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Fig.
1.
Flowchart representing the preparation of FNC/RGO/MDCF.
| Cite this article as: |
Konghu Tian, Hang Yang, Chao Zhang, Ruiwen Shu, Qun Shao, Xiaowei Liu, and Kaipeng Gao, Fabrication of flake-like NiCo2O4/reduced graphene oxide/melamine-derived carbon foam as an excellent microwave absorber, Int. J. Miner. Metall. Mater., 32(2025), No. 3, pp.556-565. https://dx.doi.org/10.1007/s12613-024-3008-3
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Carbon-based foams with a three-dimensional structure can serve as a lightweight template for the rational design and controllable preparation of metal oxide/carbon-based composite microwave absorption materials. In this study, a flake-like nickel cobaltate/reduced graphene oxide/melamine-derived carbon foam (FNC/RGO/MDCF) was successfully fabricated through a combination of solvothermal treatment and high-temperature pyrolysis. Results indicated that RGO was evenly distributed in the MDCF skeleton, providing effective support for the load growth of FNC on its surface. Sample S3, the FNC/RGO/MDCF composite prepared by solvothermal method for 16 h, exhibited a minimum reflection loss (RLmin) of −66.44 dB at a thickness of 2.29 mm. When the thickness was reduced to 1.50 mm, the optimal effective absorption bandwidth was 3.84 GHz. Analysis of the absorption mechanism of FNC/RGO/MDCF revealed that its excellent absorption performance was primarily attributed to the combined effects of conduction loss, multiple reflection, scattering, interface polarization, and dipole polarization.
Lightweight, high-performance microwave absorption materials (MAMs) can effectively mitigate the harmful effects of electromagnetic radiation pollution on precision electronic equipment and human health [1–12]. Scientific material selection and special structural design enable the synergistic interaction between components to improve the comprehensive wave absorption performance of MAMs.
Nickel cobaltate (NiCo2O4), with its spinel structure, offers the advantages of controllable morphology and good chemical stability [13–14]. Fan et al. [15] used carbon microspheres as templates to grow acicular NiCo2O4 and granular zinc oxide (ZnO) on their surfaces, creating urchin-like C/NiCo2O4/ZnO composites. The composite achieved a minimal reflection loss (RLmin) of −43.61 dB at a thickness of 2.40 mm. Ding and Wang [16] fabricated reduced graphene oxide (RGO)–NiCo2O4 nanochain composites using two-step pyrolysis, achieving a RLmin of −42.10 dB at a thickness of 1.60 mm. Han et al. [17] synthesized the C/NiCo2O4 composite through electrospinning and in-situ thermal treatment, reaching a RLmin of −52.70 dB at a thickness of 1.90 mm. Thus, while NiCo2O4 is a magnetic metal oxide with controllable morphology, solely using it in high-performance MAMs is difficult due to its single loss mechanism and low wave absorption properties.
Melamine foam (MF) offers advantages such as low cost, a three-dimensional (3D) porous network structure, and low density, making it an excellent lightweight carbon foam template for preparing high-performance MAMs [18–19]. Li et al. [20] used static electricity to wrap graphene oxide (GO) onto MF and subsequently prepared a Co3O4/RGO/melamine-derived carbon foam (MDCF) composite with a 3D layered structure through annealing and hydrothermal methods. The RLmin reached −31.88 dB at a thickness of 2.00 mm, with a lightweight density of 10.60 mg/cm3. Cheng et al. [21] synthesized the RGO/MXene/Ni–MF composites through electrostatic assembly and hydrazine vapor reduction, achieving a RLmin of −61.30 dB at a thickness of 2.10 mm. Additionally, Ma et al. [22] fabricated the RGO/multiwalled carbon nanotube (MWCNT)-modified melamine sponge composite using a dip-coating and hydrazine reduction process. They found that at a thickness of 4.60 mm, the RLmin was −50.43 dB, and the effective absorption bandwidth (EAB) was 10.80 GHz, demonstrating favorable infrared stealth and thermal insulation characteristics.
Moreover, porous carbon materials constructed from RGO offer the advantages of high conductivity, low density, and high specific surface area, and their continuous 3D porous structure aids in the controllable preparation of high-performance MAMs [23–24]. However, the electromagnetic loss of a single RGO material is limited. Therefore, conducting multicomponent composite and component regulation with metal oxides, constructing metal oxides/carbon-based foam multicomponent composite with a 3D structure, and optimizing electromagnetic parameters and impedance matching are necessary, thus enhancing microwave absorption capacities [25–28].
In this study, MDCF and RGO were used as the basic 3D framework for the carbon foam, with flake-like nickel cobaltate (FNC) serving as the magnetic filler component. The FNC/RGO/MDCF composite MAMs, featuring a 3D structure with a dielectric network and electromagnetic coordination, were successfully prepared using solvothermal and high-temperature pyrolysis methods. In addition, this study offers a feasible approach for the microstructural design and multifunctional expansion of 3D lightweight, high-efficiency MAMs.
Cobalt nitrate hexahydrate (Co(NO3)2·6H2O, 99%), urea, and nickel nitrate hexahydrate (Ni(NO3)2·6H2O, 99%) were supplied by Aladdin Reagent (Shanghai) Co. Graphene oxide solution (5 mg/mL) was provided by Suzhou Tanfeng Graphene Technology Co. All chemical reagents were analytically pure and used as received. Deionized water was prepared in the laboratory.
Fig. 1 presents the synthesis process of FNC/RGO/MDCF. First, MF with dimensions of 6.0 cm × 3.0 cm × 3.5 cm was immersed in a 2.5 mg/mL GO solution for 24 h and then dried at 60°C for 12 h to obtain GO/MF. Second, RGO/MDCF was obtained by placing GO/MF into a tube furnace and maintaining it at 700°C for 60 min under a N2 atmosphere. Third, a solution containing 3 mM Ni(NO3)2·6H2O, 40 mM urea, and 6 mM Co(NO3)2·6H2O was prepared by dissolving these compounds in 60 mL of a mixed solvent (ethanol : water = 1:1, vol%). The precursor for FNC/RGO/MDCF was then obtained by immersing RGO/MDCF in this mixed solution for 24 h, and then transferring it to a 100 mL hydrothermal reactor. After solvothermal treatment at 140°C for 16 h, the precursor was washed four times with water and ethanol. Finally, the washed precursor was placed in the tube furnace and maintained at 400°C for 2 h under a N2 atmosphere to obtain FNC/RGO/MDCF. In addition, samples subjected to solvothermal treatment times of 8, 12, and 16 h were designated as S1, S2, and S3, respectively.
The microstructure of the FNC/RGO/MDCF composites was examined with scanning electron microscopy (SEM, FlexSEM1000), while their crystal phase structures were analyzed through X-ray diffraction (XRD, SmartLab SE, Cu-Kα radiation (λ = 0.154 nm)). In addition, X-ray photoelectron spectroscopy (XPS, ESCALAB Xi+) was performed to assess the elements and chemical states of the FNC/RGO/MDCF composites. Subsequently, the sample was mixed with paraffin wax at a 30wt% ratio and pressed into a ring with outer and inner diameters of 7.00 and 3.04 mm, respectively. The electromagnetic parameters of FNC/RGO/MDCF composites were then determined using a vector network analyzer (Keysight E5080B) based on the coaxial method.
The microstructure of FNC/RGO/MDCF was analyzed using SEM (Fig. 2). Fig. 2(a) shows the RGO/MDCF with a 3D network skeleton structure. The introduction of RGO into MDCF effectively prevented foam collapse, which not only supported the stability of the dielectric network structure but also provided additional attachment sites for the load growth of NiCo2O4 sheets. At solvothermal times of 8 h (S1) and 12 h (S2), only small-sized FNCs were observed, as shown in Fig. 2(b) and (c). After increasing the solvothermal time to 16 h (S3), FNCs with a relatively regular morphology were observed in FNC/RGO/MDCF, as shown in Fig. 2(d), with a flake size of approximately 3–5 μm. As presented in Fig. 2(b)–(d), the optimal solvothermal time was 16 h. At this duration, FNC was uniformly embedded in the RGO/MDCF, resulting in an FNC/RGO/MDCF with a 3D continuous porous structure. In addition, a rich, heterogeneous interface formed between the different components, which prolonged the electromagnetic wave transmission path and effectively enhanced electromagnetic wave dissipation.
Fig. 3(a) displays the XRD patterns of FNC/RGO/MDCF. The diffraction peak at 26.0° mainly originates from the carbon components in MDCF and RGO. The diffraction peaks found at 18.9°, 31.1°, 36.7°, 44.6°, 38.4°, 55.4°, 59.1°, and 65.0° for samples S1, S2, and S3 correspond to the (111), (220), (311), (222), (400), (422), (511), and (440) crystal faces of NiCo2O4, respectively (JCPDS No. 20-0781). Furthermore, no additional diffraction peaks were observed, indicating the high purity of NiCo2O4 in the fabricated FNC/RGO/MDCF. With the increasing solvothermal time, the diffraction peak intensities for samples S1–S3 increased. This increase is likely due to the gradual formation of a more regular sheet structure of FNC morphology, as observed by SEM. These results may be conducive to improving the effective attenuation capability of FNC/RGO/MDCF for incident electromagnetic waves. The hysteresis loops obtained using a vibrating sample magnetometer for samples S1–S3 are displayed in Fig. 3(b). Saturation magnetization and coercivity are important parameters to measure the magnetic loss. The saturation magnetization values of S1, S2, and S3 are 0.012, 0.014, and 0.020 A·m2·kg−1, respectively. As the solvothermal time increases, the saturation magnetization of samples also gradually increases. This enhancement in saturation may contribute to improved microwave absorption performance [29].
XPS was used to analyze the types and chemical valence states of the elements in FNC/RGO/MDCF (Fig. 4). As shown in Fig. 4(a), the total energy spectrum revealed the presence of five elements, including C, N, O, Co, and Ni. Fig. 4(b)–(f) presents the high-resolution energy spectra for C, N, O, Co, and Ni. Fig. 4(b) displays the high-resolution energy spectrum for C 1s, with three representative peaks at binding energies of 284.5, 286.2, and 288.6 eV, corresponding to C–C, C–O, and O–C=O, respectively; carbon is predominantly present as C–C [30]. Fig. 4(c) presents the high-resolution energy spectrum for N 1s, with representative peaks at binding energies of 397.8, 398.9, and 399.8 eV, attributed to pyridine N, pyrrole N, and graphite N, respectively, and the N element was derived from MDCF. Fig. 4(d) exhibits the high-resolution energy spectrum for O 1s, with binding energies of 529.2, 531.2, and 533.0 eV, attributed to Ni–O/Co–O, C–O, and C=O, respectively [29]. Fig. 4(e) shows the four main peaks for the Co 2p orbit, with binding energies of 779.5 eV (Co3+) and 781.1 eV (Co2+) at the Co 2p3/2 peak and 794.5 eV (Co3+) and 796.1 eV (Co2+) at the Co 2p1/2 peak. Additionally, two satellite (sat.) vibration peaks were detected at 787.9 and 803.6 eV. Fig. 4(f) displays the four main peaks fitted for the Ni 2p orbit, with binding energies of 853.8 eV (Ni2+) and 855.5 eV (Ni3+) at the Ni 2p3/2 peak and 872.3 eV (Ni2+) and 875.6 eV (Ni3+) at the Ni 2p1/2 peak. Two sat. vibration peaks were observed at 861.1 and 880.1 eV. The XPS analysis results indicate that FNC exhibits a spinel-type structure [31], which is consistent with the XRD analysis results.
Consistent with transmission line theory, the microwave absorption performance of FNC/RGO/MDCF was studied and calculated using Eqs. (1) and (2) [32–33]:
| RL=20lg|Zin−Z0Zin+Z0| | (1) |
| Zin=Z0(√μrεr)tanh[j(2πdfc)√μrεr] | (2) |
where Zin indicates the input impedance of FNC/RGO/MDCF, Z0 represents impedance in free space, f indicates frequency, d indicates the thickness of FNC/RGO/MDCF, and c refers to light speed in a vacuum. εr and μr represent complex permittivity (εr = ε′ − jε″) and complex permeability (μr = μ′ − jμ″).
Fig. 5 presents the RL curve and 3D mappings of FNC/RGO/MDCF (fill ratio, 30wt%). In Fig. 5(a) and (b), the RLmin was −51.85 dB (located at 15.20 GHz) for S1 with a thickness of 5.46 mm. Meanwhile, the EAB was 1.76 GHz for S1 with a thickness of 5.00 mm, indicating that the microwave absorption performance of S1 was concentrated in the high-frequency band (12–18 GHz) region. In Fig. 5(c) and (d), the RLmin reached −54.57 dB (located at 3.76 GHz) for S2 with a thickness of 5.80 mm, while the EAB was 3.12 GHz at a thickness of 4.30 mm, indicating that the microwave absorption performance of S2 was concentrated in the low-frequency band (2–8 GHz) region. As shown in Fig. 5(e) and (f), the RLmin reached −66.44 dB (at 9.84 GHz) for S3 with a thickness of 2.29 mm, and the EAB was 3.84 GHz at a thickness of 1.50 mm, covering the entire X-band and Ku-band. This finding demonstrates that S3 exhibited the best microwave absorption performance. Compared to S1 and S2, the RLmin and EAB of S3 were notably improved. Therefore, the microwave absorption frequency band, RLmin, and the EAB of FNC/RGO/MDCF can be adjusted by changing the solvothermal time and material thickness. This approach offers a promising strategy for the development of high-performance MAMs using FNC and MDCF.
Fig. 6 indicates the electromagnetic parameters of FNC/RGO/MDCF. Real parts, ε′ and μ′, represent the capability of FNC/RGO/MDCF to store electromagnetic energy, whereas the imaginary part, ε″ and μ″, reflect its capability to dissipate electromagnetic energy. The tangent values of magnetic loss (tanδμ = μ″/μ′) and dielectric loss (tanδε = ε″/ε′) indicate the magnetic and dielectric loss capacities of FNC/RGO/MDCF, respectively. Based on Fig. 6(a) and (b), ε′ and ε″ for samples S1, S2, and S3 decrease with increasing frequency, while RGO has a large number of bound charges at its residue and defect sites, revealing the difficulty of nitrogen (N) atoms in MDCF to reorient with the increasing frequency of the applied electromagnetic field, which leads to the reduction in ε′ and ε″ values of these samples at high frequencies, that is, the electric dispersion phenomenon [29]. Oxygen vacancies and lattice defects on the surface of MDCF and RGO act as polarization centers, forming dipolar and defect polarizations, respectively [34]. As shown in Fig. 6(c), tanδε follows the trend of S3 > S2 > S1. This trend is attributed to the slower response of dipoles to the external electric field due to changes in tanδε. Therefore, the polarization time of RGO and MDCF in the alternating electric field lags behind the frequency of the electric field, causing ε′, ε″, and tanδε of FNC/RGO/MDCF to increase with rising solvothermal time. Consequently, S3 exhibits superior dielectric loss capacity compared to S1 and S2, indicating that S3 might have the best microwave absorption performance. In Fig. 6(d) and (e), μ′ and μ″ show similar fluctuation trends, with μ′ values ranging from 0.95 to 1.06 and μ″ values ranging from −0.01 to 0.10 across the frequency of 2–18 GHz. The observed fluctuations in these parameters could be due to the natural ferromagnetic resonance and exchange resonance in samples S1–S3 [15]. The obtained result showed that prolonging solvothermal time exerted a limited effect on the magnetic loss of FNC/RGO/MDCF. Comparing Fig. 6(c) and (f), the tanδε values for all samples (S1–S3) are higher than the tanδμ values, demonstrating that dielectric loss is the dominant factor in the microwave attenuation of FNC/RGO/MDCF. Overall, S3 exhibits the best microwave absorption performance.
Debye relaxation is a crucial mechanism influencing the dielectric loss of FNC/RGO/MDCF. The Debye relaxation process of FNC/RGO/MDCF was analyzed using Cole–Cole curve analysis. Each semicircle in this curve represents a complete Debye relaxation process in FNC/RGO/MDCF. Fig. 7 presents the Cole–Cole curve for FNC/RGO/MDCF, displaying the presence of multiple Cole–Cole semicircles for samples S1–S3. Multiple Cole–Cole semicircles in sample S1 were located at 7.2–8.5 GHz, those in sample S2 were located at 9.5–11.5 GHz, and those of sample S3 were located at 10.3–13.5 GHz. Irregular semicircles were also observed in S1–S3, indicating that, in addition to Debye relaxation, other loss mechanisms, including interfacial polarization and conduction loss, also exist [35]. Furthermore, the Cole–Cole curves exhibit a long straight tail line at high-frequency bands, indicating that conduction loss plays a crucial role in the dielectric loss of FNC/RGO/MDCF [36].
Attenuation constant (α) and impedance matching (Z) should be also considered in the construction of FNC/RGO/MDCF with excellent absorption performance.
α was calculated in accordance with Eq. (3) [37–38]:
| α=√2cπf√(μ″ε″−μ′ε′)+√(μ″ε″−μ′ε′)2+(ε′μ″+ε″μ′)2 | (3) |
Z was calculated by Eq. (4) [39]:
| Z=|ZinZ0|=|√μrεrtanh[j(2πfdc)√μrεr]| | (4) |
Fig. 8(a) shows the relationship between α and frequency for samples S1–S3. The α increases synchronously with frequency across all samples, with S3 exhibiting the highest α value. This finding indicates that S3 exhibited the strongest capability to attenuate incident electromagnetic waves inside FNC/RGO/MDCF. In the design application of MAMs, in addition to focusing on α, ensuring that the Z value of FNC/RGO/MDCF is as close to 1.0 as possible is also necessary. The Z value of 1.0 indicates complete electromagnetic wave absorption, with the optimal range generally regarded as 0.8–1.2. Fig. 8(b)–(d) presents the relationship between impedance matching of samples S1–S3 and frequency. The Z values for samples S1 and S2 deviate from the optimal range, indicating less ideal impedance matching. In contrast, the Z values for S3 at different thicknesses are mostly in the optimal range. Considering α and Z value analyses, S3 demonstrates superior microwave absorption performance, which aligns with the conclusions drawn from the electromagnetic parameter analysis.
Table 1 lists the optimal RL and effective bandwidth of various NiCo2O4-based composites to analyze the wave absorption performance of FNC/RGO/MDCF. The FNC/RGO/MDCF prepared in this study exhibited excellent microwave absorption capabilities.
| Composites | Thickness / mm | RLmin / dB | EAB / GHz | Reference |
| NiCo2O4/CF | 2.01 | −59.75 | 4.60 (2.57 mm) | [14] |
| C/NiCo2O4/ZnO | 2.40 | −43.61 | 4.32 (2.40 mm) | [15] |
| rGO-NiCo2O4 | 1.60 | −42.10 | 4.88 (1.80 mm) | [16] |
| C–NiCo2O4 | 1.90 | −52.70 | 5.20 (1.90 mm) | [17] |
| C@NiCo2O4@Fe3O4 | 3.40 | −43.00 | 2.10 (3.40 mm) | [40] |
| FNC/RGO/MDCF | 2.29 | −66.44 | 3.84 (1.50 mm) | This work |
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Fig. 9 illustrates the microwave absorption mechanism of FNC/RGO/MDCF. Initially, MDCF provides a 3D network skeleton. When incident electromagnetic waves enter FNC/RGO/MDCF, they undergo absorption, reflection, and transmission, resulting in effective attenuation of electromagnetic energy. Second, the incorporation of RGO in the MDCF skeleton enhances the stability of the structure and increases the load area for FNC, thereby improving dielectric loss capacity. Third, the uniform distribution of FNC on RGO/MDCF introduces numerous scattering sites but contributes to magnetic loss. Magnetic FNC produces natural resonance in low-frequency bands and a smaller eddy current loss in high-frequency bands. Additionally, N atoms and functional groups on RGO and MDCF surfaces contribute to dipole polarization and polarization relaxation loss [34,41]. The heterogeneous interface formed within FNC/RGO/MDCF acts similarly to a capacitor. As the charge accumulates, micro-currents are due to increased interface polarization and conduction loss. The absorption efficiency of FNC/RGO/MDCF for electromagnetic waves is notably improved by optimizing the combination of the three components and leveraging electromagnetic synergy. This unique structural design and the combined action of several loss mechanisms render FNC/RGO/MDCF with excellent microwave absorption performance.
In this study, using RGO/MDCF as the basic framework of carbon foam, the FNC was uniformly grown on its surface using solvothermal and high-temperature pyrolysis methods, and the FNC/RGO/MDCF composite MAM was prepared. The results indicated that by adjusting the solvothermal treatment time, the NiCo2O4 could be controlled to form a well-defined sheet structure, leading to optimized impedance matching of the FNC/RGO/MDCF composite. Particularly, at a thickness of 2.29 mm, sample S3 achieved a RL of −66.44 dB, and at a thickness of 1.50 mm, its EAB was 3.84 GHz. This exceptional wave absorption performance can be attributed to the excellent impedance matching, the optimal 3D foam structure, and the synergistic electromagnetic loss mechanism in the material. Moreover, this study provides valuable insights into the development of lightweight, high-performance 3D foam MAMs.
The authors are grateful for the support of the Key Science Research Project in Colleges and Universities of Anhui Province, China (No. 2022AH050813) and the Medical Special Cultivation Project of Anhui University of Science and Technology, China (No. YZ2023H2A002).
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.
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| Composites | Thickness / mm | RLmin / dB | EAB / GHz | Reference |
| NiCo2O4/CF | 2.01 | −59.75 | 4.60 (2.57 mm) | [14] |
| C/NiCo2O4/ZnO | 2.40 | −43.61 | 4.32 (2.40 mm) | [15] |
| rGO-NiCo2O4 | 1.60 | −42.10 | 4.88 (1.80 mm) | [16] |
| C–NiCo2O4 | 1.90 | −52.70 | 5.20 (1.90 mm) | [17] |
| C@NiCo2O4@Fe3O4 | 3.40 | −43.00 | 2.10 (3.40 mm) | [40] |
| FNC/RGO/MDCF | 2.29 | −66.44 | 3.84 (1.50 mm) | This work |
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