| Cite this article as: |
Yuanyuan Zhou, Zhongyi Bai, Xiangyang Yang, Wei Liu, Bingbing Fan, Zhikai Yan, and Xiaoqin Guo, In-situ grown NiCo bimetal anchored on porous straw-derived biochar composites with boosted microwave absorption properties, Int. J. Miner. Metall. Mater., 30(2023), No. 3, pp.515-524. https://dx.doi.org/10.1007/s12613-022-2496-2
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The rapid progress of electronic technology has gradually produced a series of problems, such as electromagnetic (EM) radiation and electromagnetic interference (EMI) [1–4]. Exploring excellent microwave absorption materials is urgently warranted to resolve these serious problems. The easiest and most effective method is to find a material with high conductivity and improve its absorbing performance by promoting strong conductive loss and dielectric loss [5–8].
Highly conductive materials mainly include metals [9–13] (Fe, Co, Ni, Cu, and Ag), carbon materials [14–18] (graphene, graphite, carbon black, carbon fiber, and carbon nanotubes), and conductive polymers [19–21] (polyacetylene, polypyrrole, and polyaniline). Among these, carbon materials have aroused significant enthusiasm due to their merits of low density, light weight, high aspect ratio and conductivity, good dielectric properties, low specific gravity, and strong chemical stability. Despite their many advantages, carbon materials still have the problems of complicated preparation and high economic cost. Therefore, the development of a novel method to fabricate carbon materials will be of scientific significance.
Biomass is an attractive renewable resource, and its utilization and development exhibit the sustainable cycle feature. It is a natural carrier of carbon elements and has a great potential to be converted into functional carbon materials. In general, biomass is abundant in nature, including forests, agriculture, aquatic vegetation, and crustaceans. Moreover, biomass waste has become one of the largest pollutants in the world, and its utilization will help protect resources and the environment. Many biomass carbon materials have been used as absorbing materials. For example, Aslam et al. [22] selected wheat straw as a carbon source and controlled its KOH content to modify the microstructure of the generated 3D foam-like biocarbon with a minimal reflection loss (RLmin) of −37 dB and an effective absorption band (EAB) of 8.8 GHz (7.2–16 GHz). Yan’s group [23] proposed a cellulose-derived carbon aerogel that was obtained through carbonization at a low temperature of about 550°C for 2 h and showed exceptional RLmin of −43.6 dB and EAB of 7.42 GHz. Zhao et al. [24] prepared porous skeleton carbon media by employing wheat flour as the biomass carbon source, and the carbon material showed an exceptional absorbing ability with an RLmin of −51 dB. Sun et al. [25] fabricated a hierarchical carbonized waxberry, and the natural radial-gradient structure endowed the biomass with strong polarization loss because of the gradient dielectric property. However, the EM wave absorption property of a single carbon component is seriously restrained by poor impedance matching. To alleviate the impedance mismatch caused by highly conductive carbon materials, Gou’s group [26] synthesized biocarbon composites by using FeCl3·6H2O as the magnetic raw material and found that the formed magnetic nanoparticles are beneficial for the improvement of magnetic loss. Studies have also been conducted on the absorbing performance of carbon-cotton/Co@nanoporous carbon [27], Ni/rice-derived porous carbon [28], biochar/(Fe,Ni) hybrid [29], bark-derived Co-doped porous carbon [30], and ferrite/biocarbon [31].
Owing to the double loss mechanism of magnetic composite materials, an enhanced microwave absorption capability can be obtained through the proper design and preparation of magnetic–dielectric composites. On the one hand, the dielectric carbon component acts as the center of electric polarization and prompts the reduction of eddy current loss caused by magnetic metals. On the other hand, the synergy effect of dielectric loss and magnetic loss favors a good impedance match. Herein, straw-derived biochar was obtained by acid washing and subsequent high-temperature annealing. The as-fabricated biocarbon composites anchored with magnetic NiCo were synthesized by the electrostatic assembly and in-situ reduction of Ni2+ and Co2+ ions. During carbonization and hydrothermal reaction, the addition of magnetic NiCo bimetal into biocarbon increased the interfacial polarization and impedance matching to improve the microwave absorption.
Straw-derived biochar was prepared as follows. Cleaned wheat straws were obtained through calcination, and the as-prepared wheat straw wastes were acidified by HF solution for 2 h and then washed with deionized water until the solution was neutralized. The mixture was then blended with KOH aqueous solution and dried at 70°C overnight. KOH was applied as an activation agent that contributes to the formation of micropores and defects in the biocarbon. The biocarbon product was then calcined at 1000°C under an inert atmosphere.
Straw-derived biocarbon/NiCo materials were fabricated by hydrothermal process. First, distilled water, hydrazine hydrate, biocarbon, CoCl2·6H2O, and NiCl2·6H2O (equivalent molar ratio between Ni2+ and Co2+) were combined and mixed evenly, transferred into a stainless-steel autoclave, and maintained at 180°C for 12 h. For convenience, the obtained biocarbon/NiCo materials prepared at 0.5, 1, and 2 mmol metal ions were labeled as C–NiCo-1, C–NiCo-2, and C–NiCo-3, respectively.
The phase composition and surface chemical composition were measured by X-ray diffraction (XRD, Smart Lab, Japan) and X-ray photoelectron spectroscopy (XPS, Thermo Fisher ESCALAB 250Xi, USA), respectively. The microstructures were investigated by a scanning electron microscope (SEM, JSM-7001F, Japan) and a transmission electron microscope (TEM, JEOL, JEM-2100F, Japan). Specific surface area (SBET) and pore structure were studied by analyzing N2 adsorption–desorption isotherms. Functional groups and defect degree were investigated by a Fourier transform infrared spectroscope (FT-IR, Nicolet iS10, USA) and a Raman spectrometer (LabRAM HR Evolution, Japan), respectively. The EM parameters of the 30wt% biocarbon@NiCo/paraffin wax composites were measured by a vector network analyzer (Agilent N5234A, USA).
The crystal structures of the straw-derived biocarbon/NiCo composites are shown in Fig. 1(a) and (b). The broad peak at 24° corresponded to amorphous carbon (Fig. 1(a)), indicating that biocarbon was successfully fabricated by calcining the wheat straws. The three diffraction peaks of the biocarbon/NiCo samples (Fig. 1(b)) located at 44.2°, 51.6°, and 76.0° were attributed to the (111), (200), and (220) crystal planes of faced-centered cubic (FCC) metals, respectively. In addition, diffraction peaks were found between FCC Co (PDF No. 15-0806) and FCC Ni (PDF No. 04-0850) metals, indicating the formation of NiCo alloys [32].
The chemical states and surface elements of biocarbon/NiCo material were analyzed by XPS as shown in Fig. 1(c)–(f). According to the full spectra of the XPS survey (Fig. 1(c)), the biocarbon/NiCo composites consisted of C, O, Co, and Ni elements. In the high-resolution C 1s XPS spectra (Fig. 1(d)), the peaks located at binding energies of 284.8 and 285.4 eV confirmed the presence of C–C (sp2 carbon atoms) and C–O bonds, respectively, which were obtained from carbonization and can be used as dipole polarization centers to cause polarization loss. In the Co 2p spectra (Fig. 1(e)), one typical peak located at 778.3 eV was attributed to the metallic state of Co. In addition, two peaks of 781.3 and 796.5 eV were associated with Co 2p3/2 and Co 2p1/2, respectively, and accompanied by the shake-up satellite peaks (786.6 and 804.0 eV denoted as “Satellite”). This finding indicated the existence of minor oxidation on the Co surface. Similarly, the Ni 2p spectra (Fig. 1(f)) presented the typical peak for metallic Ni (853.0 eV). Ni oxidation was proven via the peaks of Ni 2p3/2 and Ni 2p1/2 (855.9 and 873.4 eV) and the two “Satellite” (861.7 and 879.6 eV). All these results confirmed the presence of NiCo metals and slight oxidation in the biocarbon composites [8].
Fig. 2 shows the SEM images of the biocarbon/NiCo products. A smooth surface and a few micropores could be observed in the pure straw-derived biochar, as shown in Fig. 2(a). Compared with that of pristine biocarbon, the surface of the straw-derived biochar composites gradually became rough due to the formation of numerous anchored NiCo nanoparticles. This finding revealed that the in-situ reduction of NiCo bimetal occurred during the hydrothermal reaction. The number of nanoparticles deposited on porous straw-derived biocarbon increased with the NiCo amount. Therefore, the addition of magnetic NiCo might be favorable for alleviating EM wave absorption.
The TEM and high-resolution TEM (HRTEM) images of straw-derived biocarbon/NiCo composites are shown in Fig. 3. As displayed in Fig. 3(a)–(c), the nanoparticles were evenly distributed in the amorphous biocarbon matrix, and almost no agglomeration was observed. Fig. 3(e) and (f) shows the HRTEM image of the biocarbon/NiCo sample. The NiCo particles were tightly anchored on the carbon even after intensive grinding. The interlayer spacing of the lattice fringes of the presented NiCo particle was 0.205 nm (Fig. 3(f)), which is assigned to the (111) plane of face-centered cubic NiCo crystals. The considerably sharp ring-like features of the corresponding selected electron diffraction (SAED) pattern (Fig. 3(d)) suggest the polycrystalline nature of the as-prepared sample with clear (200) and (111) diffraction planes.
Fig. 4(a) shows the specific surface area and pore size of the three biocarbon/NiCo samples tested by N2 adsorption–desorption isotherms. The hysteresis loop with type IV isotherm confirmed the formation of mesopores in the composites. The SBET values of the C–NiCo-1, C–NiCo-2, and C–NiCo-3 samples (Fig. 4(b)) were 355.258, 400.003, and 357.185 m2/g, respectively. In Fig. 4(b), the pore size of the three composites was mainly in the range of 0.2–5 nm, with an average of 2.59, 2.45, and 2.73 nm, indicating their mesoporous characteristics. Therefore, the large specific surface area and broad pore size distribution can cause intense interfacial polarizations, which is believed to boost EM absorption. Fig. 4(c) displays the Raman spectra for evaluating the carbon graphitization degree of these biocarbon/NiCo composites. The carbon component has two characteristic peaks, namely, D (~1350 cm−1) and G (1590 cm−1) bands that are associated with the defects of the carbon atom lattice and the graphited carbon atom, respectively. In addition, the value of ID/IG was used to evaluate the degree of graphitization of the carbon-based material, where ID denotes the intensity of the D-peak and IG denotes the intensity of the G-peak. As shown in Fig. 4(c), the ID/IG ratios of C–NiCo-1, C–NiCo-2, and C–NiCo-3 were 1.12, 1.24, and 1.03, respectively, which are slightly larger than that of pure biocarbon (ID/IG = 1.02), This finding indicated that the addition of NiCo alloy has minimal effects on the graphitization degree. The slight change may originate from the catalytic graphitization effect of the NiCo alloy on local carbons [33]. The functional groups of the biocarbon/NiCo composites with different NiCo contents were characterized by FT-IR spectra (Fig. 4(d)). For the pure biocarbon, the characteristic absorption peaks of 3498 and 1629 cm−1 corresponded to the –OH (hydroxyl) stretching vibration peak and the deformation vibration absorption peak of water molecules, respectively. The stretching vibration peaks at ~1384 and 1050 cm−1 were ascribed to the –C–O and –C–OH, respectively. On the basis of the above results, the presence of the –OH and –O–C=O groups on the porous biocarbon surface confirmed that the straw-derived biochar could attract Ni2+ and Co2+ metal ions through electrostatic force.
Fig. 5 exhibits the measured EM parameters of the biocarbon/NiCo composites. The
As shown in Fig. 5(c) and (d), the
In general, the microwave energy dissipated in an applied electric field is attributed to conductivity and polarization loss. However, the use of materials with low amounts of the biocarbon/NiCo can suppress the formation of conductive networks in paraffin wax-based composites to a certain degree (30wt%). Therefore, the ohmic loss is not the main contributor to dielectric loss [39]. Owing to the vast contacting sites among porous biocarbon and NiCo alloys, a great number of dipolar pairs would accumulate in their interfaces and result in interfacial polarization loss. The relationship between the real and imaginary parts of the dielectric constant was drawn, as shown in Fig. 6, to further analyze the polarization relaxation process. This relationship can be expressed by the Debye dipolar polarization in the following equation of cole–cole curve [40–41]:
| {\left( {{\varepsilon ' } - \frac{{{\varepsilon _{\rm{s}}} + {\varepsilon _\infty }}}{2}} \right)^2} + {\left( {{\varepsilon ''}} \right)^2} = {\left( {\frac{{{\varepsilon _{\rm{s}}} - {\varepsilon _\infty }}}{2}} \right)^2} | (1) |
where
Fig. 7(a)–(d) reveals that the RL curves of the biocarbon/NiCo composites with different NiCo contents were dependent on the absorption thickness (2.0–3.0 mm) and frequency (2.0–18.0 GHz). RL is commonly calculated by transmission line theory shown in Eqs. (2) and (3) [14–15]:
| \mathrm{R}\mathrm{L}=20\,\mathrm{lg} \left|\frac{{Z}_{\text{in}}-{\text{Z}}_{0}}{{Z}_{\text{in}}\text+{\text{Z}}_{0}}\right| | (2) |
| {Z}_{\mathrm{i}\mathrm{n}}={Z}_{0}\sqrt{\frac{{\mu }_\text{r}}{{\varepsilon }_\text{r}}}\mathrm{tanh} \left({\rm{j}}\frac{2\mathrm{\text{π} }df\sqrt{{\mu }_\text{r}{\varepsilon }_\text{r}}}{c}\right) | (3) |
where Zin, Z0, c, f , d,
An appropriate impedance match obtained by tuning the component, thickness, and frequency of the promising absorber is pivotal in the absorbing properties. The matched thickness versus frequency was simulated using the quarter-wavelength model in the following formula:
| d=\frac{n\lambda }{4}=\frac{n{\lambda }_{0}}{4\sqrt{\left|{\mu }_{\mathrm{r}}\right|\left|{\varepsilon }_{\mathrm{r}}\right|}}(n=\mathrm{1,3},\mathrm{5,7},9,\dots ) | (4) |
where λ and λ0 are the wavelengths of the incident EM wave inside the material and in the vacuum, respectively. The minimal RL values shifted to the low frequency range when the simulated thickness was increased, and this finding agreed with the theory of the λ/4 matching model [43].
Table 1 presents the comparison of microwave capability of various carbon materials [10,44–54]. The NiCo/biocarbon composites exhibited competitive microwave absorption properties. The possible mechanism of the microwave absorption of porous biocarbon/NiCo composites was explained in the following aspects. First, the biocarbon and magnetic components can induce interfacial polarization loss and conductive loss, thus creating a high dielectric loss [55]. Second, the magnetic nature of NiCo alloys provides a good magnetic loss ability through natural resonance and eddy current effect [56]. Third, the NiCo alloy could transform EM energy into heat because of magnetic loss, thus leading to magnetic coupling interactions occurring in adjacent magnetic nanoparticles; the density of the magnetic flux line irradiated out from the shell surface could be slightly deformed and augmented around the NiCo, thus transferring the biocarbon surface to a “magnetism-rich” configuration [8]. Finally, the porous structure of straw-derived biochar would cause the scattering of EM waves in the absorber and dissipate the incident EM wave as far as possible [57]. Thus, the combination of dielectric loss and magnetic loss can provide a good impedance match, thereby endowing the biocarbon/NiCo composites with a high-efficiency absorbing ability.
| Sample | Filler content / wt% | Matrix | RLmin / dB | Thickness / mm | Frequency range (RL<−10 dB) / GHz | Ref. |
| Co/CoO@C | 50 | Paraffin | −45.0 | 6.0 | 4.4–18.0 | [44] |
| Co/C | 30 | Paraffin | −15.7 | 1.7 | 12.3–17.7 | [45] |
| Co/CNT | 50 | Paraffin | −16.0 | 2.0 | 5.1–8.8 | [46] |
| MWCNTs/Co | 60 | Epoxy resin | −37.0 | 5.25 | 6.7–18.0 | [47] |
| Co/MOF-derived C | 60 | paraffin | −25.0 | 1.9 | 12.3–18.0 | [48] |
| Fe–Co/ MOF-derived C | 50 | Paraffin | −21.7 | 1.2 | 12.2–18.0 | [49] |
| FeNi/C nanofibers | 30 | Paraffin | −24.8 | 2.7 | 12.8–17.2 | [50] |
| NiCo/C | 25 | Paraffin | −36.5 | 2.2 | 14.4–18.0 | [51] |
| Fe/CNT | 17 | Epoxy | −25.0 | 1.2 | 2.0–18.0 | [10] |
| Co0.2Ni0.8Fe2O4/RGO | 60 | Paraffin | −19.5 | 2.0 | 10.5–12.4 | [52] |
| Ni/C | 30 | Paraffin | −20.5 | 1.7 | 11.8–18.0 | [53] |
| Co–Ni/C | 30 | Paraffin | −34.3 | 3.3 | 13.8–18.0 | [53] |
| Fe–Ni/C | 30 | Paraffin | −42.3 | 5.7 | 15.2–18.0 | [53] |
| Ni/carbon spheres | 40 | paraffin | −20.3 | 9.0 | 12.5–15.5 | [54] |
| NiCo/biocarbon | 30 | Paraffin | −27.0 | 2.2 | 11.7–16.1 | This work |
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Porous structured biocarbon/NiCo materials were fabricated through high-temperature reduction and subsequent hydrothermal reaction. The magnetic NiCo alloys enhanced the dielectric loss through intense interfacial polarization. The formation of conductive networks between the porous biocarbon and NiCo alloys induced conductive loss. An exceptional RLmin of −27.0 dB at 2.2 mm thickness and an EAB width of 4.4 GHz (11.7–16.1 GHz) were achieved. We believe that the construction of magnetic biocarbon composites will be useful in designing a high-performance absorbing material.
This work was financially supported by the National Natural Science Foundation of China (No. U2004177), the Henan Province Science and Technology Research and Development Project in 2020, China (No. 202300410491), and the Key Scientific Research Projects of Provincial Universities in 2021, China (No. 21A430045).
The authors declare no conflict of interest.
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Figures(7) / Tables(1)
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| Sample | Filler content / wt% | Matrix | RLmin / dB | Thickness / mm | Frequency range (RL<−10 dB) / GHz | Ref. |
| Co/CoO@C | 50 | Paraffin | −45.0 | 6.0 | 4.4–18.0 | [44] |
| Co/C | 30 | Paraffin | −15.7 | 1.7 | 12.3–17.7 | [45] |
| Co/CNT | 50 | Paraffin | −16.0 | 2.0 | 5.1–8.8 | [46] |
| MWCNTs/Co | 60 | Epoxy resin | −37.0 | 5.25 | 6.7–18.0 | [47] |
| Co/MOF-derived C | 60 | paraffin | −25.0 | 1.9 | 12.3–18.0 | [48] |
| Fe–Co/ MOF-derived C | 50 | Paraffin | −21.7 | 1.2 | 12.2–18.0 | [49] |
| FeNi/C nanofibers | 30 | Paraffin | −24.8 | 2.7 | 12.8–17.2 | [50] |
| NiCo/C | 25 | Paraffin | −36.5 | 2.2 | 14.4–18.0 | [51] |
| Fe/CNT | 17 | Epoxy | −25.0 | 1.2 | 2.0–18.0 | [10] |
| Co0.2Ni0.8Fe2O4/RGO | 60 | Paraffin | −19.5 | 2.0 | 10.5–12.4 | [52] |
| Ni/C | 30 | Paraffin | −20.5 | 1.7 | 11.8–18.0 | [53] |
| Co–Ni/C | 30 | Paraffin | −34.3 | 3.3 | 13.8–18.0 | [53] |
| Fe–Ni/C | 30 | Paraffin | −42.3 | 5.7 | 15.2–18.0 | [53] |
| Ni/carbon spheres | 40 | paraffin | −20.3 | 9.0 | 12.5–15.5 | [54] |
| NiCo/biocarbon | 30 | Paraffin | −27.0 | 2.2 | 11.7–16.1 | This work |
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