CN112492869A - Prussian blue redox-derived iron-based wave-absorbing material and preparation method thereof - Google Patents
Prussian blue redox-derived iron-based wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Prussian blue redox-derived iron-based wave-absorbing material and a preparation method thereof, belonging to the technical field of microwave absorbing materials. The iron-based wave-absorbing material is black-gray powder and consists of iron-based magnetic particles, and the material components can comprise Fe, FeO and Fe3O4、C、Fe3C. The effective absorption bandwidth of the composite material can reach 5.44 GHz under the conditions of 40 wt% filling degree and 1.5 mm thickness, and the excellent wave-absorbing performance of low thickness and broadband is shown. The preparation method is simple and feasible, and comprises air oxidation, resin coating and carbon thermal reduction. Wherein, the air oxidation of the Prussian blue effectively ensures that the derivative product has higher magnetic phase content, and the content of the phenolic resin is accurately regulated and controlled to realize the Fe2O3Effective control of the degree of reduction, composition of the derivative phase and microstructure. The moderate particle size and high magnetic phase content ensure strong magnetic losses, while the presence of conductive iron, graphite, and multi-phase interfaces ensure strong dielectric losses and proper impedance matching.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and particularly relates to a Prussian blue redox-derived iron-based wave absorbing material and a preparation method thereof.
Background
In recent years, microwave detection communication technology is rapidly developed in the military and civil fields, and troubles are brought to the safety of stealth military targets and the normal operation of electronic equipment. The electromagnetic wave absorbing material can absorb electromagnetic waves by means of a dielectric or magnetic loss mechanism, so as to effectively eliminate adverse effects of the electromagnetic waves, and thus the electromagnetic wave absorbing material becomes a current hot research field. A great deal of research finds that the Metal Organic Frameworks (MOFs) derived iron-based magnetic wave-absorbing material has high conductivity and excellent magnetic loss and can become an ideal microwave absorbing material. For example, Wu et al use Fe-MIL-88A as a precursor at N2Heat treatment under atmosphere to obtain porous rod-like Fe/Fe3O4A/C material having an effective absorption band up to 4.6 GHz at 40 wt% fill (Carbon 2019, 145, 433). Zhu et al successfully prepared a porous iron-based wave-absorbing material with strong dielectric loss by using MIL-100-Fe as a precursor and performing two-step heat treatment through argon and air, and could obtain an effective absorption band of 4 GHz at a thickness of 3 mm (J. mater. Sci. mater. electron. 2020, 31, 6843). However, the derived wave-absorbing material still has the problems of large matching thickness and narrow effective absorption band, and is difficult to meet the requirements of practical application. From the derivation process, most of research focuses on carbothermic reduction of iron MOFs, and some research adopts the subsequent air oxidation technology. The direct carbothermic reduction of the iron MOFs is easy to generate excessive graphite phases, and the product components lack an effective regulation and control means. Although the subsequent air oxidation process can remove part of the carbon material, Fe and Fe can be caused3O4Oxidation of the iso-magnetic phase causes a substantial weakening of the magnetic losses. Therefore, the process adopted by the wave-absorbing material has the defect that the components of the material are difficult to regulate and control as required, so that the derived wave-absorbing material is easy to cause excessive dependence on the strong dielectric loss of a graphite phase, and the effective absorption of incident microwaves is difficult to realize.
Disclosure of Invention
In order to solve the problem that the effective absorption band of the MOFs derived iron-based wave-absorbing material is narrow under low thickness, the invention provides a Prussian blue redox derived iron-based wave-absorbing material and a preparation method of the Prussian blue redox derived iron-based wave-absorbing material.
The Prussian blue redox-derived iron-based wave-absorbing material is black gray powder and consists of iron-based magnetic particles, the particle size of the iron-based magnetic particles is 200-2000 nm, and the iron-based magnetic particles comprise iron (Fe), iron oxide (FeO) and ferroferric oxide (Fe)3O4) Carbon (C), iron carbide (Fe)3C) (ii) a Wherein the iron (Fe) content is 25-90 wt%;
the effective absorption bandwidth of the iron-based wave-absorbing material under the conditions that the filling degree is 40 wt% and the thickness is 1-5 mm is 0-5.44 GHz, and the maximum coverage rate of the iron-based wave-absorbing material in a Ku wave band is more than 90%.
The preparation operation steps of the Prussian blue redox-derived iron-based wave-absorbing material are as follows:
(1) dissolving required amount of potassium ferrocyanide, polyvinylpyrrolidone and hydrochloric acid in a proper amount of deionized water to obtain a mixed material, wherein Fe3+The concentration of the hydrochloric acid is 5-20 mmol/L, the adding volume of the hydrochloric acid is 1-3 mL, the concentration of the polyvinylpyrrolidone (K-30) in the solution is 1.67-3.33 mmol/L, and the volume of the deionized water is 150-300 mL; the mixed materials are subjected to heat preservation reaction for 1-24 hours in an oven at the temperature of 80 ℃, and are subjected to centrifugation, filtration, cleaning and drying to obtain Prussian blue powder; the Prussian blue powder is blue powder, and the molecular formula is Fe4[Fe(CN)6]3The particles are cubic and have the particle size of 200-2000 nm;
(2) carrying out high-temperature heat treatment on the Prussian blue powder in air, wherein the heating rate is 2-10 ℃/min, the heat preservation temperature is 300-500 ℃, and the heat preservation time is 3-9 h; naturally cooling to obtain ferric oxide (Fe)2O3) Powder; the ferric oxide powder is dark red powder, the granules of the ferric oxide powder are in an irregular cube shape formed by assembling small granules, and the grain diameter is 100-2000 nm;
(3) 1 g of ferric oxide (Fe)2O3) Ultrasonically dispersing the powder in a mixed solution, wherein the volume of deionized water in the mixed solution is 60-100 mL, the volume of absolute ethyl alcohol is 20-40 mL, and the volume of ammonia water is 0.2-1 mL; adding 0.1-1g, resorcinol, and mixing uniformly; adding 0.2-1.2 mL of formaldehyde solution with the concentration of 38 wt%, and polymerizing for 24 h; centrifuging, cleaning and drying to obtain the ferric oxide (Fe) coated by the phenolic resin2O3) Powder; the ferric oxide powder coated by the phenolic resin is brown powder, particles are irregular cubes, a resin coating layer exists on the surface of the particles, the particles have an agglomeration phenomenon, and the particle size is 10-2000 nm;
(4) iron (Fe) oxide coated with a phenolic resin2O3) And (3) carrying out heat treatment on the powder in inert gas, wherein the heating rate of the heat treatment is 1-10 ℃/min, the temperature is 650-750 ℃, the heat preservation time is 1-4 h, and naturally cooling to obtain the iron-based wave-absorbing material derived from iron Prussian blue oxidation reduction.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the invention takes Prussian blue as a precursor, and prepares the iron-based wave-absorbing material by means of air oxidation, resin coating and carbon thermal reduction. The obtained iron-based wave-absorbing material can avoid the adverse effect of overlarge eddy current on magnetic conductivity due to proper particle size, and can meet the design requirements of high-efficiency wave absorption on complex magnetic conductivity and magnetic loss due to the fact that the content of magnetic phase components is far higher than that of a traditional carbon-based derivative wave-absorbing agent. And the existence of Fe simple substance, graphite phase C material and other strong conductive substances and the existence of a multiphase interface structure are also beneficial to the enhancement of dielectric loss and the improvement of impedance matching. Therefore, under the condition that the filling degree is 40 wt%, the effective absorption bandwidth of the optimal product under the thickness of 1.5 mm can reach 5.44 GHz, the coverage rate of a Ku wave band is more than 90%, and the ideal wave-absorbing performance is shown.
2. The invention breaks through the limitation of the MOFs derived Fe-based wave-absorbing material process, and develops a brand-new process of resin coating and carbon thermal reduction after air oxidation. The air oxidation process removes organic elements in the Prussian blue, and provides a foundation for the high magnetic phase content of subsequent products. And the content of the phenolic resin is accurately regulated and controlled, so that the requirement of reducing Fe is met2O3The method meets the requirement of obtaining the iron-based wave-absorbing material with strong magnetic loss, and effectively controls the residual quantity of the carbon material in the derivative. The preparation cost of the novel processLow cost, simple and feasible property and wide applicability.
Drawings
Fig. 1 is an SEM photograph of the prussian blue powder obtained in example 1.
FIG. 2 shows Fe obtained in example 12O3SEM photograph of the powder.
FIG. 3 is an SEM photograph of the iron-based wave absorbing material prepared in example 1.
FIG. 4 is an XRD spectrum of the iron-based absorbing material prepared in example 1.
FIG. 5 is an electromagnetic parameter diagram of the iron-based wave-absorbing material prepared in example 1.
FIG. 6 is a reflection loss curve of the iron-based wave-absorbing material obtained in example 1.
FIG. 7 is an XRD spectrum of the iron-based absorbing material prepared in example 2.
FIG. 8 is an electromagnetic parameter diagram of the iron-based wave-absorbing material prepared in example 2.
FIG. 9 is a reflection loss curve of the iron-based wave-absorbing material prepared in example 2.
FIG. 10 is an XRD spectrum of the iron-based absorbing material prepared in example 3.
FIG. 11 is an electromagnetic parameter chart of the iron-based wave-absorbing material prepared in example 3.
FIG. 12 is a reflection loss curve of the iron-based wave-absorbing material prepared in example 3.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
Example 1
The preparation operation steps of the Prussian blue redox derived iron-based wave-absorbing material are as follows:
(1): adding 15.2 g polyvinylpyrrolidone and 1.7 mL hydrochloric acid into 200 mL deionized water, stirring for dissolving, adding 0.44 g ferrous potassium chloride, stirring for 30 min, sealing the beaker, and adding 80oC, keeping the temperature of the oven for reaction for 24 hours; and filtering, washing and drying the product after reaction to obtain Prussian blue powder. The Prussian blue powder is blue powder, and the molecular formula is Fe4[Fe(CN)6]3The particles are cubic and have the particle size of 400-800 nm.
Referring to fig. 1, the prepared prussian blue powder particles had a distinct cubic morphology and a smooth surface with an average particle size of about 500 nm.
(2): mixing Prussian blue powder in air at a ratio of 2oThe temperature rise rate of C/min is increased to 350oC, preserving the heat for 6 hours, and naturally cooling to obtain ferric oxide (Fe)2O3) And (3) powder. The ferric oxide powder is dark red powder, the particles are in an irregular cube shape formed by assembling small particles, and the particle size is 200-800 nm.
Referring to FIG. 2, iron sesquioxide (Fe) was prepared2O3) The cubic shape of the powder particles is kept relatively complete, and a large number of small particles are arranged on the surface of the powder particles.
(3): 1 g of ferric oxide (Fe)2O3) Adding the powder into a mixed solution, uniformly mixing 80 mL of water, 32 mL of anhydrous ethanol and 0.4 mL of ammonia water to prepare the mixed solution, performing ultrasonic treatment to ensure uniform dispersion, adding 0.2 g of resorcinol, stirring for 1 h, adding 0.2 mL of formaldehyde solution with the concentration of 38 wt%, and performing polymerization reaction for 24 h; filtering, washing and drying the reaction product to obtain the ferric oxide (Fe) coated by the phenolic resin2O3) And (3) powder. The ferric oxide powder coated by the phenolic resin is brown powder, the particles are in an irregular cube shape, a small particle aggregation resin coating layer exists on the surface, the particles after being coated have an agglomeration phenomenon, and the particle size is 100-600 nm.
Referring to fig. 3, it can be seen that the SEM photograph of the iron-based wave absorbing material prepared in example 1 is irregular polyhedral particles with a particle size distribution of 10 to 300 nm.
(4): iron oxide (Fe) coated with phenolic resin2O3) Powder in nitrogen (N)2) Under the atmosphere with 5oC/min is increased to 700oAnd C, preserving the temperature for 2 h, and naturally cooling to obtain the Prussian blue redox-derived iron-based wave-absorbing material. The Prussian blue redox-derived iron-based wave-absorbing material is black gray powder and consists of iron-based magnetic particles, the particle size of the iron-based magnetic particles is 10-300 nm, and the iron-based wave-absorbing material comprises iron (Fe),Iron oxide (FeO) and ferroferric oxide (Fe)3O4) And carbon (C).
Referring to FIG. 4, the XRD spectrum of the iron-based absorbing material prepared in example 1 can be seen, wherein 35.4o、57.9o、62.5oIs ferroferric oxide (Fe)3O4) Characteristic diffraction peak of (1), 36.1o、41.9o、60.8oCharacteristic diffraction peak of iron oxide (FeO), 44.7o、65.1o、82.5oIs a characteristic diffraction peak of iron (Fe), and proves that the phenolic resin can realize ferric oxide (Fe) as a carbon source2O3) And the reduction product comprises multiple phases. Wherein the iron content is 25-89 wt%.
Referring to fig. 5, it can be seen that the electromagnetic parameter spectrum of the iron-based wave-absorbing material prepared in example 1 at a filling degree of 40 wt% is provided. It can be seen that the real part of the complex dielectric constant fluctuates around 6, and the imaginary part fluctuates around 1; the real part of the magnetic permeability is basically maintained at 1.1, and the imaginary part fluctuates around 0.1. The product has lower dielectric constant and magnetic permeability, because of Fe2O3Lower degree of reduction, resulting in lower complex permittivity and complex permeability of Fe3O4Occupies a large specific gravity.
Referring to fig. 6, the reflection loss curve of the iron-based wave-absorbing material prepared in example 1 can be seen. The effective wave-absorbing frequency band of the material is 2.8 GHz under the thickness of 2.8 mm. It can be known that the effective absorption frequency band is narrow and the required thickness is large because the magnetic conductivity of the material is too low, the magnetic loss is too weak, and the attenuation capability does not meet the wave-absorbing requirement.
Example 2
The preparation operation steps of the Prussian blue redox derived iron-based wave-absorbing material are as follows:
(1): adding 15.2 g polyvinylpyrrolidone and 1.7 mL hydrochloric acid into 200 mL deionized water, stirring for dissolving, adding 0.44 g ferrous potassium chloride, stirring for 30 min, sealing the beaker, and adding 80oC, keeping the temperature of the oven for reaction for 24 hours; and filtering, washing and drying the product after reaction to obtain Prussian blue powder. The Prussian blue powder is blue powder, and the molecular formula is Fe4[Fe(CN)6]3The particles are cubic and have a particle size of 400-800 nm.
(2): mixing Prussian blue powder in air at a ratio of 2oThe temperature rise rate of C/min is increased to 350oC, preserving the heat for 6 hours, and naturally cooling to obtain ferric oxide (Fe)2O3) And (3) powder. The ferric oxide powder is dark red powder, the particles are in an irregular cube shape formed by assembling small particles, and the particle size is 200-800 nm.
(3): 1 g of iron (Fe) oxide from step 22O3) Adding the powder into a mixed solution, uniformly mixing the mixed solution with 80 mL of water, 32 mL of anhydrous ethanol and 0.4 mL of ammonia water, performing ultrasonic treatment to ensure uniform dispersion, adding 0.6 g of resorcinol, stirring for 1 h, adding 1.2 mL of formaldehyde solution with the concentration of 38 wt%, and polymerizing for 24 h; filtering, washing and drying the reaction product to obtain the ferric oxide (Fe) coated by the phenolic resin2O3) And (3) powder. The ferric oxide powder coated by the phenolic resin is brown powder, the particles are in an irregular cube shape, a large-particle resin coating layer exists on the surface, the particles after coating have an agglomeration phenomenon, and the particle size is 100-600 nm.
(4): iron oxide (Fe) coated with phenolic resin2O3) Powder in nitrogen (N)2) Under the atmosphere with 5oC/min is increased to 700oAnd C, preserving the temperature for 2 h, and naturally cooling to obtain the Prussian blue redox-derived iron-based wave-absorbing material. The Prussian blue redox-derived iron-based wave-absorbing material is black gray powder and consists of iron-based magnetic particles, the particle size of the particles is 50-1000 nm, and the components comprise Fe and Fe3C、C。
Referring to FIG. 7, the XRD spectrum of the iron-based absorbing material prepared in example 2 can be seen, wherein 44.7o、65.0o、82.3oIs a characteristic diffraction peak of Fe, 26.6oIs the characteristic diffraction peak of C, and the rest is Fe3C, and no diffraction peak belonging to iron oxide. Illustrating Fe at this time2O3Has been completely reduced while Fe3The appearance of C and C peaks also indicates the excess of carbon source in the material, carbon element to carbonizeAnd the graphite phase carbon. Wherein the iron content is 50-87 wt%.
Referring to fig. 8, it can be seen that the electromagnetic parameter spectrum of the iron-based wave-absorbing material prepared in example 2 is shown. The real part of the complex permittivity at 2 GHz is about 20 and the imaginary part is about 17. The higher real part and imaginary part indicate that the sample has stronger dielectric storage and loss capacity, which may be due to Fe, C and Fe3The interface composition of the components such as C and the like and the existence of Fe simple substance with strong conductivity and graphite phase C. Meanwhile, the magnetic permeability of the sample under 2 GHz can reach 1.32, which is higher than that of most MOFs derived Fe-based wave-absorbing materials, and the method proves that the carbon content limiting strategy adopted by the process is favorable for improving the magnetic permeability of derived products.
Referring to fig. 9, it can be seen that the reflection loss curve of the iron-based wave-absorbing material prepared in example 2 has a relatively high magnetic permeability and a relatively high dielectric loss, the absorption frequency range is 9.32 to 18 GHz at a thickness of 1 to 5 mm, the effective absorption bandwidth of the material at a thickness of 1.5 mm can reach 5.44 GHz, and the coverage rate at Ku band is 90.7%, so that the iron-based wave-absorbing material shows relatively ideal wave-absorbing performance.
Example 3
(1): adding 15.2 g polyvinylpyrrolidone and 1.7 mL hydrochloric acid into 200 mL deionized water, stirring for dissolving, adding 0.44 g ferrous potassium chloride, stirring for 30 min, sealing the beaker, and adding 80oC, performing oven reaction for 24 hours; and filtering, washing and drying the product after reaction to obtain Prussian blue powder. The Prussian blue powder is blue powder, and the molecular formula is Fe4[Fe(CN)6]3The particles are cubic and have the particle size of 400-800 nm.
(2): mixing Prussian blue powder in air at a ratio of 2oThe temperature rise rate of C/min is increased to 350oC, preserving the heat for 6 hours, and naturally cooling to obtain ferric oxide (Fe)2O3) And (3) powder. The ferric oxide powder is dark red powder, the particles are in an irregular cube shape formed by assembling small particles, and the particle size is 200-800 nm.
(3): 1 g of the iron (Fe) trioxide obtained in step 22O3) The powder was added to a mixed solution of 80 mL of water, 32 mL of absolute ethanol and 0.4 mL of ammoniaUniformly mixing water, performing ultrasonic treatment to ensure uniform dispersion, adding 0.8 g of resorcinol, stirring for 1 h, adding 1.2 mL of formaldehyde solution with the concentration of 38 wt%, and polymerizing for 24 h; filtering, washing and drying the reaction product to obtain the ferric oxide (Fe) coated by the phenolic resin2O3) And (3) powder. The ferric oxide powder coated by the phenolic resin is brown powder, the particles are in an irregular cube shape, a large-particle resin coating layer exists on the surface, the particles after coating have an agglomeration phenomenon, and the particle size is 100-600 nm.
(4): iron oxide (Fe) coated with phenolic resin2O3) Powder in nitrogen (N)2) Under the atmosphere with 5oC/min is increased to 700oAnd C, preserving the temperature for 2 h, and naturally cooling to obtain the Prussian blue redox-derived iron-based wave-absorbing material. The Prussian blue redox derived iron-based wave-absorbing material is black gray powder and consists of iron-based magnetic particles, the particle size of the iron-based magnetic particles is 100-1800 nm, and the components comprise Fe and Fe3C、C。
Referring to FIG. 10, it can be seen that the XRD spectrum of the iron-based absorbing material prepared in example 3 is substantially the same as that of example 2, wherein Fe3The peak intensity of the C characteristic diffraction peak is increased, indicating that the crystallinity is enhanced, which is related to the increase of the carbon content. Wherein the iron content is 40-77 wt%.
Referring to fig. 11, it can be seen that the electromagnetic parameter spectrogram of the iron-based wave-absorbing material prepared in example 3 is that, as can be seen from the chart, the complex permittivity of the sample is high, wherein the real part of the complex permittivity is about 40, and the imaginary part is about 45, and the permeability is also reduced compared with that of example 1. The reason is that the residual non-magnetic graphite phase has too high a carbon content, resulting in an increase in the complex permittivity and a decrease in the complex permeability.
Referring to fig. 12, it can be seen that the reflection loss curve of the iron-based wave-absorbing material prepared in example 3 shows that, at a thickness of 1-5 mm, the sample does not have an effective wave-absorbing ability, because impedance matching is seriously unbalanced due to an excessively high dielectric constant.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included within the scope of the present invention.
Claims (2)
1. A Prussian blue redox-derived iron-based wave-absorbing material is characterized in that:
the iron-based wave-absorbing material is black gray powder and consists of iron-based magnetic particles, the particle size of the iron-based magnetic particles is 200-2000 nm, and the components of the iron-based wave-absorbing material comprise iron, ferric oxide, ferroferric oxide, carbon and iron carbide; wherein the iron content is 25-90 wt%;
the effective absorption bandwidth of the iron-based wave-absorbing material under the conditions that the filling degree is 40 wt% and the thickness is 1-5 mm is 0-5.44 GHz, and the maximum coverage rate of the iron-based wave-absorbing material in a Ku wave band is more than 90%.
2. The preparation method of the Prussian blue redox-derived iron-based wave-absorbing material disclosed by claim 1 is characterized by comprising the following operation steps of:
(1) dissolving required amount of potassium ferrocyanide, polyvinylpyrrolidone and hydrochloric acid in a proper amount of deionized water to obtain a mixed material, wherein Fe3+The concentration of the hydrochloric acid is 5-20 mmol/L, the adding volume of the hydrochloric acid is 1-3 mL, the concentration of the polyvinylpyrrolidone (K-30) in the solution is 1.67-3.33 mmol/L, and the volume of the deionized water is 150-300 mL; the mixed materials are subjected to heat preservation reaction for 1-24 hours in an oven at the temperature of 80 ℃, and are subjected to centrifugation, filtration, cleaning and drying to obtain Prussian blue powder; the Prussian blue powder is blue powder, and the molecular formula is Fe4[Fe(CN)6]3The particles are cubic and have the particle size of 200-2000 nm;
(2) carrying out high-temperature heat treatment on the Prussian blue powder in air, wherein the heating rate is 2-10 ℃/min, the heat preservation temperature is 300-500 ℃, and the heat preservation time is 3-9 h; naturally cooling to obtain ferric oxide powder; the ferric oxide powder is dark red powder, the granules of the ferric oxide powder are in an irregular cube shape formed by assembling small granules, and the grain diameter is 100-2000 nm;
(3) ultrasonically dispersing 1 g of ferric oxide powder in a mixed solution, wherein the volume of deionized water in the mixed solution is 60-100 mL, the volume of absolute ethyl alcohol is 20-40 mL, and the volume of ammonia water is 0.2-1 mL; adding 0.1-1 g of resorcinol, and uniformly mixing; adding 0.2-1.2 mL of formaldehyde solution with the concentration of 38 wt%, and polymerizing for 24 h; centrifuging, cleaning and drying to obtain ferric oxide powder coated with phenolic resin; the ferric oxide powder coated by the phenolic resin is brown powder, particles are irregular cubes, a resin coating layer exists on the surface of the particles, the particles have an agglomeration phenomenon, and the particle size is 10-2000 nm;
(4) and carrying out heat treatment on the iron sesquioxide powder coated by the phenolic resin in inert gas, wherein the heating rate of the heat treatment is 1-10 ℃/min, the temperature is 650-750 ℃, the heat preservation time is 1-4 h, and naturally cooling is carried out to obtain the iron-based wave absorbing material derived from iron prussian blue oxidation reduction.
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| CN114032067A (en) * | 2021-12-03 | 2022-02-11 | 中国海洋大学 | CoFe @ C/rGO electromagnetic wave absorption composite material and preparation method thereof |
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