CN108483508B - Porous flaky Fe3O4Electromagnetic wave absorbing agent and preparation method thereof - Google Patents

Porous flaky Fe3O4Electromagnetic wave absorbing agent and preparation method thereof Download PDF

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CN108483508B
CN108483508B CN201810382761.6A CN201810382761A CN108483508B CN 108483508 B CN108483508 B CN 108483508B CN 201810382761 A CN201810382761 A CN 201810382761A CN 108483508 B CN108483508 B CN 108483508B
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electromagnetic wave
wave absorbing
absorbing agent
porous flaky
porous
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CN108483508A (en
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姬广斌
赵唤琴
成岩
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Changzhou Weisi Shuanglian Technology Co ltd
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Nanjing University of Aeronautics and Astronautics
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide (Fe3O4)
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution

Abstract

The invention discloses porous flaky Fe3O4Electromagnetic wave absorber, said Fe3O4The electromagnetic wave absorbing agent is of a sheet structure, and each sheet structure is provided with a plurality of hole structures. The invention also discloses the porous flaky Fe3O4A method for preparing an electromagnetic wave absorber. Porous flaky Fe of the invention3O4The electromagnetic wave absorbing agent still has the characteristics of high absorption strength and wide effective absorption frequency band under low thickness, and the excellent wave absorbing performance is mainly concentrated in X and C wave bands; the preparation method has simple process and low cost, does not need complex synthesis equipment, and can realize large-scale and large-batch production.

Description

Porous flaky Fe3O4Electromagnetic wave absorbing agent and preparation method thereof
Technical Field
The invention relates to porous flaky Fe3O4Electromagnetic wave absorber and the porous sheet Fe3O4A preparation method of an electromagnetic wave absorbing agent belongs to the technical field of wave absorbing materials.
Background
In recent years, the rapidly developed high-frequency wireless communication equipment brings great convenience to daily life and scientific research of people. Meanwhile, electromagnetic wave radiation causes great interference to the living environment, human health, and normal operation of electronic equipment. In addition, in the military field, the stealth technology can improve the viability of a target equipment system in actual operation and is closely connected with national defense strength of the country. Therefore, the electromagnetic wave absorbing material has been widely regarded and studied in both civil and military fields. At present, wave-absorbing materials are mainly classified into dielectric loss and magnetic loss wave absorbers according to loss mechanisms. Among them, the magnetic loss absorber occupies a very important position in the field of electromagnetic wave absorption by virtue of good impedance matching and magnetic loss capability.
Magnetite Fe3O4As a traditional ferromagnetic material, it has been widely used in the field of wave absorption because of its low cost, low toxicity and good biocompatibility. For example, the co-precipitation method is used for the co-precipitation of Fe in the professor Cao flourishing university of Beijing Phytolian3O4The nanoparticles are deposited on carbon nanotubes (MWCNTs) to obtain Fe3O4The effective electromagnetic wave absorption bandwidth of the MWCNTs composite material can reach 11GHz (7-18GHz) at 3 mm. (M.S.Cao, J.Yang, W.L)Song, d.q.zhang, b.wen, h.b.jin, z.l.hou, j.yuan, ferro Oxide/Multiwalled Carbon Nanotube vs polyanaline/ferro Oxide/Multiwalled Carbon Nanotube multinuclear absorption, acs appl.mater.interface 2012,4, 6949-. Professor Doudhei university of Harbin industry, university of Duchen, by2Calcination of Fe in an atmosphere3O4And phenolic resin complex to obtain Fe3O4The effective absorption bandwidth of the @ C microsphere can reach 4.0 (12.9-17.8) GHz under the thickness of 1.5 mm. (Y.C.Du, W.W.Liu, R.Qiang, Y.Wang, X.J.Han, J.Ma, P.xu.Shell thickness-dependent microwaveorientation of core-shell Fe3O4@ C compositions. ACS appl.Mater. interfaces 2014,6, 12997-one 13006.). However, Fe in the prior art3O4The wave absorber still has the defects of 1.Fe3O4The performance of the wave absorbing agent is mainly concentrated on a Ku (12-18GHz) wave band, and the radio communication and radar frequency ranges are mostly concentrated on X (8-12) and C (4-8) wave bands; 2. the preparation process is complex, the time consumption is long, the yield is low, and the cost is high; 3. at present Fe3O4The wave absorbing agent is mainly a binary composite material, the performance research of a single-component material needs to be further deepened, and the relation between a microstructure and electromagnetic parameters is still fuzzy.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing porous flaky Fe3O4The electromagnetic wave absorber has a low density and good dielectric property due to the sheet-shaped porous structure.
The technical problem to be solved by the invention is to provide the porous flaky Fe3O4Preparation method of electromagnetic wave absorber, and Fe in sheet structure can be prepared by the preparation method3O4The electromagnetic wave absorbing agent has simple preparation process and low cost, and can be suitable for industrial large-scale production.
In order to solve the technical problems, the technical means adopted by the invention is as follows:
porous flaky Fe3O4Electromagnetic wave absorber, said Fe3O4The electromagnetic wave absorbing agent is of a sheet structure, and each sheet structure is provided with a plurality of hole structures.
Wherein, the diameter of each sheet structure is 4.7-6.0 μm, and the thickness is 0.59-0.7 μm.
Wherein the aperture of each pore structure is 10-110 nm.
The above porous flaky Fe3O4The preparation method of the electromagnetic wave absorbing agent specifically comprises the following steps:
step 1, preparing α -Fe by solvothermal method2O3Dissolving a required amount of ferric acetylacetonate in a triethylene glycol solvent, adding a proper amount of NaOH solution into the mixed solution after complete dissolution to obtain a mixed material, placing the mixed material in a sealed reaction container, preserving the temperature for 4 hours at 200-220 ℃ to obtain a primary product, centrifugally washing and drying the primary product to obtain a precursor α -Fe2O3；
Step 2, the precursor α -Fe obtained in the step 12O3Dispersed in NaBH containing reducing agent4The mixture is placed in a sealed reaction container for heat preservation for 12 hours at 160-170 ℃ after being completely mixed to obtain an initial product, and the initial product is subjected to magnetic decantation separation after reaction to obtain porous flaky Fe3O4An electromagnetic wave absorber.
In the step 1, the volume of the triethylene glycol solvent is 40-60 mL, the addition amount of the ferric acetylacetonate is 0.6g, and the addition volume of the NaOH solution is 2-20 mL.
Wherein the concentration of the NaOH solution is 6 mol/L.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
porous flaky Fe of the invention3O4Compared with the traditional Fe, the electromagnetic wave absorber3O4Wave absorbing material and Fe3O4The base composite material has the characteristics of high absorption strength under low thickness and wide effective absorption frequency band, and the excellent wave absorption performance is mainly concentrated in X and C wave bands; the preparation method has simple process and low cost, does not need complex synthesis equipment, and can realize large-scale productionAnd (4) mass production.
Drawings
FIG. 1 shows Fe obtained in examples 1, 2 and 3 of the present invention3O4An X-ray diffraction pattern of the electromagnetic wave absorber;
FIG. 2 shows Fe obtained in example 1 of the present invention3O4-2 SEM photograph;
FIG. 3 shows Fe obtained in example 2 of the present invention3O4SEM photograph of-10;
FIG. 4 shows Fe obtained in example 3 of the present invention3O4SEM photograph of-20;
FIG. 5 shows Fe obtained in example 1 of the present invention3O4-2 reflection loss spectrum;
FIG. 6 shows Fe obtained in example 2 of the present invention3O4-a reflection loss map of 10;
FIG. 7 shows Fe obtained in example 3 of the present invention3O4-a reflection loss map of 20;
FIG. 8 shows Fe obtained in example 2 of the present invention3O4-10 map of effective absorption bandwidth.
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
Porous flaky Fe of the invention3O4The electromagnetic wave absorbing agent is in a sheet structure, each sheet structure is provided with a plurality of hole structures, and the electromagnetic wave absorbing agent is prepared into α -Fe by using a solvothermal method2O3Reuse of NaBH4Reduction method for preparing porous flaky Fe3O4An electromagnetic wave absorber.
Example 1
Porous flaky Fe of the invention3O4The preparation method of the electromagnetic wave absorbing agent comprises the following steps:
step 1, preparing α -Fe by solvothermal method2O3: adding 0.6g of ferric acetylacetonate into 60mL of triethylene glycol solvent, completely dissolving, adding 2mL of 6mol/L NaOH solution (providing an alkaline environment) into the mixed solution, and continuously stirring for 1h to obtain a mixed material; will be provided withSealing the mixture in a reaction kettle, keeping the temperature at 200 deg.C for 4h to obtain a primary product, centrifuging, washing, and drying to obtain precursor α -Fe2O3Marked α -Fe2O3-2. obtaining a precursor α -Fe2O3-2 is also a porous sheet-like structure, except that the sheet-like structure is relatively thin;
step 2, 0.1g of precursor α -Fe obtained in step 12O3Dispersing in 30mL of distilled water, and adding 10mmol of NaBH into the distilled water4Ultrasonic treating for 15min, sealing the mixture in a reaction kettle, keeping the temperature at 160 deg.C for 12 hr, and naturally cooling to obtain final product labeled as Fe3O42, due to precursor α -Fe2O3The-2 sheet structure is relatively thin, so that the precursor sheet structure is destroyed after reduction to become granular.
Example 2
Porous flaky Fe of the invention3O4The preparation method of the electromagnetic wave absorbing agent comprises the following steps:
step 1, preparing α -Fe by solvothermal method2O3Adding 0.6g of ferric acetylacetonate into 50mL of triethylene glycol solvent, dissolving completely, adding 10mL of 6mol/L NaOH solution into the mixed solution, continuously stirring for 1h to obtain a mixed material, sealing the mixed material in a reaction kettle, preserving the temperature for 4h at 200 ℃ to obtain a primary product, centrifugally washing and drying the primary product to obtain a precursor α -Fe2O3Marked α -Fe2O3-10, precursor α -Fe obtained2 O 310 is also in the form of a porous sheet structure, with a moderate thickness;
step 2, 0.1g of precursor α -Fe obtained in step 12O3Dispersing in 30mL of distilled water, and adding 10mmol NaBH into the distilled water4Ultrasonic treating for 15min, sealing the mixture in a reaction kettle, keeping the temperature at 160 deg.C for 12 hr, and naturally cooling to obtain final product labeled as Fe3O410, due to precursor α -Fe2O3-10 sheets thick, hence precursorThe sheet-like structure is still porous after reduction.
Example 3
Porous flaky Fe of the invention3O4The preparation method of the electromagnetic wave absorbing agent comprises the following steps:
step 1, preparing α -Fe by solvothermal method2O3Adding 0.6g of ferric acetylacetonate into 40mL of triethylene glycol solvent, dissolving completely, adding 20mL of 6mol/L NaOH solution into the mixed solution, continuously stirring for 1h to obtain a mixed material, sealing the mixed material in a reaction kettle, preserving the temperature for 4h at 200 ℃ to obtain a primary product, centrifugally washing and drying the primary product to obtain a precursor α -Fe2O3Marked α -Fe2O3-20；
Step 2, 0.1g of precursor α -Fe obtained in step 12O3Dispersing in 30mL of distilled water, and adding 10mmol NaBH into the distilled water4Ultrasonic treating for 15min, sealing the mixture in a reaction kettle, keeping the temperature at 160 deg.C for 12 hr, and naturally cooling to obtain final product labeled as Fe3O4-10。
FIG. 1 shows Fe obtained in examples 1, 2 and 3 of the present invention3O4The X-ray diffraction pattern of the electromagnetic absorber, as can be seen from FIG. 1, is only Fe3O4The final product composition is Fe according to the combination of the characteristic peak and the experimental principle3O4。
FIG. 2 shows Fe obtained in example 1 of the present invention3O4SEM photograph of-2, it can be seen from fig. 2 that the precursor sheet structure is substantially destroyed and a number of irregular particles are formed.
FIG. 3 shows Fe obtained in example 2 of the present invention3O4SEM photograph of-10, as can be seen from FIG. 3, Fe at a higher NaOH content3O4A porous sheet-like structure was formed, which had a diameter of about 4.70 μm and a thickness of about 0.59. mu.m.
FIG. 4 shows Fe obtained in example 3 of the present invention3O4SEM photograph of-20, flakes with further increase in NaOH contentThe diameter increase of the structure was 6.0 μm and the thickness increase was 0.7 μm, indicating that an increase in NaOH content favors Fe3O4And (4) growing a sheet structure.
FIG. 5 shows Fe obtained in example 1 of the present invention3O4Reflection loss spectrum of-2, as can be seen from FIG. 5, Fe obtained in example 13O4The wave absorbing material-2 has poor wave absorbing performance, and the frequency bandwidth with the optimal reflection loss value less than-14 dB and less than-10 dB is only 2.3 GHz.
FIG. 6 shows Fe obtained in example 2 of the present invention3O4Reflection loss spectrum of-10, as can be seen from FIG. 6, Fe obtained in example 23O4The-10 wave-absorbing material shows excellent wave-absorbing performance. Under the condition of 2.05 mm thickness, the reflection loss value can reach-49.0 dB; under the condition of 2.25 mm of thickness, the bandwidth less than-10 dB is 4.32 (7.52-11.84) GHz. Thus, the generation of the porous sheet structure is beneficial to improving the electromagnetic wave absorption performance of the material.
FIG. 7 shows Fe obtained in example 3 of the present invention3O4Reflection loss spectrum of-20, as can be seen from FIG. 7, the wave absorbing property of the product is between that of Fe3O4-2 and Fe3O4-10. The reflection loss value is up to-27 dB and the frequency bandwidth which is less than-10 dB is 3.0GHz under the condition of 1.85 mm thickness.
FIG. 8 shows Fe obtained in example 2 of the present invention3O4The diagram of the effective absorption bandwidth of-10, it can be seen from FIG. 8 that the effective absorption bandwidth (RL ≦ 10dB) covers almost the entire C-band and X-band when the coating thickness is between 2.05 and 3.05 mm. At present, conventional granular Fe3O4The electromagnetic wave absorbing agent has wave absorbing performance incapable of meeting the requirement of reaching relatively wide effective absorbing frequency band (not less than 4GHz) in low thickness (not more than 3mm) in low frequency band. Therefore, Fe of the flaky porous structure of the present invention3O4The electromagnetic wave absorbing agent can be used as an excellent low-frequency electromagnetic wave absorbing material. In addition, granular Fe in the prior art3O4The electromagnetic wave absorbing agent not only has wave absorbing performance inferior to that of the porous flaky Fe3O4Electromagnetic wave absorber, and other carbon fiber impurities contained therein, and the inventionPorous flaky Fe3O4The electromagnetic wave absorber only has Fe with a sheet structure3O4。
Porous flaky Fe of the invention3O4Firstly adopting a one-step solvothermal method to synthesize α -Fe by using an electromagnetic wave absorbing agent2O3Precursor and then NaBH as reducer4Under the action of (1), precursor α -Fe2O3Reduction to Fe having a porous sheet structure3O4. The synthesized porous sheet structure is beneficial to improving the dielectric property of the material, enhancing the impedance matching characteristic and the interface polarization loss of the material, and simultaneously, the existence of the porous structure is beneficial to reducing the density of the wave absorbing agent.

Claims (6)

1. Porous flaky Fe3O4The electromagnetic wave absorbing agent is characterized in that: said Fe3O4The electromagnetic wave absorbing agent is of a sheet structure, and each sheet structure is provided with a plurality of hole structures;
wherein the porous flaky Fe3O4The electromagnetic wave absorbing agent is prepared by the following method, and the specific steps are as follows:
step 1, preparing α -Fe by solvothermal method2O3Dissolving a required amount of ferric acetylacetonate in a triethylene glycol solvent, adding a proper amount of NaOH solution into the mixed solution after complete dissolution to obtain a mixed material, placing the mixed material in a sealed reaction container, preserving the temperature for a certain time at 200-220 ℃ to obtain a primary product, centrifugally washing and drying the primary product to obtain a precursor α -Fe2O3(ii) a The volume of the triethylene glycol solvent is 40-60 mL, the addition amount of ferric acetylacetonate is 0.6g, and the addition volume of the NaOH solution is 2-20 mL;
step 2, the precursor α -Fe obtained in the step 12O3Dispersed in NaBH containing reducing agent4The mixture is placed in a sealed reaction container for heat preservation for a certain time at 160-170 ℃ after being completely mixed to obtain an initial product, and the initial product obtained after the reaction is subjected to magnetic decantation separation to obtain porous flaky Fe3O4An electromagnetic wave absorber.
2. Porous flaky Fe according to claim 13O4The electromagnetic wave absorbing agent is characterized in that: each sheet-like structure has a diameter of 4.7 to 6.0 μm and a thickness of 0.59 to 0.7 μm.
3. Porous flaky Fe according to claim 13O4The electromagnetic wave absorbing agent is characterized in that: the pore diameter of the pore structure is 10-110 nm.
4. Porous flaky Fe according to claim 13O4The electromagnetic wave absorbing agent is characterized in that: the concentration of the NaOH solution is 6 mol/L.
5. Porous flaky Fe according to claim 13O4The electromagnetic wave absorbing agent is characterized in that: in the step 1, the heat preservation time is 4 hours.
6. Porous flaky Fe according to claim 13O4The electromagnetic wave absorbing agent is characterized in that: in the step 2, the heat preservation time is 12 hours.
CN201810382761.6A 2018-04-25 2018-04-25 Porous flaky Fe3O4Electromagnetic wave absorbing agent and preparation method thereof Active CN108483508B (en)

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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102001712A (en) * 2010-12-16 2011-04-06 苏州康立达纳米生物工程有限公司 Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template
CN103723773A (en) * 2012-10-16 2014-04-16 国家纳米科学中心 Hydrosol of ferroferric oxide nanoparticles and preparation method and application thereof

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102001712A (en) * 2010-12-16 2011-04-06 苏州康立达纳米生物工程有限公司 Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template
CN103723773A (en) * 2012-10-16 2014-04-16 国家纳米科学中心 Hydrosol of ferroferric oxide nanoparticles and preparation method and application thereof

Non-Patent Citations (1)

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Title
"Precipitation synthesis of magnetite Fe3O4 nanoflakes";Andris Šutka et al.;《Ceramics International》;20140402;第40卷;第11438页左栏第4段至第11439页左栏倒数第1段，图3 *

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