
Cite this article as: | Baohua Liu, Shuai Liu, Zaigang Luo, and Ruiwen Shu, Construction of iron manganese metal–organic framework-derived manganese ferrite/carbon-modified graphene composites toward broadband and efficient electromagnetic dissipation, Int. J. Miner. Metall. Mater., 32(2025), No. 3, pp.546-555. https://dx.doi.org/10.1007/s12613-024-2999-0 |
The preparation of carbon-based electromagnetic wave (EMW) absorbers possessing thin matching thickness, wide absorption bandwidth, strong absorption intensity, and low filling ratio remains a huge challenge. Metal–organic frameworks (MOFs) are ideal self-sacrificing templates for the construction of carbon-based EMW absorbers. In this work, bimetallic FeMn–MOF-derived MnFe2O4/C/graphene composites were fabricated via a two-step route of solvothermal reaction and the following pyrolysis treatment. The results reveal the evolution of the microscopic morphology of carbon skeletons from loofah-like to octahedral and then to polyhedron and pomegranate after the adjustment of the Fe3+ to Mn2+ molar ratio. Furthermore, at the Fe3+ to Mn2+ molar ratio of 2:1, the obtained MnFe2O4/C/graphene composite exhibited the highest EMW absorption capacity. Specifically, a minimum reflection loss of −72.7 dB and a maximum effective absorption bandwidth of 5.1 GHz were achieved at a low filling ratio of 10wt%. In addition, the possible EMW absorption mechanism of MnFe2O4/C/graphene composites was proposed. Therefore, the results of this work will contribute to the construction of broadband and efficient carbon-based EMW absorbers derived from MOFs.
The rapid development of fifth-generation communication technology and the wide application of electronic equipment add convenience to people’s daily lives. However, the potential harm of high-energy electromagnetic radiation to human health and equipment stability is also increasing [1–3]. To solve the problem of electromagnetic radiation pollution and mitigate the harm to human health, scholars are focusing on novel electromagnetic wave (EMW) absorption materials with wide absorption bandwidth, strong absorption intensity, low filling ratio, and thin matching thickness in the field of functional materials [4–5].
Metal–organic frameworks (MOFs) comprise typical porous crystal materials constructed via coordination self-assembly, with organic ligands as linkers and inorganic metal ions or clusters as nodes [6]. In addition, MOFs possess broad application prospects as EMW absorbers owing to their large specific surface area, high porosity, and controllable morphology [7–8]. MOFs, an ideal self-sacrificing templates, have been widely used in the preparation of carbon-based EMW absorption materials [9–12].
Iron-based MOFs (Fe-based MOFs) have attracted considerable attention in the field of EMW absorption due to their advantages, such as low cost, simple fabrication process, and tunable micromorphology [13–19]. Wu et al. [17] initially synthesized the rod-like Fe-MIL-88A precursor via a hydrothermal method and then pyrolyzed it to generate magnetic porous carbon nanorods. At the matching thickness of 3.07 mm and filling ratio of 40wt%, a minimum reflection loss (RLmin) of −52.9 dB and an effective absorption bandwidth (EAB) of 4.64 GHz were achieved. Peng et al. [18] fabricated a flower-like Fe3C/C composite (FC-650) through the pyrolysis of the precursor of MIL-101(Fe) at 650°C. The obtained FC-650 exhibited a RLmin of −39.43 dB and a maximum EAB of 5.36 GHz at a moderate filling ratio of 30wt% and a thickness of 2 mm. Li et al. [19] prepared Fe/Fe3C@NC composites by pyrolyzing the precursors of hexagonal biconical Fe–MOFs. At the filling ratio of 70wt%, the attained Fe/Fe3C@NC composites exhibited a maximum EAB of 5.15 GHz and a RLmin of −70.8 dB at a thickness of 2.5 mm. Nevertheless, most of the reported Fe-based MOF-derived EMW absorbers display disadvantages, such as a large filling ratio and a thick thickness. Therefore, under a low loading ratio and a thin matching thickness, the preparation of carbon-based EMW absorbers with a strong absorption intensity and a wide absorption bandwidth using Fe-based MOFs remains a challenging task. The introduction of a second metal node [20–25] that complexes with reduced graphene oxide (RGO) [26–30] and MXene [31–34] can considerably improve the wave dissipation capability of Fe-based MOF-derived composites.
In this work, iron manganese bimetallic MOFs/RGO (FeMn–MOFs/RGO) precursors were initially synthesized via a simple solvothermal method with graphene oxide (GO) as the template. Then, MnFe2O4/C/graphene composites were prepared via the pyrolysis of FeMn–MOFs/RGO precursors. Various characterization techniques were performed to study in detail the crystal structure, degree of graphitization, surface chemical composition, microscopic morphology, magnetic properties, and electromagnetic parameters of the obtained composites. The results demonstrate that the microscopic morphology, electromagnetic parameters, and EMW absorption performance of MnFe2O4/C/graphene composites can be regulated through the adjustment of the molar ratio of Fe3+ to Mn2+. At the Fe3+ to Mn2+ molar ratio of 2:1, the resulting MnFe2O4/C/graphene composite exhibited the best EMW absorption performance with a strong absorption and a wide bandwidth at a low filling ratio. In addition, the probable EMW absorption mechanisms of the ternary composites were elucidated. This paper provides a new idea for the use of MOFs in the preparation of magnetic carbon composites as broadband and high-efficiency EMW absorbers.
FeMn–MOF-derived MnFe2O4/C/graphene composites were prepared via a two-step route of solvothermal reaction and pyrolysis treatment. First, 80 mg multilayer GO was dispersed in 80 mL N,N-dimethylformamide (DMF) through ultrasonication to prepare a 1-mg/mL GO/DMF dispersion. Then, metal salts of FeCl3·6H2O and MnCl2·4H2O of various Fe3+ to Mn2+ molar ratios (total molar number of Fe3+ and Mn2+ equal to 7.36 mmol) and the organic ligand of terephthalic acid (H2BDC, 7.36 mmol) were successively dissolved in the prepared dispersion under vigorous magnetic stirring for 1 h. Next, the mixed dispersion was heated to 110°C and reacted in a Teflon-lined autoclave for 24 h. The resulting product was washed several times with DMF and C2H5OH and dried in a vacuum oven at 55°C for 24 h. Lastly, pyrolysis of the synthesized FeMn–MOFs/RGO precursors was conducted at 750°C in Ar atmosphere for 3 h to transform them into MnFe2O4/C/graphene composites. The schematic of the construction process of MnFe2O4/C/graphene composites is shown in Fig. 1. For convenience, the obtained MnFe2O4/C/graphene composites with various molar ratios of Fe3+ to Mn2+ were labeled as S1 (4:1), S2 (2:1), and S3 (1:1).
The Supplementary Information includes the raw materials, detailed characterization, and radar cross-section (RCS) simulation of MnFe2O4/C/graphene composites.
The crystal structure of MnFe2O4/C/graphene composites was examined via X-ray diffraction (XRD). As displayed in Fig. 2(a), the diffraction peaks at 30.0°, 35.2°, 42.7°, 53.3°, 56.6°, 62.3°, and 73.7° of S1–S3 can be assigned to the (220), (311), (400), (422), (511), (440), and (622) crystal planes of cubic spinel MnFe2O4 (JCPDS No. 10-0319), respectively [35–36]. However, no carbon-related peaks were observed. This phenomenon may be due to the weaker crystallinity of carbon than MnFe2O4 [37]. Following Scheller’s equation, the average grain size (L) of the samples was calculated using the following formula [36]:
L=Kλβcosθ | (1) |
where K equals 0.89, β denotes the half-width of the characteristic diffraction peak, and λ indicates the wavelength of X-ray (0.154 nm). The calculated average grain sizes of MnFe2O4 particles in S1, S2, and S3 for the characteristic peak at 35.2° were 33.6, 29.6, and 19.7 nm, respectively. Therefore, the grain size gradually decreased with the decrease in the molar ratio of Fe3+ to Mn2+.
Fig. 2(b) shows the Raman spectra of S1–S3. Notably, two scattering peaks at 1597 and 1350 cm−1 were ascribed to the G and D band, respectively [38–39]. The D band shows an association with sp3 hybridized carbon atoms from disordered or defective carbon, and the G band relates to the sp2 hybridized carbon atoms from graphite [38–39]. The intensity ratio of D band to G band (ID/IG) is often used in the evaluation of the degree of disorder [38–39]. The calculated values of ID/IG for S1, S2, and S3 were 0.93, 0.89, and 0.95, respectively. Therefore, the S2 possessed the lowest ID/IG of 0.89 with fewer internal defects.
X-ray photoelectron spectroscopy (XPS) was used to determine the surface chemical composition and valence states of S2. Fig. 2(c) displays the wide scan spectrum, which indicates the existence of Mn, Fe, C, and O. From the C 1s spectrum in Fig. 2(d), three notable peaks were detected at 284.5, 285.2, and 288.1 eV, and they can be attributed to C–C, C–O, and C=O, respectively [36]. Fig. 2(e) shows the O 1s spectrum. The binding energies at 530, 532, and 533.6 eV can be ascribed to metal–O, C=O, and C–O, respectively [36]. Fig. 2(f) shows that the Fe 2p spectrum can be fitted into three main parts: the peaks of Fe2+ (711.2 and 723.3 eV) and Fe3+ (713.5 and 724.8 eV) were attributed to Fe 2p3/2 and Fe 2p1/2, respectively, which indicates the oxidization of the surface of Fe; in addition, the binding energies at 719.2 and 733.2 eV may be assigned to the satellite peaks [40]. Fig. 2(g) depicts the Mn 2p spectrum. Specifically, the peak that appeared at 640.8 eV was assigned to Mn 2p3/2, that at 653.5 eV can be ascribed to Mn 2p1/2, and that at 646.9 eV represented a satellite peak [36,41].
Scanning electron microscopy (SEM) was performed to observe the microscopic morphology of MnFe2O4/C/graphene composites. The carbon skeletons of S1 exhibited a loofah-like shape (Fig. 3(a)–(c)). When the molar ratio of Fe3+ to Mn2+ was reduced to 2:1, a number of octahedral carbon skeletons were almost uniformly loaded on the graphene surface (Fig. 3(d)–(f)). Nevertheless, as the molar ratio of Fe3+ to Mn2+ was further reduced to 1:1, the carbon skeletons in the S3 displayed polyhedral and pomegranate-like shapes (Fig. 3(g)–(i)). As a consequence, the microscopic morphology of carbon skeletons of MnFe2O4/C/graphene composites can be elaborately modulated by changing the molar ratio of Fe3+ to Mn2+.
Transmission electron microscopy (TEM) was performed to further examine the microstructure of S2. Fig. 3(j)–(k) shows the uniform distribution of some octahedral MnFe2O4/C skeletons on the surface of graphene. Fig. 3(l) depicts the high-resolution TEM (HRTEM) image of S2. The interplanar spacings of 0.34 and 0.30 nm should be attributed to the (002) crystal plane of graphitic carbon and (220) crystal plane of MnFe2O4, respectively [36,42]. The elemental distribution of S2 was determined via energy dispersive spectrometry (EDS) (Fig. 3(m)–(q)). Fig. 3(n) shows the uniform distribution of C throughout the test area. Nevertheless, Mn, Fe, and O were primarily distributed on the carbon skeletons (Fig. 3(o)–(q)).
Fig. 4 displays the magnetization versus magnetic field (M–H) curves of S1–S3 at room temperature. The inset in Fig. 4 shows that the magnified magnetization curves clearly revealed the typical ferromagnetic behavior of all the samples, which can generate a notable magnetic loss in the gigahertz-frequency region [43–45]. The saturation magnetization (Ms) values of S1, S2, and S3 were 49.5, 45.6, and 41.6 emu·g−1, respectively. Meanwhile, S1, S2, and S3 showed coercive force (Hc) values of 110.9, 79.7, and 105.8 Oe, respectively. In general, the magnetic properties of spinel ferrite show a relation to the crystallinity, particle size, and magnetocrystalline anisotropy [43]. In the present study, the static magnetic properties of MnFe2O4/C/graphene composites were mainly influenced by grain size and crystallinity. The notable saturation magnetization and coercive force can promote magnetic loss under alternating electromagnetic fields.
To assess the EMW absorption capacity of MnFe2O4/C/graphene composites, we calculated the reflection loss (RL) and EAB. Fig. 5 shows the three-dimensional (3D) plots of RL and corresponding 2D contour maps of S1–S3 at a low filling ratio of 10wt%. The RLmin values of S1, S2, and S3 reached −16.7 (5.00 mm), −72.7 (2.17 mm), and −12.1 dB (5.00 mm), respectively. Meanwhile, the EAB values of S1, S2, and S3 were 1.76 GHz (3.00 mm), 5.10 GHz (1.95 mm), and 2.40 GHz (2.11 mm), respectively. Therefore, the S2 exhibited the best EMW absorption capacity among the samples.
Electromagnetic parameters were used to determine the EMW absorption capacity of materials [44–45]. The real parts of the complex permittivity (ε') and permeability (μ') represent the storage capacity of electric and magnetic field energies, respectively; the imaginary part of the complex permittivity (ε'') denotes the dissipation capacity of electric energy, and the imaginary part of the complex permeability (μ'') indicates the magnetic field energy [44–45]. Therefore, the frequency dependence of electromagnetic parameters of S1–S3 was investigated. The ε' and ε'' of S1–S3 decreased with the increase in frequency (f) (Fig. 6(a) and (b)). This result can be explained by the frequency dispersion effect, which favored the attenuation of the incident waves [46]. In addition, the S2 exhibited notably larger ε' and ε'' than S1 and S3 in almost the entire frequency range. As presented in Fig. 6(c), all samples had μ' values close to 1, and no evident difference was observed among them. Fig. 6(d) shows the μ'' vs. f curves of S1–S3. The μ'' of all samples decreased with the increase in frequency and fluctuated. The dielectric (tanδe) and magnetic loss tangents (tanδm) are often used to evaluate the dielectric loss and magnetic loss capacity, respectively. Fig. 6(e) and (f) shows that tanδe is considerably larger than the tanδm of all samples, which indicates that dielectric loss was the main source of EMW dissipation. The tanδe values of S2 were notably larger than those of S3 and S1 over the entire frequency range, which suggests that S2 had the strongest dielectric loss capacity. In addition, the μ'' and tanδm exhibited similar trends with two evident peaks located in the range of <5 GHz for S1–S3 and 12–14 GHz for S2 and S3; this finding suggests the presence of natural and exchange resonances [44–45].
For further investigation of the dielectric loss mechanism, the Cole–Cole curves were plotted according to the following formula [47–48]:
(ε′−εs+ε∞2)2+(ε″ | (2) |
where εs denotes the static dielectric constant, and ε∞ represents the relative dielectric constant at a high-frequency limit. Based on the above formula, each semicircle denotes a Debye relaxation process [47–48]. As shown in Fig. 6(g), the Cole–Cole curves of all samples comprised a semicircle and a long smooth tail. This result indicates the presence of conduction loss and polarization relaxation in the MnFe2O4/C/graphene composites [47–48].
The eddy current loss criterion C0 = μ″(μ′)−2f −1 can be used to determine the dominance of the eddy current loss during magnetic loss [49–50]. Variations of C0 with the frequency displayed in Fig. 6(h) indicate that the magnetic loss was dominated by natural and/or exchange resonance [49–50].
The design of EMW absorbing materials with excellent performance should consider attenuation loss and impedance matching. Attenuation loss is often assessed using the attenuation constant (α), which can be expressed by the following equation [51–52]:
\begin{aligned}[b] & \alpha = \frac{{\sqrt 2 \text{π} f}}{c} \times \\ & \quad \sqrt {(\mu ''\varepsilon '' - \mu '\varepsilon ') + \sqrt {{{(\mu ''\varepsilon '' - \mu '\varepsilon ')}^2} + {{(\varepsilon '\mu '' + \varepsilon ''\mu ')}^2}} } \end{aligned} | (3) |
Fig. 6(i) shows the overall increasing trend of α with the increase in the frequency for all samples. Notably, the α values of S2 were notably larger than those of S3 and S1, which indicates that S2 had the strongest EMW attenuation capability.
In general, the impedance matching characteristic can be evaluated using the normalized impedance of Z' and Z'' [53–54]. Fig. 7 shows the Z' (Fig. 7(a)) and Z'' (Fig. 7(b)) for S1–S3 at a thickness of 2.17 mm. The optimal impedance matching for the S2 shows that Z' and Z'' are closer to 1 and 0, respectively, compared with the other samples. Consequently, effective synergistic attenuation and impedance matching can be achieved for S2.
The possible EMW absorption mechanisms of MnFe2O4/C/graphene composites are schematically described in Fig. 8. Initially, conductive graphene worked synergistically with the ferromagnetic MnFe2O4 for the effective adjustment of the dielectric constant and optimization of impedance matching [27]. Second, some structural defects were observed on the graphene surface. These surface defects caused an imbalance in the dipole moment, which resulted in dipole polarization relaxation and the dissipation of electromagnetic energy [27]. Third, numerous heterogeneous interfaces formed among MnFe2O4, C, and graphene in the ternary composites. The space charges accumulated in these heterogeneous interfaces resulted in the formation of a capacitance-like structure; as a consequence, the interfacial polarization and the attenuation capability of incident EMWs improved under alternating electromagnetic fields [55–56]. Fourth, according to Cao’s electron hopping model, electrons can absorb electromagnetic energy to transfer to the surface of carbon frameworks and graphene, which results in conduction loss [57]. Lastly, the ferromagnetic MnFe2O4 in the ternary composites caused a notable magnetic loss in the form of natural and exchange resonances under alternating electromagnetic fields [58].
To explore the EMW dissipation capacity of prepared MnFe2O4/C/graphene composites in practical application scenarios, we carried out RCS simulation using computer simulation technology (CST) [59–60]. Fig. 9(a) illustrates the CST simulation model diagram. The RCS fluctuation was plotted (Fig. 9(b)), with the θ values ranging from −90° to 90°. Significantly, the model coated by S2 displayed the smallest scattered signal value, which indicates its excellent EMW dissipation capability. As the model was coated with S2 at a thickness of 2.17 mm, the RCS value can be reduced by 34.1 dB·m2, which suggests a notable dissipation effect on radar waves [59–60]. Fig. 9(c)–(f) shows the 3D simulation scenarios and the models of all samples. Fig. 9(g)−(j) describes the RCS simulation diagrams of the pure perfect electrical conductor (PEC) model and the models covered with S1, S2, and S3. The RCS values of PEC, S1, S2, and S3 were −24.0, −37.1, −51.9, and −39.2 dB·m2, respectively. Notably, the excellent RCS attenuation capacity endowed S2 with tremendous practical application prospects.
Bimetallic FeMn–MOF-derived MnFe2O4/C/graphene composites were prepared via a facile two-step method of solvothermal reaction and pyrolysis treatment. The results indicate that the microscopic morphology of carbon skeletons in the prepared MnFe2O4/C/graphene composites can be modulated through the adjustment of the molar ratio of Fe3+ to Mn2+. The obtained MnFe2O4/C/graphene composite with the molar ratio of Fe3+ to Mn2+ of 2:1 demonstrated a comprehensive and excellent EMW absorption performance. Specifically, at a 10wt% filling ratio, an optimal RLmin of −72.7 dB at a thickness of 2.17 mm and a maximum EAB of 5.10 GHz at a thin thickness of 1.95 mm were achieved. Furthermore, CST simulation was performed to explore the EMW dissipation capacity of the ternary composites in practical application scenarios. In addition, the underlying EMW absorption mechanisms were clarified. The excellent EMW absorption performance was mainly attributed to the improved impedance matching, enhanced dipole and interfacial polarization, notable conduction loss, and natural and exchange resonances. The prepared MnFe2O4/C/graphene composites derived from FeMn–MOFs can be used as broadband and efficient EMW absorbers.
This work is financially supported by the Natural Science Research Project of the Anhui Educational Committee, China (No. 2022AH050827), the Open Research Fund Program of Anhui Province Key Laboratory of Specialty Polymers, Anhui University of Science and Technology, China (No. AHKLSP23-12), and the Joint National-Local Engineering Research Center for Safe and Precise Coal Mining Fund, China (No. EC2022020)
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.
The online version contains supplementary material available at https://doi.org/10.1007/s12613-024-2999-0.
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