CN112210345A - Method for improving performance of wave-absorbing material with spherical composite core-shell structure - Google Patents
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000011258 core-shell material Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 40
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 29
- 229920000767 polyaniline Polymers 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 22
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 22
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 22
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002114 nanocomposite Substances 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 238000000975 co-precipitation Methods 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000003980 solgel method Methods 0.000 claims abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
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- 238000003756 stirring Methods 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 10
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- 238000005406 washing Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
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- 239000002086 nanomaterial Substances 0.000 description 6
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 239000012043 crude product Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- 235000006408 oxalic acid Nutrition 0.000 description 2
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- 230000010287 polarization Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
Improved spherical alpha-Fe2O3@PANI/SiO2The method for combining the performance of the composite core-shell structure wave-absorbing material with the traditional ferrite alpha-Fe2O3Conductive polymer polyaniline and nano SiO2. During preparation, alpha-Fe is prepared by adopting various preparation methods2O3(coprecipitation method, hydrothermal method and solid phase method), and alpha-Fe is coated with polyaniline by adopting in-situ polymerization method2O3Nanoparticles to obtain alpha-Fe2O3The @ PANI nano composite wave-absorbing material with the core-shell structure. The nanometer SiO is prepared by a sol-gel method2Coated with alpha-Fe2O3Nanoparticles to obtain alpha-Fe2O3@SiO2A nano composite wave-absorbing material with a core-shell structure. alpha-Fe prepared by the invention2O3@PANI、α‑Fe2O3@SiO2NanocompositeThe core-shell structure wave-absorbing material can be used as an electromagnetic shielding material and a wave-absorbing stealth material.
Description
Technical Field
The invention relates to improved spherical alpha-Fe2O3@PANI/SiO2A method for compounding the property of wave-absorbing material with nuclear shell structure relates to electromagnetic shielding material and wave-absorbing stealth material.
Background
From the fact that electromagnetic waves are expected to be widely used, electromagnetic waves have penetrated into the surrounding of us. The system comprises household appliances, computers, mobile phones and information transmission and reception in the information era in daily life, and is used for defense and military attack.
With the rapid development of radar detection technology, the wave-absorbing stealth material becomes a research hotspot of military technology. A plurality of stealth technologies such as an anti-radar detection technology and an infrared stealth technology of electronic stealth are used for improving self defense capability. A new generation of stealth fighter autonomously researched and developed in China adopts a wave-absorbing material made of graphene. At present, the wave-absorbing material is not only used for military stealth defense, but also used for human body safety protection, electromagnetic compatibility or electromagnetic interference resistance. Electromagnetic wave pollution has become the fourth largest pollution.
With the development of science and technology, electromagnetic pollution is more serious, and electromagnetic radiation is greatly increased. The existing hot method for treating electromagnetic radiation is to absorb and lose electromagnetic waves or convert the electromagnetic energy, namely the principle of the wave-absorbing material in the invention.
The high-performance wave-absorbing material has good impedance matching, namely low reflectivity, and can convert electromagnetic waves into internal energy through electric loss and magnetic loss. With the development of the wave-absorbing material technology, a single wave-absorbing agent cannot meet the comprehensive requirements of absorption and interference of electromagnetic waves at present, and a composite wave-absorbing agent becomes a development trend. The absorbent with the core-shell structure has a special electronic structure and surface properties, and can have physicochemical properties of the two particles through effective compounding of the two particles at a micro-nano level, so that a synergistic effect is fully exerted, and a novel composite absorbent is obtained. In view of the whole, the wave-absorbing material should have strong wave-absorbing capability, thin thickness, wide absorption frequency band and small mass. Moreover, the requirements of high temperature resistance, corrosion resistance, low cost and the like also need to be met.
The ferrite is a traditional wave-absorbing material with double complex media, the wave-absorbing principle of the ferrite has two functions of magnetic loss and dielectric loss, the dielectric loss mainly is natural resonance in the aspect of magnetic loss through polarization effect, and the ferrite has good wave-absorbing performance. The ferrite wave-absorbing material has the advantages of high absorption frequency band, lower reflectivity, thin matching thickness and the like. Spherical alpha-Fe2O3The microstructure of the device is zero-dimensional, the reflection direction is not single, the electromagnetic wave can be better lost, and the reflected wave is reduced to be monitored by a radar. Fe2O3The iron oxide can not be oxidized again, so the iron oxide is stable, easy to obtain and low in cost.
Polyaniline (PANI) is a conductive polymer with conjugated pi electrons. The PANI can increase the interface area of the wave-absorbing material compounded with the PANI, enhance the interface polarization and adjust the magnetic conductivity and the dielectric constant of the material. The material can reach the maximum reflection loss.
Nano SiO2Has a low density and a certain dielectric constant. Mixing nano SiO2With alpha-Fe2O3The composite material can effectively reduce the density of the wave-absorbing material and improve the wave-absorbing performance.
Disclosure of Invention
Improved spherical alpha-Fe2O3@PANI/SiO2The method for combining the performance of the composite core-shell structure wave-absorbing material with the traditional ferrite alpha-Fe2O3Conductive polymer polyaniline and nano SiO2. During preparation, alpha-Fe is prepared by adopting various preparation methods2O3(coprecipitation method, hydrothermal method and solid phase method), and alpha-Fe is coated with polyaniline by adopting in-situ polymerization method2O3Nanoparticles to obtain alpha-Fe2O3The @ PANI nano composite wave-absorbing material with the core-shell structure. The nanometer SiO is prepared by a sol-gel method2Coated with alpha-Fe2O3Nanoparticles to obtain alpha-Fe2O3@SiO2A nano composite wave-absorbing material with a core-shell structure. alpha-Fe prepared by the invention2O3@PANI、α-Fe2O3@SiO2The nano composite wave-absorbing material with the core-shell structure can be used as an electromagnetic shielding material and a wave-absorbing stealth material.
The preparation method comprises the following steps:
(1) coprecipitation method for preparing alpha-Fe2O3Nano material
120mL of 1mol/L FeCl is taken3·6H2O and beaker, 5mL citric acid (0.1mol/L) is added, and concentrated NH is added under stirring at a proper rotation speed3·H2O, stop until pH 9 and continue stirring for 10 min. Filtration, washing the product well to pH 7 and no Cl in the filtrate-. Drying the precipitateDrying, grinding, placing into a sintering furnace, heating to 350 deg.C at 1 deg.C/min from room temperature, holding for 20min, stopping heating, and naturally cooling to room temperature.
(2) Hydrothermal method for preparing alpha-Fe2O3Nano material
Weighing 4.04g Fe (NO)3)3·9H2O, 1.375g oxalic acid and 35mL deionized water, fully stirring for 30min, pouring the solution into a 50mL reaction kettle with a polytetrafluoroethylene inner container, and reacting for 10h at the high temperature of 180 ℃. After the high-temperature hydrothermal reaction, centrifuging, and washing twice with deionized water and absolute ethyl alcohol respectively. Drying the precipitate, grinding, placing into a muffle furnace, heating to 600 deg.C, maintaining for 30min, stopping heating, and naturally cooling to room temperature.
(3) Preparation of alpha-Fe by solid phase method2O3Nano material
Taking 0.06mol of Fe (NO)3)3·9H2O and 0.18mol NaOH are mixed in a mortar and fully ground for 30 min. The solid phase product was washed three times with distilled water and alcohol, respectively. Naturally drying to obtain a crude product. Grinding the crude product, placing into a muffle furnace, heating to 600 deg.C, maintaining for 30min, stopping heating, and naturally cooling to room temperature.
(4) In-situ polymerization method for preparing alpha-Fe2O3@ PANI composite wave-absorbing material
alpha-Fe with good crystal appearance and better wave-absorbing performance2O30.8g of precursor is added with 50mL of deionized water, then 5mL of 2mol/L HC1 solution is added, and ultrasonic dispersion is carried out for 1h to obtain suspension. Adding 2mL of aniline into the suspension, magnetically stirring for 1h, adding the prepared APS solution, and stirring for 12h to obtain a precipitate. And finally, repeatedly washing the mixture by using deionized water and absolute ethyl alcohol, and drying the mixture for 4 hours at the temperature of 60 ℃.
(5) Sol-gel process for preparing alpha-Fe2O3@SiO2Composite wave-absorbing material
Taking the raw materials of Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and 0.1mol/L HC1 solution, namely 1:12:10:0.1, firstly dripping half of the absolute ethyl alcohol into the TEOS, then dripping HC1 solution and the other half of the absolute ethyl alcohol, and stirring L h. alpha-Fe with good crystal appearance and better wave-absorbing performance2O3And adding 0.8g of precursor into the mixed solution under stirring, continuously stirring for 24h, finally washing the product with absolute ethyl alcohol for 3 times, and drying for 10 h.
The invention has the beneficial effects that: combined with conventional ferrite alpha-Fe2O3Conductive polymer polyaniline and nano SiO2Firstly, alpha-Fe is prepared by adopting various preparation methods2O3(coprecipitation method, hydrothermal method and solid phase method), and alpha-Fe is coated with polyaniline by adopting in-situ polymerization method2O3Nanoparticles to obtain alpha-Fe2O3The @ PANI nano composite wave-absorbing material with the core-shell structure. The nanometer SiO is prepared by a sol-gel method2Coated with alpha-Fe2O3Nanoparticles to obtain alpha-Fe2O3@SiO2A nano composite wave-absorbing material with a core-shell structure. alpha-Fe prepared by the invention2O3@PANI、α-Fe2O3@SiO2The nano composite wave-absorbing material with the core-shell structure can be used as an electromagnetic shielding material and a wave-absorbing stealth material.
Detailed Description
The present invention is further illustrated below, but the scope of the invention is not limited to the disclosure.
In the following description, for purposes of clarity, not all features of an actual implementation are described, well-known functions or constructions are not described in detail since they would obscure the invention with unnecessary detail, it being understood that in the development of any actual embodiment, numerous implementation details must be set forth in order to achieve the developer's specific goals, such as compliance with system-related and business-related constraints, changing from one implementation to another, and it being recognized that such development effort might be complex and time consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art.
Example 1: preparation of alpha-Fe2O3Precursor body
The method comprises the following steps: coprecipitation method for preparing alpha-Fe2O3Nano material
(1) 120mL of 1mol/L FeCl is taken3·6H2O in a beaker, adding 5mL of 0.1mol/L citric acid, and rotating properlyAdding concentrated NH under rapid stirring3·H2O, stop until pH 9 and continue stirring for 10 min. Filtration, washing the product well to pH 7 and no Cl in the filtrate-. Drying the precipitate, grinding, placing into a sintering furnace, heating to 350 deg.C at 1 deg.C/min from room temperature, maintaining for 20min, stopping heating, and naturally cooling to room temperature.
(2) Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD) are adopted to treat alpha-Fe2O3And (5) performing characterization on the precursor. For alpha-Fe by vector network instrument2O3And (5) testing the wave absorbing performance of the precursor.
Step two: hydrothermal method for preparing alpha-Fe2O3Nano material
(1) Weighing 4.04g Fe (NO)3)3·9H2O, 1.375g oxalic acid and 35mL deionized water, fully stirring for 30min, pouring the solution into a 50mL reaction kettle with a polytetrafluoroethylene inner container, and reacting for 10h at the high temperature of 180 ℃. After the high-temperature hydrothermal reaction, centrifuging, and washing twice with deionized water and absolute ethyl alcohol respectively. Drying the precipitate, grinding, placing into a muffle furnace, heating to 600 deg.C, maintaining for 30min, stopping heating, and naturally cooling to room temperature.
(2) Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD) are adopted to treat alpha-Fe2O3And (5) performing characterization on the precursor. For alpha-Fe by vector network instrument2O3And (5) testing the wave absorbing performance of the precursor.
Step three: preparation of alpha-Fe by solid phase method2O3Nano material
(1) Taking 0.06mol of Fe (NO)3)3·9H2O and 0.18mol NaOH are mixed in a mortar and fully ground for 30 min. The solid phase product was washed three times with distilled water and alcohol, respectively. Naturally drying to obtain a crude product. Grinding the crude product, placing into a muffle furnace, heating to 600 deg.C, maintaining for 30min, stopping heating, and naturally cooling to room temperature.
(2) Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD) are adopted to treat alpha-Fe2O3And (5) performing characterization on the precursor. For alpha-Fe by vector network instrument2O3Precursor is subjected toAnd (5) testing the wave absorbing performance.
Example 2: in-situ polymerization method for preparing alpha-Fe2O3@ PANI composite wave-absorbing material
The method comprises the following steps: alpha-Fe with good crystal appearance and better wave-absorbing performance2O30.8g of precursor is added with 50mL of deionized water, then 5mL of 2mol/L HC1 solution is added, and ultrasonic dispersion is carried out for 1h to obtain suspension. Adding 2mL of aniline into the suspension, magnetically stirring for 1h, adding the prepared APS solution, and stirring for 12h to obtain a precipitate. And finally, repeatedly washing the mixture by using deionized water and absolute ethyl alcohol, and drying the mixture for 4 hours at the temperature of 60 ℃.
Step two: scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD) are adopted to treat alpha-Fe2O3@ PANI. For alpha-Fe by vector network instrument2O3And @ PANI is used for testing the wave absorbing performance.
Example 3: sol-gel process for preparing alpha-Fe2O3@SiO2Composite wave-absorbing material
The method comprises the following steps: taking the raw materials according to the proportion that TEOS, absolute ethyl alcohol, deionized water and 0.1mol/L HC1 solution are 1:12:10:0.1, firstly, dropwise adding half of absolute ethyl alcohol into TEOS, then dropwise adding HC1 solution and the other half of absolute ethyl alcohol, and stirring L h. alpha-Fe with good crystal appearance and better wave-absorbing performance2O3And adding 0.8g of precursor into the mixed solution under stirring, continuously stirring for 24h, finally washing the product with absolute ethyl alcohol for 3 times, and drying for 10 h.
Step two: scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD) are adopted to treat alpha-Fe2O3@SiO2And (6) performing characterization. For alpha-Fe by vector network instrument2O3@SiO2And (5) carrying out wave-absorbing performance test.
Although the invention has been described and illustrated in some detail, it should be understood that various modifications may be made to the described embodiments or equivalents may be substituted, as will be apparent to those skilled in the art, without departing from the spirit of the invention.
Claims (3)
1. A method for improving the performance of a wave-absorbing material with a spherical composite core-shell structure is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing alpha-Fe by respectively adopting a coprecipitation method, a hydrothermal method and a solid-phase method2O3A precursor;
step two, coating alpha-Fe with polyaniline by adopting in-situ polymerization method2O3Nanoparticles to obtain alpha-Fe2O3The @ PANI nano composite core-shell structure wave-absorbing material;
thirdly, adopting a sol-gel method to prepare the nano SiO2Coated with alpha-Fe2O3Nanoparticles to obtain alpha-Fe2O3@SiO2A nano composite wave-absorbing material with a core-shell structure.
2. Spherical alpha-Fe2O3@PANI/SiO2The composite wave-absorbing material with the core-shell structure is applied to electromagnetic shielding materials and wave-absorbing stealth materials.
3.α-Fe2O3@PANI、α-Fe2O3@SiO2The nano composite wave-absorbing material with the core-shell structure is applied to electromagnetic shielding materials and wave-absorbing stealth materials.
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| CN113423256A (en) * | 2021-07-15 | 2021-09-21 | 华东理工大学 | Composite wave-absorbing material and preparation method and application thereof |
| CN113490403A (en) * | 2021-05-12 | 2021-10-08 | 南昌航空大学 | Preparation method of alpha-Fe 2O3 doped silica nanoparticle wave-absorbing material |
| CN113980464A (en) * | 2021-11-23 | 2022-01-28 | 深圳市北测检测技术有限公司 | Based on Fe4Preparation of Fe from N4Method for N @ PANI nano composite wave-absorbing material |
| CN114276781A (en) * | 2021-12-07 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | MO @ NC core-shell structure type nano wave-absorbing material and preparation method thereof |
| CN115746787A (en) * | 2022-11-23 | 2023-03-07 | 中南大学 | Composite wave-absorbing material, preparation method and application |
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| CN113490403A (en) * | 2021-05-12 | 2021-10-08 | 南昌航空大学 | Preparation method of alpha-Fe 2O3 doped silica nanoparticle wave-absorbing material |
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