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In situ regulation of microstructure and microwave-absorbing properties of FeSiAl through HNO3 oxidation

  • Yang Guo , Liwen Zhang EMAIL logo , Haipeng Lu EMAIL logo and Xian Jian
Published/Copyright: December 21, 2021
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 11 Issue 1

Abstract

Wrapping insulation of coatings is effective for enhancing the microwave-absorbing properties (MAPs) of ferromagnetic absorbents (FMAs). However, the process is still limited by the low bonding strength with the matrix. Herein, an in situ regulation strategy based on the preparation of thin thickness and strong adhesion insulating layers through HNO3 oxidation was developed to address the limitations. The oxidation process of FeSiAl (FSA) powders was carried out by HNO3 following three main steps. First, the original oxide layer first reacted with HNO3 to form Fe3+ and Al3+. Second, the oxide layer composed of Al2O3 and Fe3O4 was preferentially formed due to the negative change in Gibbs free energy. Finally, the oxide and pigment-deposition layers were subjected to competitive growth and dissolution accompanied by the dissolution of Fe and Al atoms. Oxidation time up to 10 min resulted in the formation of a bilayer structure with a thickness of ∼50 nm on the FSA surface, as well as an outer layer crammed of Al(OH)3 and Fe(OH)3, and an inner layer containing mixed Fe2O3, Fe3O4, Al2O3, and SiO2. The MAPs of as-treated FSA achieved minimum reflection loss (RL) of −25.90 dB at 13.36 GHz, as well as absorption bandwidth of 5.61 GHz (RL < −10 dB) at 10.13–15.74 GHz and thickness of 2.5 mm. In sum, the developed route looks promising for the preparation of high-performance FMAs.

Keywords: FeSiAl powders; HNO3 oxidation; microstructure; microwave-absorbing properties

1 Introduction

Advances in the high-speed development of electronic devices and systems led to serious electromagnetic pollution, which attracted increasing attention for the development of high-performance microwave absorbents (MAs) with less pollution [1,2,3,4]. This can be achieved by improving the properties of MAs, especially the reflection loss (RL) value and absorption bandwidth (ABW) below −10 dB through adjustment of composition and/or microstructure [5,6,7,8]. Most methods used for improving microwave-absorbing properties (MAPs) are based on rising the impedance matching degree (Δ) and attenuation constant (a) for electromagnetic wave (EMW) [9,10,11]. For ferromagnetic absorbents (FMAs; Fe, CoNi, and FeNi, etc.), playing an important role in MAs, one way to solve such issues lies in the preparation of thin insulation layers with high resistivity and strong bonding to FMAs [12,13].

In this regard, although organic layers provide desirable bonding strengths, they still suffer from poor resistance in high-temperature treatment (>200°C). This greatly restrains the posttreatment processing temperature [14], thereby reorienting the focus of research to inorganic insulating coatings with good thermal stability [15,16,17,18]. Common inorganic coatings include SiO2 [19], Al2O3 [20], ZnO [21], and MnO2 [22] prepared via hydrothermal reaction and sol–gel method. For hierarchical CoNi@SiO2@C structure, SiO2 and carbon layers could endow CoNi with improved absorbing capability [19]. In this case, RLmin value could reach −46.0 dB at 10.8 GHz, and ABW value may attain 5.6 GHz for film thickness of 2.2 mm. The reason for this has been attributed to the cladding layer enriching the polarization intensity (interface polarization and dipolar relaxation), leading to improved Δ. However, dual-oxide shell ZnO/Al2O3 prepared atomic layer deposition technique showed enhanced MAP of FeSiAl (FSA), thereby can be used as a strong barrier to improve the corrosion resistance [12]. However, the complex and high-cost process would inhibit the commercialization of these methods. In addition, the above processes used for preparing insulating layers suffer from low bonding strength with the matrix. For instance, although SiO2@Al2O3 layer in situ prepared by plasma-induced process is characterized by good bonding strength [23], further optimization in cost control and equipment simplification is required.

Herein, an alternative method involving a direct reaction of microwave absorber with HNO3 to form a surface insulating layer was proposed. To this end, FSA powders were first oxidized by 20 wt% HNO3 at different reaction times. Next, a bilayer structure with a thickness of ∼50 nm was formed at an oxidation time of 10 min, along with an outer layer crammed of Al(OH)3 and Fe(OH)3, as well as an inner layer containing mixed Fe2O3, Fe3O4, Al2O3, and SiO2 grown on the FSA surface. Field-emission scanning electron microscopy (FESEM) and X-ray photoelectron spectroscopy (XPS) analyses provided sufficient information about the morphology and elemental distribution of the oxidation layers, as well as the evolution and growth mechanism of oxide layers. The insulating layers raised the MAP of FSA, with RLmin reaching −25.90 dB at 13.36 GHz and ABW attaining 5.61 GHz at 10.13–15.74 GHz for the film thickness of 2.5 mm. FSA with good “Δ” and strong “a” was achieved by tuning the HNO3 oxidation time, providing a reference for the preparation of other high-performance FMAs.

2 Experimental

2.1 Materials

FSA powders (9.6 wt% Si, 5.4 wt% Al, and 85 wt% Fe) with a mean particle diameter of 45 μm were obtained from Changsha Hualiu Metallurgy Powder Co., Ltd. (Changsha) (AR 99.9%). The preparation process was based on an atomization method.

2.2 Sample synthesis

The materials were prepared by dispersing FSA powders (10 g) in HNO3-ethanol solution (20 wt%, 30 mL) under constant stirring at different oxidation times (1, 5, 10, 20, and 30 min). The resulting suspensions were then filtered and dried at 80°C to yield FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA, respectively.

2.3 Characterization

The surface morphologies of the samples were viewed by FESEM (JEOL 7600F, Japan Electronics). X-ray diffraction (XRD, XRD-7000, Shimadzu) at the scanning rate of 2°/min and 2θ of 10–90° was used to investigate the changes in the composition of all samples. The microstructure and composition details of FSA10NA were collected on transmission electron microscopy (TEM, FEI Talos F200x). The XPS data of oxidized coatings were recorded on Escalab 220i spectrometer (VG Scientific) with a monochromatic Al-Kα (1486.7 eV) radiation at 200 W working power. The static magnetic parameters of all samples were collected by vibrating sample magnetometry (cryogen-free magnet-9) mounted on an integrated physical property measurement system. The complex permittivity (ε r ) and permeability (μ r ) of FSA-based composites were obtained by a PNA-L Vector Network Analyzer (type-N5230A, Agilent) at frequencies of 0.5–18 GHz. FSA-based composites were made of FSA and paraffin at a mass ratio of 4:1. The power flow and power loss density were calculated through computer simulation technology (CST) using measured electromagnetic parameters as dielectric and magnetic dispersions. The simulation model was composed of ten lamina with a thickness of 0.25 mm and incident EMWs generated along the opposite Z-direction.

3 Results and discussion

In this study, FSA powders were subjected to a chemical method. Typically, 10 g of as-purchased FSA powders were homogenized in 20 wt% HNO3 solution and mechanically stirred for 1–30 min. The as-treated FSA samples were then filtered off, subsequently washed with deionized water and ethanol, and finally dried in an oven at 80°C for 24 h. The detailed preparation process is depicted in Figure 1a. The evolution SEM images of the microscopic morphologies of the as-treated FSA samples are summarized in Figure 1(b–g). For untreated FSA, the surface remained relatively smooth, as shown in Figure 1b. At processing time with HNO3 of 1 min (Figure 1c), the FSA exhibited a rough surface. The reason for this may have to do with the surface oxide layer of FSA prepared by atomization process during reaction with HNO3, resulting in an exposed matrix. At a treatment time of 5 min, smooth regions were formed on the FSA surface due to the production of thin oxidation coatings (Figure 1d). Further increase in the processing time to 10 min generated a smooth area (Figure 1e). However, corrosion pits and cracks appeared at oxidation times exceeding 20 min (Figure 1f). The cracks then disappeared and oxide films appeared at oxidation times exceeding 30 min (Figure 1g). The reaction products obtained by oxidation with 20 wt% HNO3 for 10 min were further analyzed by high-resolution TEM (Figure 1(h–j)). As shown in Figure 1h, the thickness of the oxide layer was less than 50 nm. The lattice fringe with a distance of 0.21 nm was consistent with Fe3O4 (Figure 1i), and that with a distance of 0.2 nm corresponded to (020) crystalline plane of Fe2O3 (Figure 1j).

Figure 1 (a) Schematic of as-treated FSA powders. SEM images showing the surface appearance of FSA powders oxidized at different periods: (b) 0 min, (c) 1 min, (d) 5 min, (e) 10 min, (f) 20 min, and (g) 30 min. (h) TEM image and corresponding HTEM images (I and j) of corrosion products of FSA10NA.
Figure 1

(a) Schematic of as-treated FSA powders. SEM images showing the surface appearance of FSA powders oxidized at different periods: (b) 0 min, (c) 1 min, (d) 5 min, (e) 10 min, (f) 20 min, and (g) 30 min. (h) TEM image and corresponding HTEM images (I and j) of corrosion products of FSA10NA.

The evolution of the surface composition of as-treated FSA during oxidation was studied by XRD. The diffraction peaks of FSA and Al75Fe25 were detected in Figure S1. All samples showed eight peaks corresponding to FSA (JCPDS no. 45-1206) and Al75Fe25 intermetallic compounds (JCPDS no. 45-1178). Also, no significant differences were noticed in XRD patterns of all samples due to the low contents of corrosion products.

The surface composition evolution of as-treated FSA was investigated by probing the surface composition of as-treated FSA using XPS (Figure 2). For untreated FSA, three prominent peaks were noticed at 706.5 [24], 709.9 [25], and 711.4 eV [26] in the high-resolution Fe 2p spectra (Figure 2a) attributable to the Fe0, Fe2+, and Fe3+, respectively. The rough evaluation of surface Fe2+/Fe3+ ratio (>1:2) indicated the existence of FeO. The high-resolution XPS of Al 2p also confirmed the presence of Al0 (72.1 eV) and Al3+ (74.2 eV; Figure 2b). Furthermore, the high-resolution O 1s XPS spectra exhibited four subpeaks located at 530.1, 530.7, 531.9, and 532.8 eV ascribed to FeO [27], Fe3O4 [28], Al2O3 [29], and SiO2 [30], respectively (Figure 2c). Hence, the surface oxide of FSA was produced during the atomization process.

Figure 2 High-resolution XPS spectra of (a) Fe 2p, (b) Al 2p, and (c) O 1s recorded for FSA. High-resolution XPS spectra of (d) Fe 2p, (e) Al 2p, and (f) O 1s recorded for FSA10NA. High-resolution XPS spectra of (g) Fe 2p, (h) Al 2p, and (i) O 1s recorded for FSA20NA.
Figure 2

High-resolution XPS spectra of (a) Fe 2p, (b) Al 2p, and (c) O 1s recorded for FSA. High-resolution XPS spectra of (d) Fe 2p, (e) Al 2p, and (f) O 1s recorded for FSA10NA. High-resolution XPS spectra of (g) Fe 2p, (h) Al 2p, and (i) O 1s recorded for FSA20NA.

After oxidation with 20 wt% HNO3 for 10 min, the oxidation products on the FSA surface changed significantly. As indicated by the marks in Figure 2d, the Fe 2p peak at binding energy of 712.3 eV could be assigned to Fe3+ [31], whereas that at 709.5 eV with a satellite signal at 716.0 eV was characteristic of Fe2+ [32]. In high-resolution Al 2p spectra, an Al3+ peak was detected at 73.7 eV and attributed to Al2O3 [33] (Figure 2e). Five peaks were reasonably fitted in O 1s spectrum of Figure 2f, located at 531.4, 531.9, 532.5, 533.2, and 533.8 eV corresponding to Fe3+ [28], Al3+ [29], Si4+ [30], and OH− [34], and organic matter (C–O–H) [35], respectively.

At corrosion time of 20 min, the Fe 2p spectrum presented two peaks at 712.5 eV (Fe3+) [36] and 706.5 eV (Fe0) (Figure 2g). As shown in Figure 2h, the Al 2p spectrum can be fitted into two components at 72.1 eV (Al0) and 74.00 eV (Al3+). The appearance of the zero-valent iron and aluminum indicated exposed substrate after corrosion with 20 wt% HNO3-alcohol solutions for 20 min. The O 1 s spectrum displayed in Figure 2f can be deconvoluted into Al3+ (531.9 eV), Si4+ (532.5 eV), OH− (533.2 eV), and organic compound (C–O–H; 533.8 eV).

Thermodynamically, Fe3O4 can further be oxidized into Fe2O3 by HNO3. Both zero-valent Fe and Al in FSA might be oxidized by HNO3. In this case, the change in Gibbs free energy (GFE) of Al showed the most negative value due to high reactivity. During the oxidation process, hydroxides like Al(OH)3 and Fe(OH)3 were generated as sediments and may react with nitric acid. Possible reactions occurring during the oxidation can be summarized as follows:

(1) Fe 3 O 4 + 10 HNO 3 = 3 Fe ( NO 3 ) 3 + NO 2 + 5 H 2 O, Δ r G m θ = − 327.34 kJ/mol,

(2) Fe 2 O 3 + HNO 3 = 2 Fe ( NO 3 ) 3 + 3 H 2 O, Δ r G m θ = − 565.26 kJ/mol,

(3) Al 2 O 3 + 6 HNO 3 = 2 Al ( NO 3 ) 3 + 3 H 2 O, Δ r G m θ = − 284.83 kJ/mol ,

(4) 2 Al + 6 HNO 3 = Al 2 O 3 + 6 NO 2 + 3 H 2 O, Δ r G m θ = − 1501.72 kJ/mol,

(5) 3 Fe + 8 HNO 3 = Fe 3 O 4 + 8 NO 2 + 4 H 2 O, Δ r G m θ = − 907.96 kJ/mol,

(6) Fe ( OH ) 3 + 3 HNO 3 = Fe ( NO ) 3 + 3 H 2 O, Δ r G m θ = − 102.82 kJ/mol, and

(7) Al ( OH ) 3 + 3 HNO 3 = Al ( NO ) 3 + 3 H 2 O, Δ r G m θ = − 136.32 kJ/mol .

The evolution of surface corrosion of FSA powders oxidized by 20 wt% HNO3 is illustrated in Figure 3. The evolution process mainly included three stages. For pure FSA, the surface oxide layer contained mixed FeO, Fe3O4, Al2O3, and SiO2 formed initially. At an oxidation time of 1 min (Stage I), the original oxide layer reacted with HNO3 to form Fe3+ and Al3+, and the FSA matrix became exposed. At a reaction time of 5 min (Stage II), the oxide layer composed of Al2O3 and Fe3O4 preferentially formed due to the more negative change in GFE. At an oxidation time of 10 min (Stage III), the oxide and precipitation layer experienced competitive growth and dissolution accompanied by the dissolution of iron and aluminum. An oxidation time up to 10 min resulted in the formation of a bilayer structure composed of an outer layer crammed of Fe(OH)3 and Al(OH)3, with an oxide layer containing mixed Fe2O3, Fe3O4, Al2O3, and SiO2. Also, large numbers of bubbles were generated from the violent exothermic reactions at oxidation reaction exceeding 10 min. Such a phenomenon accelerated the dissolution of the surface oxide layer of FSA. As corrosion time increased to 20 min, the oxidation reaction finished one cycle and started a new one. At an extended reaction time of 20 min (Stage IV), the oxide layer and precipitation layer gradually dissolved, leading to an exposed FSA matrix and a new oxidation round of Al and Fe. The difference in reaction rate resulted in the formation of corrosion pits and cracks on the FSA surface. Note that Stage IV was a repetition of Stage I.

Figure 3 Schematic showing the evolution mechanism of surface corrosion products of FSA powders oxidized with 20 wt% HNO3.
Figure 3

Schematic showing the evolution mechanism of surface corrosion products of FSA powders oxidized with 20 wt% HNO3.

The complex ε r and μ r obtained at frequencies of 0.5–18 GHz are summarized in Figure 4. The real part (μ′) and imaginary part (μ″) of μ r deputy the magnetic capacity, the real part (ε′) and imaginary part (ε″) of ε r express the dielectric capability. No significant differences in μ′ and μ″ of μ r were seen for samples oxidized by 20 wt% HNO3 for 1–30 min (Figure 4(a–b)). The ε′ of ε r first increased and then decreased within 1–10 min. Besides, the trend appeared periodically at a reaction time of 10–30 min. The ε′ of FSA5NA increased from 8.9 to 8.2 when compared to FSA, which enhanced from 7.0 to 7.5 (Figure 4c). The increase in 20 wt% HNO3 oxidation time to 10 min led to a decline in ε′ from 8.2 to 7.9. As the oxidation time further increased to 20 min, the ε′ of FSA20NA incremented from 7.9 to 8.7 and then 7.5 to 7.9. Two vibration peaks were observed at ∼10 and ∼14 GHz and could, respectively, be attributed to surface geometric enhancement effect and local space charge accumulation [37,38]. Nevertheless, the ε″ of ε r of as-treated FSA showed an opposite trend when compared to the real part, accompanied by some slight fluctuations (Figure 4d). The changes in ε″ and μ″ demonstrated the dissipation capabilities of the electric and magnetic energies, respectively [39]. In other words, FSA10NA exhibited excellent EMW attenuation and loss ability due to the high ε″ value originating from the oxide layers with unique micro-nano construction features.

Figure 4 Frequency dependence of electromagnetic parameters of FSA, FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA. (a) Real part and (b) imaginary part of complex permeability. (c) Real part and (d) imaginary part of complex permittivity.
Figure 4

Frequency dependence of electromagnetic parameters of FSA, FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA. (a) Real part and (b) imaginary part of complex permeability. (c) Real part and (d) imaginary part of complex permittivity.

The MAP values of all samples were obtained by calculating RL from measured electromagnetic parameters based on transmit line theory that can be expressed by equations (8) and (9) [40,41,42]:

(8) Z in = Z 0 μ r ε r tanh j 2 π f c d μ r ⋅ ε r ,

(9) RL = 20 lg Z in − Z 0 Z in + Z 0 ,

where Z in represents input impedance (Z in), Z 0 is air impedance, f refers to microwave frequency, d denotes absorber thickness, and c is the speed of light.

The three-dimensional (3D) colormaps of FSA, FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA obtained by regulating the thickness from 0.5 to 5.0 mm are depicted in Figure 5(a–f). The comparison of RL values at different thicknesses revealed FSA10NA with the strongest MAP. The RL curves of FSA, FSA10NA, and FSA20NA at 0.5–18 GHz and thickness of 2.5 mm are compared in Figure 5g. The RLmin of −25.30, −25.90, and −20.21 dB, as well as ABW of 4.47 GHz (11.29–15.75 GHz), 5.61 GHz (10.13–15.74 GHz), and 4.44 GHz (10.99–17.43 GHz), corresponded to FSA, FSA10NA, and FSA20NA, respectively. The RL curves in Figure S2 exhibited a shift in minimum RL frequency (f min) to lower values as d increased from 0.5 to 5.0 mm. Thus, thicker coatings suppressed the region with narrow reflection frequency. This can be explained by the quarter-wavelength equation:

t m = n λ 4 = n c 4 f m ∣ μ r ∣ ∣ ε r ∣ , ( n = 1 , 3 , 5 , … ) ,

[43,44,45], where t m presents the thickness of the absorber, λ stands for the wavelength of EMW, f m is the peak frequency of minimum RL, and c refers to the speed of light in vacuum. The comparison suggested enhanced MAP of FSA10NA toward EMW. The reason for this had to do with, first, the oxide layers formed on the FSA surface by nitric acid, which reduced the reflectivity of EMW and provided abundant electron transportation path to hop into the FSA10NA conducive due to loss in electromagnetic waves. Second, the polarization movement also fell behind the change in the alternating electromagnetic field, resulting in a relaxation phenomenon (Figure 5h). According to the Debye relaxation theory [46,47], a single semicircle curve of ε′ versus ε″ would indicate relative materials with strong polarization behavior, where each semicircle would present one Debye relaxation process. Here, FSA, FSA10NA, and FSA20NA exhibited some Cole–Cole semicircles, revealing strong polarization relaxations (Figure S3). Third, FSA10NA had better magnetic properties (122.6 emu/g), favorable to the formation of 3D magnetically connected network, which can catch up with the incident EMW to enhance the magnetic loss ability (Figure S4 and Table S1). In general, the magnetic loss capability induced by the eddy-current effect would primarily be located in the high-frequency region (∼11 GHz) for MAs. Here, the μ ″ ( μ ′ ) − 2 ( f ) − 1 values of FSA, FSA10NA, and FSA20NA were almost constant at 11–18 GHz (Figure S5), indicating the contribution of eddy-current loss to enhancement in MAP values (Figure 5i).

Figure 5 Frequency and thickness dependence of simulated 3D color maps of (a) FSA, (b) FSA1NA, (c) FSA5NA, (d) FSA10NA, (e) FSA20NA, and (f) FSA30NA. (g) RL curves of FSA, FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA in 0.5–18 GHz at a thickness of 2.5 mm. Schematic of (h) interfacial polarization, (i) eddy current, and (j) natural resonance in FSA-based 3D net.
Figure 5

Frequency and thickness dependence of simulated 3D color maps of (a) FSA, (b) FSA1NA, (c) FSA5NA, (d) FSA10NA, (e) FSA20NA, and (f) FSA30NA. (g) RL curves of FSA, FSA1NA, FSA5NA, FSA10NA, FSA20NA, and FSA30NA in 0.5–18 GHz at a thickness of 2.5 mm. Schematic of (h) interfacial polarization, (i) eddy current, and (j) natural resonance in FSA-based 3D net.

In general, the loss in capacity of MAs to EMW could be mainly reflected in the balance between Δ and a [48]. A higher a would lead to better dissipation ability for EMW, while a Δ closed to 0 would indicate optimal impedance matching characteristics. The a–f curves of FSA, FSA10NA, and FSA20NA are given in Figure S6. Obviously, the a of FSA10NA showed a rising trend at frequencies of 4–16 GHz, demonstrating an enhanced EMW attenuation ability. Figure 6a displays the Δ–f contour maps of FSA, FSA10NA, and FSA20NA under 0.5–5.0 mm. FSA10NA displayed the optimal Δ values (as blue as possible), showing the beneficial effects after moderate oxidation on MAP.

Figure 6 (a) The calculated data maps of FSA, FSA10NA, and FSA20NA at 0.5–18 GHz. (b) Power flow and (c) power loss density distribution images of FSA, FSA10NA, and FSA20NA under 2.5 mm at 13.36 GHz.
Figure 6

(a) The calculated data maps of FSA, FSA10NA, and FSA20NA at 0.5–18 GHz. (b) Power flow and (c) power loss density distribution images of FSA, FSA10NA, and FSA20NA under 2.5 mm at 13.36 GHz.

To further confirm the beneficial effects of moderate oxidation on “a” and “Δ”, the power flow and power loss density distributions of FSA, FSA10NA, and FSA20NA were obtained by CST simulations. To this end, the CST simulation model was confirmed by comparing the S11 parameters with the calculated RL values. As shown in Figure S8, the S11 curves of FSA, FSA10NA, and FSA20NA all agreed with the corresponding calculated RL, indicating the suitability of the simulation method. Based on this simulation model, the power flow density and power loss density were simulated through CST. Note that the power flow density can be obtained by equations (10) and (11) [49]：

(10) S av → = 1 T ∫ 0 T S → d t = 1 2 Re [ E → × H → ] ,

(11) S → = E → × H → .

According to the arrows marked with different color fills (Figure 6b), the power flow entering the absorbers declined in the following order: FSA10NA > FSA > FSA20NA. This further verified the impedance characteristics of all absorbers demonstrated in Figure 6a. The values of power loss density (W/m3) of FSA, FSA10NA, and FSA20NA under 2.5 mm at 13.36 GHz are displayed in Figure 6c. The values of power loss density of all three absorbers illustrated a revised trend under the same fixed conditions, confirming the gradual EMW consumption inside the absorbers. The comprehensive comparison revealed FSA10NA with optimal attenuation capacity when compared to FSA and FSA20NA. The above CST simulation results proved the importance of balance between “a” and “Δ.”

4 Conclusion

An ultra-thin insulating layer was successfully formed on the FSA surface through HNO3 oxidation. The oxidation process of FSA powders with 20 wt% HNO3 mainly involved three stages. At an oxidation time of 1 min (Stage I), the original oxide layer reacted with HNO3 to form Fe3+ and Al3+, and the FSA matrix was exposed. For oxidation reaction time up to 5 min (Stage II), an oxide layer composed of Al2O3 and Fe3O4 preferentially formed due to the more change in negative GFE. At an oxidation time of 10 min (Stage III), the oxide layer and precipitation layer exhibited competitive growth and dissolution accompanied by the dissolution of iron and aluminum. A bilayer structure with a thickness of ∼50 nm formed with the outer layer composed of Fe(OH)3 and Al(OH)3. The oxide layer contained mixed Fe2O3, Fe3O4, Al2O3, and SiO2. FSA10NA exhibited significantly enhanced MAP with RLmin reaching up to −25.90 dB at 13.36 GHz and ABW attaining up to 5.61 GHz (<−10 dB) at the thickness of 2.5 mm. In sum, the suggested method looks promising for the preparation of high-performance FMAs with stronger RL and wider ABW.

  1. Funding information: The study was supported by funds from the Guiding Science and Technology Plan Project of Panzhihua (2021ZD-G-4), the Open Projects of Vanadium and Titanium Resource Comprehensive Utilization Key Laboratory of Sichuan Province (2021FTSZ05 and 2021FTSZ11), the Open Foundation of National Engineering Research Center of Electromagnetic Radiation Control Materials (ZYGX202K003-1), and the National Natural Science Foundation of China (No. 51972046).

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2021-10-17
Revised: 2021-10-26
Accepted: 2021-10-31
Published Online: 2021-12-21

© 2022 Yang Guo 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/ntrev-2022-0012
Keywords for this article
FeSiAl powders; HNO3 oxidation; microstructure; microwave-absorbing properties
Creative Commons
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Articles in the same Issue

  1. Research Articles
  2. Theoretical and experimental investigation of MWCNT dispersion effect on the elastic modulus of flexible PDMS/MWCNT nanocomposites
  3. Mechanical, morphological, and fracture-deformation behavior of MWCNTs-reinforced (Al–Cu–Mg–T351) alloy cast nanocomposites fabricated by optimized mechanical milling and powder metallurgy techniques
  4. Flammability and physical stability of sugar palm crystalline nanocellulose reinforced thermoplastic sugar palm starch/poly(lactic acid) blend bionanocomposites
  5. Glutathione-loaded non-ionic surfactant niosomes: A new approach to improve oral bioavailability and hepatoprotective efficacy of glutathione
  6. Relationship between mechano-bactericidal activity and nanoblades density on chemically strengthened glass
  7. In situ regulation of microstructure and microwave-absorbing properties of FeSiAl through HNO3 oxidation
  8. Research on a mechanical model of magnetorheological fluid different diameter particles
  9. Nanomechanical and dynamic mechanical properties of rubber–wood–plastic composites
  10. Investigative properties of CeO2 doped with niobium: A combined characterization and DFT studies
  11. Miniaturized peptidomimetics and nano-vesiculation in endothelin types through probable nano-disk formation and structure property relationships of endothelins’ fragments
  12. N/S co-doped CoSe/C nanocubes as anode materials for Li-ion batteries
  13. Synergistic effects of halloysite nanotubes with metal and phosphorus additives on the optimal design of eco-friendly sandwich panels with maximum flame resistance and minimum weight
  14. Octreotide-conjugated silver nanoparticles for active targeting of somatostatin receptors and their application in a nebulized rat model
  15. Controllable morphology of Bi2S3 nanostructures formed via hydrothermal vulcanization of Bi2O3 thin-film layer and their photoelectrocatalytic performances
  16. Development of (−)-epigallocatechin-3-gallate-loaded folate receptor-targeted nanoparticles for prostate cancer treatment
  17. Enhancement of the mechanical properties of HDPE mineral nanocomposites by filler particles modulation of the matrix plastic/elastic behavior
  18. Effect of plasticizers on the properties of sugar palm nanocellulose/cinnamon essential oil reinforced starch bionanocomposite films
  19. Optimization of nano coating to reduce the thermal deformation of ball screws
  20. Preparation of efficient piezoelectric PVDF–HFP/Ni composite films by high electric field poling
  21. MHD dissipative Casson nanofluid liquid film flow due to an unsteady stretching sheet with radiation influence and slip velocity phenomenon
  22. Effects of nano-SiO2 modification on rubberised mortar and concrete with recycled coarse aggregates
  23. Mechanical and microscopic properties of fiber-reinforced coal gangue-based geopolymer concrete
  24. Effect of morphology and size on the thermodynamic stability of cerium oxide nanoparticles: Experiment and molecular dynamics calculation
  25. Mechanical performance of a CFRP composite reinforced via gelatin-CNTs: A study on fiber interfacial enhancement and matrix enhancement
  26. A practical review over surface modification, nanopatterns, emerging materials, drug delivery systems, and their biophysiochemical properties for dental implants: Recent progresses and advances
  27. HTR: An ultra-high speed algorithm for cage recognition of clathrate hydrates
  28. Effects of microalloying elements added by in situ synthesis on the microstructure of WCu composites
  29. A highly sensitive nanobiosensor based on aptamer-conjugated graphene-decorated rhodium nanoparticles for detection of HER2-positive circulating tumor cells
  30. Progressive collapse performance of shear strengthened RC frames by nano CFRP
  31. Core–shell heterostructured composites of carbon nanotubes and imine-linked hyperbranched polymers as metal-free Li-ion anodes
  32. A Galerkin strategy for tri-hybridized mixture in ethylene glycol comprising variable diffusion and thermal conductivity using non-Fourier’s theory
  33. Simple models for tensile modulus of shape memory polymer nanocomposites at ambient temperature
  34. Preparation and morphological studies of tin sulfide nanoparticles and use as efficient photocatalysts for the degradation of rhodamine B and phenol
  35. Polyethyleneimine-impregnated activated carbon nanofiber composited graphene-derived rice husk char for efficient post-combustion CO2 capture
  36. Electrospun nanofibers of Co3O4 nanocrystals encapsulated in cyclized-polyacrylonitrile for lithium storage
  37. Pitting corrosion induced on high-strength high carbon steel wire in high alkaline deaerated chloride electrolyte
  38. Formulation of polymeric nanoparticles loaded sorafenib; evaluation of cytotoxicity, molecular evaluation, and gene expression studies in lung and breast cancer cell lines
  39. Engineered nanocomposites in asphalt binders
  40. Influence of loading voltage, domain ratio, and additional load on the actuation of dielectric elastomer
  41. Thermally induced hex-graphene transitions in 2D carbon crystals
  42. The surface modification effect on the interfacial properties of glass fiber-reinforced epoxy: A molecular dynamics study
  43. Molecular dynamics study of deformation mechanism of interfacial microzone of Cu/Al2Cu/Al composites under tension
  44. Nanocolloid simulators of luminescent solar concentrator photovoltaic windows
  45. Compressive strength and anti-chloride ion penetration assessment of geopolymer mortar merging PVA fiber and nano-SiO2 using RBF–BP composite neural network
  46. Effect of 3-mercapto-1-propane sulfonate sulfonic acid and polyvinylpyrrolidone on the growth of cobalt pillar by electrodeposition
  47. Dynamics of convective slippery constraints on hybrid radiative Sutterby nanofluid flow by Galerkin finite element simulation
  48. Preparation of vanadium by the magnesiothermic self-propagating reduction and process control
  49. Microstructure-dependent photoelectrocatalytic activity of heterogeneous ZnO–ZnS nanosheets
  50. Cytotoxic and pro-inflammatory effects of molybdenum and tungsten disulphide on human bronchial cells
  51. Improving recycled aggregate concrete by compression casting and nano-silica
  52. Chemically reactive Maxwell nanoliquid flow by a stretching surface in the frames of Newtonian heating, nonlinear convection and radiative flux: Nanopolymer flow processing simulation
  53. Nonlinear dynamic and crack behaviors of carbon nanotubes-reinforced composites with various geometries
  54. Biosynthesis of copper oxide nanoparticles and its therapeutic efficacy against colon cancer
  55. Synthesis and characterization of smart stimuli-responsive herbal drug-encapsulated nanoniosome particles for efficient treatment of breast cancer
  56. Homotopic simulation for heat transport phenomenon of the Burgers nanofluids flow over a stretching cylinder with thermal convective and zero mass flux conditions
  57. Incorporation of copper and strontium ions in TiO2 nanotubes via dopamine to enhance hemocompatibility and cytocompatibility
  58. Mechanical, thermal, and barrier properties of starch films incorporated with chitosan nanoparticles
  59. Mechanical properties and microstructure of nano-strengthened recycled aggregate concrete
  60. Glucose-responsive nanogels efficiently maintain the stability and activity of therapeutic enzymes
  61. Tunning matrix rheology and mechanical performance of ultra-high performance concrete using cellulose nanofibers
  62. Flexible MXene/copper/cellulose nanofiber heat spreader films with enhanced thermal conductivity
  63. Promoted charge separation and specific surface area via interlacing of N-doped titanium dioxide nanotubes on carbon nitride nanosheets for photocatalytic degradation of Rhodamine B
  64. Elucidating the role of silicon dioxide and titanium dioxide nanoparticles in mitigating the disease of the eggplant caused by Phomopsis vexans, Ralstonia solanacearum, and root-knot nematode Meloidogyne incognita
  65. An implication of magnetic dipole in Carreau Yasuda liquid influenced by engine oil using ternary hybrid nanomaterial
  66. Robust synthesis of a composite phase of copper vanadium oxide with enhanced performance for durable aqueous Zn-ion batteries
  67. Tunning self-assembled phases of bovine serum albumin via hydrothermal process to synthesize novel functional hydrogel for skin protection against UVB
  68. A comparative experimental study on damping properties of epoxy nanocomposite beams reinforced with carbon nanotubes and graphene nanoplatelets
  69. Lightweight and hydrophobic Ni/GO/PVA composite aerogels for ultrahigh performance electromagnetic interference shielding
  70. Research on the auxetic behavior and mechanical properties of periodically rotating graphene nanostructures
  71. Repairing performances of novel cement mortar modified with graphene oxide and polyacrylate polymer
  72. Closed-loop recycling and fabrication of hydrophilic CNT films with high performance
  73. Design of thin-film configuration of SnO2–Ag2O composites for NO2 gas-sensing applications
  74. Study on stress distribution of SiC/Al composites based on microstructure models with microns and nanoparticles
  75. PVDF green nanofibers as potential carriers for improving self-healing and mechanical properties of carbon fiber/epoxy prepregs
  76. Osteogenesis capability of three-dimensionally printed poly(lactic acid)-halloysite nanotube scaffolds containing strontium ranelate
  77. Silver nanoparticles induce mitochondria-dependent apoptosis and late non-canonical autophagy in HT-29 colon cancer cells
  78. Preparation and bonding mechanisms of polymer/metal hybrid composite by nano molding technology
  79. Damage self-sensing and strain monitoring of glass-reinforced epoxy composite impregnated with graphene nanoplatelet and multiwalled carbon nanotubes
  80. Thermal analysis characterisation of solar-powered ship using Oldroyd hybrid nanofluids in parabolic trough solar collector: An optimal thermal application
  81. Pyrene-functionalized halloysite nanotubes for simultaneously detecting and separating Hg(ii) in aqueous media: A comprehensive comparison on interparticle and intraparticle excimers
  82. Fabrication of self-assembly CNT flexible film and its piezoresistive sensing behaviors
  83. Thermal valuation and entropy inspection of second-grade nanoscale fluid flow over a stretching surface by applying Koo–Kleinstreuer–Li relation
  84. Mechanical properties and microstructure of nano-SiO2 and basalt-fiber-reinforced recycled aggregate concrete
  85. Characterization and tribology performance of polyaniline-coated nanodiamond lubricant additives
  86. Combined impact of Marangoni convection and thermophoretic particle deposition on chemically reactive transport of nanofluid flow over a stretching surface
  87. Spark plasma extrusion of binder free hydroxyapatite powder
  88. An investigation on thermo-mechanical performance of graphene-oxide-reinforced shape memory polymer
  89. Effect of nanoadditives on the novel leather fiber/recycled poly(ethylene-vinyl-acetate) polymer composites for multifunctional applications: Fabrication, characterizations, and multiobjective optimization using central composite design
  90. Design selection for a hemispherical dimple core sandwich panel using hybrid multi-criteria decision-making methods
  91. Improving tensile strength and impact toughness of plasticized poly(lactic acid) biocomposites by incorporating nanofibrillated cellulose
  92. Green synthesis of spinel copper ferrite (CuFe2O4) nanoparticles and their toxicity
  93. The effect of TaC and NbC hybrid and mono-nanoparticles on AA2024 nanocomposites: Microstructure, strengthening, and artificial aging
  94. Excited-state geometry relaxation of pyrene-modified cellulose nanocrystals under UV-light excitation for detecting Fe3+
  95. Effect of CNTs and MEA on the creep of face-slab concrete at an early age
  96. Effect of deformation conditions on compression phase transformation of AZ31
  97. Application of MXene as a new generation of highly conductive coating materials for electromembrane-surrounded solid-phase microextraction
  98. A comparative study of the elasto-plastic properties for ceramic nanocomposites filled by graphene or graphene oxide nanoplates
  99. Encapsulation strategies for improving the biological behavior of CdS@ZIF-8 nanocomposites
  100. Biosynthesis of ZnO NPs from pumpkin seeds’ extract and elucidation of its anticancer potential against breast cancer
  101. Preliminary trials of the gold nanoparticles conjugated chrysin: An assessment of anti-oxidant, anti-microbial, and in vitro cytotoxic activities of a nanoformulated flavonoid
  102. Effect of micron-scale pores increased by nano-SiO2 sol modification on the strength of cement mortar
  103. Fractional simulations for thermal flow of hybrid nanofluid with aluminum oxide and titanium oxide nanoparticles with water and blood base fluids
  104. The effect of graphene nano-powder on the viscosity of water: An experimental study and artificial neural network modeling
  105. Development of a novel heat- and shear-resistant nano-silica gelling agent
  106. Characterization, biocompatibility and in vivo of nominal MnO2-containing wollastonite glass-ceramic
  107. Entropy production simulation of second-grade magnetic nanomaterials flowing across an expanding surface with viscidness dissipative flux
  108. Enhancement in structural, morphological, and optical properties of copper oxide for optoelectronic device applications
  109. Aptamer-functionalized chitosan-coated gold nanoparticle complex as a suitable targeted drug carrier for improved breast cancer treatment
  110. Performance and overall evaluation of nano-alumina-modified asphalt mixture
  111. Analysis of pure nanofluid (GO/engine oil) and hybrid nanofluid (GO–Fe3O4/engine oil): Novel thermal and magnetic features
  112. Synthesis of Ag@AgCl modified anatase/rutile/brookite mixed phase TiO2 and their photocatalytic property
  113. Mechanisms and influential variables on the abrasion resistance hydraulic concrete
  114. Synergistic reinforcement mechanism of basalt fiber/cellulose nanocrystals/polypropylene composites
  115. Achieving excellent oxidation resistance and mechanical properties of TiB2–B4C/carbon aerogel composites by quick-gelation and mechanical mixing
  116. Microwave-assisted sol–gel template-free synthesis and characterization of silica nanoparticles obtained from South African coal fly ash
  117. Pulsed laser-assisted synthesis of nano nickel(ii) oxide-anchored graphitic carbon nitride: Characterizations and their potential antibacterial/anti-biofilm applications
  118. Effects of nano-ZrSi2 on thermal stability of phenolic resin and thermal reusability of quartz–phenolic composites
  119. Benzaldehyde derivatives on tin electroplating as corrosion resistance for fabricating copper circuit
  120. Mechanical and heat transfer properties of 4D-printed shape memory graphene oxide/epoxy acrylate composites
  121. Coupling the vanadium-induced amorphous/crystalline NiFe2O4 with phosphide heterojunction toward active oxygen evolution reaction catalysts
  122. Graphene-oxide-reinforced cement composites mechanical and microstructural characteristics at elevated temperatures
  123. Gray correlation analysis of factors influencing compressive strength and durability of nano-SiO2 and PVA fiber reinforced geopolymer mortar
  124. Preparation of layered gradient Cu–Cr–Ti alloy with excellent mechanical properties, thermal stability, and electrical conductivity
  125. Recovery of Cr from chrome-containing leather wastes to develop aluminum-based composite material along with Al2O3 ceramic particles: An ingenious approach
  126. Mechanisms of the improved stiffness of flexible polymers under impact loading
  127. Anticancer potential of gold nanoparticles (AuNPs) using a battery of in vitro tests
  128. Review Articles
  129. Proposed approaches for coronaviruses elimination from wastewater: Membrane techniques and nanotechnology solutions
  130. Application of Pickering emulsion in oil drilling and production
  131. The contribution of microfluidics to the fight against tuberculosis
  132. Graphene-based biosensors for disease theranostics: Development, applications, and recent advancements
  133. Synthesis and encapsulation of iron oxide nanorods for application in magnetic hyperthermia and photothermal therapy
  134. Contemporary nano-architectured drugs and leads for ανβ3 integrin-based chemotherapy: Rationale and retrospect
  135. State-of-the-art review of fabrication, application, and mechanical properties of functionally graded porous nanocomposite materials
  136. Insights on magnetic spinel ferrites for targeted drug delivery and hyperthermia applications
  137. A review on heterogeneous oxidation of acetaminophen based on micro and nanoparticles catalyzed by different activators
  138. Early diagnosis of lung cancer using magnetic nanoparticles-integrated systems
  139. Advances in ZnO: Manipulation of defects for enhancing their technological potentials
  140. Efficacious nanomedicine track toward combating COVID-19
  141. A review of the design, processes, and properties of Mg-based composites
  142. Green synthesis of nanoparticles for varied applications: Green renewable resources and energy-efficient synthetic routes
  143. Two-dimensional nanomaterial-based polymer composites: Fundamentals and applications
  144. Recent progress and challenges in plasmonic nanomaterials
  145. Apoptotic cell-derived micro/nanosized extracellular vesicles in tissue regeneration
  146. Electronic noses based on metal oxide nanowires: A review
  147. Framework materials for supercapacitors
  148. An overview on the reproductive toxicity of graphene derivatives: Highlighting the importance
  149. Antibacterial nanomaterials: Upcoming hope to overcome antibiotic resistance crisis
  150. Research progress of carbon materials in the field of three-dimensional printing polymer nanocomposites
  151. A review of atomic layer deposition modelling and simulation methodologies: Density functional theory and molecular dynamics
  152. Recent advances in the preparation of PVDF-based piezoelectric materials
  153. Recent developments in tensile properties of friction welding of carbon fiber-reinforced composite: A review
  154. Comprehensive review of the properties of fly ash-based geopolymer with additive of nano-SiO2
  155. Perspectives in biopolymer/graphene-based composite application: Advances, challenges, and recommendations
  156. Graphene-based nanocomposite using new modeling molecular dynamic simulations for proposed neutralizing mechanism and real-time sensing of COVID-19
  157. Nanotechnology application on bamboo materials: A review
  158. Recent developments and future perspectives of biorenewable nanocomposites for advanced applications
  159. Nanostructured lipid carrier system: A compendium of their formulation development approaches, optimization strategies by quality by design, and recent applications in drug delivery
  160. 3D printing customized design of human bone tissue implant and its application
  161. Design, preparation, and functionalization of nanobiomaterials for enhanced efficacy in current and future biomedical applications
  162. A brief review of nanoparticles-doped PEDOT:PSS nanocomposite for OLED and OPV
  163. Nanotechnology interventions as a putative tool for the treatment of dental afflictions
  164. Recent advancements in metal–organic frameworks integrating quantum dots (QDs@MOF) and their potential applications
  165. A focused review of short electrospun nanofiber preparation techniques for composite reinforcement
  166. Microstructural characteristics and nano-modification of interfacial transition zone in concrete: A review
  167. Latest developments in the upconversion nanotechnology for the rapid detection of food safety: A review
  168. Strategic applications of nano-fertilizers for sustainable agriculture: Benefits and bottlenecks
  169. Molecular dynamics application of cocrystal energetic materials: A review
  170. Synthesis and application of nanometer hydroxyapatite in biomedicine
  171. Cutting-edge development in waste-recycled nanomaterials for energy storage and conversion applications
  172. Biological applications of ternary quantum dots: A review
  173. Nanotherapeutics for hydrogen sulfide-involved treatment: An emerging approach for cancer therapy
  174. Application of antibacterial nanoparticles in orthodontic materials
  175. Effect of natural-based biological hydrogels combined with growth factors on skin wound healing
  176. Nanozymes – A route to overcome microbial resistance: A viewpoint
  177. Recent developments and applications of smart nanoparticles in biomedicine
  178. Contemporary review on carbon nanotube (CNT) composites and their impact on multifarious applications
  179. Interfacial interactions and reinforcing mechanisms of cellulose and chitin nanomaterials and starch derivatives for cement and concrete strength and durability enhancement: A review
  180. Diamond-like carbon films for tribological modification of rubber
  181. Layered double hydroxides (LDHs) modified cement-based materials: A systematic review
  182. Recent research progress and advanced applications of silica/polymer nanocomposites
  183. Modeling of supramolecular biopolymers: Leading the in silico revolution of tissue engineering and nanomedicine
  184. Recent advances in perovskites-based optoelectronics
  185. Biogenic synthesis of palladium nanoparticles: New production methods and applications
  186. A comprehensive review of nanofluids with fractional derivatives: Modeling and application
  187. Electrospinning of marine polysaccharides: Processing and chemical aspects, challenges, and future prospects
  188. Electrohydrodynamic printing for demanding devices: A review of processing and applications
  189. Rapid Communications
  190. Structural material with designed thermal twist for a simple actuation
  191. Recent advances in photothermal materials for solar-driven crude oil adsorption
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