EM energy density within the rectangular wave loaded with sample (3.5 mm thick) is illustrated in the figure. The EM energy density within the WR90 waveguide at 8.2 GHz was determined as 86.7 µJ/m3 (Fig. 8a). Evidently, the EM energy within the section filled with the Fe3O4@PVDF sample at this frequency was less dense, with a value of 37.7 µJ/m3 (Fig. 8a׳) resulting in poor RL value of −1.05 dB. Whereas, the density of the EM energy within the WR62 waveguide at 16.9 GHz (Fig. 8b) was 2600 µJ/m3 (Fig. 8b). The total EM energy in the section filled with the Fe3O4@PVDF sample was evaluated as 2600 µJ/m3, resulting in high dissipation of EM energy with minimum RL value of −62.7 dB. This reveals that the EM wave achieves almost zero reflectivity at the interface of the sample, which can be ascribed to good match of impedance which results in a large fraction of the wave being propagated into the sample. The Fe3O4@PVDF nanocomposite thus possesses a low reflection coefficient which results from good impedance matching characteristics. The multiple scattering at the interface between Fe3O4 and PVDF can also provide multiple pathways to attenuate the EM wave [32]. Furthermore, the effective complementarities between the dielectric loss and magnetic loss contribute to the good impedance matching characteristics of the Fe3O4@PVDF nanocomposite.

4Conclusions

Fe3O4 nanoparticle has been successfully prepared through the sol–gel method and filled in PVDF matrix. XRD and FT-IR confirmed the formation of Fe3O4 nanoparticles. TEM and FESEM images reveal the spherical nanostructure of the Fe3O4 with no change in morphology after composite formation with PVDF. The Fe3O4@PVDF nanocomposite displays outstanding MAP with minimum RL value of -62.7 dB at 16.9 GHz, with an optimal absorber thickness of 3.5 mm. Finally, analysis of the EM energy density reveals that low reflection coefficient at an absorptive material interface is required for the material to dissipate large amount of the propagating EM wave. In addition to high dielectric and magnetic loss mechanism, the exceptional MAP of Fe3O4@PVDF nanocomposite can be attributed to proper impedance matching, good attenuation mechanism, and interfacial polarization.

Declaration of interests

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgement

The authors would like to acknowledge financial supports received from Universiti Teknologi PETRONAS through graduate assistance scheme and Yayasan Universiti Teknologi PETRONAS (YUTP) research grant with the cost center 015LC0-143.

Appendix A
Supplementary data

The following is Supplementary data to this article:

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