CN109574707B - Microporous magnetic medium composite ceramic wave-absorbing metamaterial and preparation method thereof - Google Patents
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Abstract
The invention discloses a microporous magnetic medium composite ceramic wave-absorbing metamaterial and a preparation method thereof, and relates to the technical field of electromagnetic functional materials, wherein the microporous magnetic medium composite ceramic metamaterial comprises periodic array microporous ceramics and nano magnetic ferrites, the holes of the periodic array microporous ceramics are square holes, the nano magnetic ferrites are embedded in the holes of the periodic array microporous ceramics, the aperture of the periodic array microporous ceramics is 0.4-1000 mu m, and the thickness of the periodic array microporous ceramics is 0.8-3.5 mm; the micropore magnetic medium composite ceramic metamaterial realizes intrinsic negative electromagnetic parameters of the material by utilizing the synergy of the dielectric loss of the periodical array micropore ceramic and the magnetic loss of the nanometer magnetic ferrite, and has the advantages of simple structure, mature preparation process, easily obtained raw materials, low cost and easy large-scale production and application.
Description
Technical Field
The invention belongs to the technical field of electromagnetic functional materials, and particularly relates to a microporous magnetic medium composite ceramic wave-absorbing metamaterial and a preparation method thereof.
Background
Electromagnetic wave absorbing materials refer to materials that absorb or substantially attenuate electromagnetic wave energy incident upon their surface and convert the energy into heat energy, thereby reducing electromagnetic wave interference. To achieve good wave absorption, the incident electromagnetic waves need to enter the wave absorbing material as much as possible without being reflected, and the wave absorbing material needs to absorb the loss of the electromagnetic waves. In engineering application, the wave-absorbing material is required to have high absorption rate to electromagnetic waves in a wider frequency band, and also required to have the properties of light weight, temperature resistance, moisture resistance, corrosion resistance and the like. With the continuous improvement and improvement of the preparation level and the microstructure characterization capability of the material, the improvement difficulty of the wave absorption performance of the traditional material is more and more increased, and the metamaterial appearing in recent years is rapidly developed due to the unusual electromagnetic response characteristic.
The electromagnetic metamaterial is a composite structure formed by artificial sub-wavelength structural units, can realize supernormal electromagnetic characteristics, and has important application value in the field of electromagnetic wave absorption. However, with the continuous expansion of the frequency range of the stealth technology, most of the metamaterials of the artificial structure are broadband wave-absorbing metamaterials obtained by overlapping or changing the size, the shape and the like of a multilayer structure at present, but the method has the disadvantages of complex preparation process, difficult processing, poor performance adjustability and relatively narrow bandwidth. Therefore, the broadband wave-absorbing metamaterial with simple structure, convenient preparation and low cost is one of the research focuses in the related fields.
Disclosure of Invention
The invention provides a microporous magnetic medium composite ceramic wave-absorbing metamaterial and a preparation method thereof, solves the problems and is realized by the following technical scheme.
One of the purposes of the invention is to provide a microporous magnetic medium composite ceramic wave-absorbing metamaterial, which comprises periodic array microporous ceramic and nano magnetic ferrite, wherein the holes of the periodic array microporous ceramic are square holes, and the nano magnetic ferrite is embedded in the holes of the periodic array microporous ceramic;
the aperture of the periodic array microporous ceramic is 0.4-1000 mu m, the thickness of the periodic array microporous ceramic is 0.8-3.5 mm, and the embedding depth of the nano magnetic ferrite is 0.5-2 mm.
Preferably, the periodic array microporous ceramic is an alumina microporous ceramic.
Preferably, the alumina microporous ceramic has a relative dielectric constant of 9 to 12.5 and a dielectric loss tangent of 0 to 0.5.
Preferably, the nano magnetic ferrite is Co Fe2O4、Ni Fe2O4Either one or both.
The invention also provides a preparation method of the microporous magnetic medium composite ceramic wave-absorbing metamaterial, which comprises the following steps:
s1: carrying out in-situ synthesis pretreatment on the periodic array microporous ceramic through coarsening, sensitizing, cleaning and drying processes;
the roughening process is to immerse the periodic array microporous ceramic into roughening liquid, wherein the periodic array microporous ceramic comprises the following steps: roughening solution 1 g: 2-5 mL, performing ultrasonic treatment for 30min at room temperature, and washing with deionized water for 2-3 times;
the sensitization process is that the periodic array microporous ceramic is immersed into the sensitization liquid, and the periodic array microporous ceramic: sensitizing solution is 1 g: 2-5 mL, performing ultrasonic treatment for 30min at room temperature, and washing with deionized water for 2-3 times;
s2: fixing the pretreated periodic array microporous ceramic in a lining of a 1000mL hydrothermal reaction kettle, pouring in-situ synthetic liquid into the lining of the hydrothermal reaction kettle, and preparing a periodic array microporous ceramic: 1g of in-situ synthesis solution: 10-15 mL, and adjusting the pH of the in-situ mixed solution to 8.0-11.0 by using sodium hydroxide; ultrasonically vibrating for 30min, covering the reaction kettle, placing the reaction kettle in an oven, keeping the temperature at 149.5-150.5 ℃, and reacting for 6-10 h;
s3: and taking out the cooled periodic array microporous ceramic after the reaction of S2, washing the surface with water, and performing vacuum drying at 70 ℃ to obtain the microporous magnetic medium composite ceramic wave-absorbing metamaterial.
Preferably, the roughening solution is a mixed solution of hydrofluoric acid with a mass concentration of 40%, ammonium chloride and deionized water, and the mass ratio of hydrofluoric acid: ammonium chloride: deionized water 20 mL: 2 g: 1L of the compound.
Preferably, the sensitizing solution is a mixed solution of palladium chloride, stannous chloride, sodium chloride, 36% by mass of concentrated hydrochloric acid and deionized water, and the ratio of the palladium chloride: stannous chloride: sodium chloride: concentrated hydrochloric acid: deionized water 0.5 g: 30g of: 120 g: 80mL of: 1L of the compound.
Preferably, the in-situ synthesis solution in step S2 is a mixed solution of iron salt, cobalt salt or nickel salt, and sodium citrate, and the ratio of the cobalt salt or nickel salt: iron salt: the molar ratio of sodium citrate is 1: 2: 55.5.
preferably, the iron salt is ferric chloride, the cobalt salt is cobalt chloride, and the nickel salt is nickel chloride.
Compared with the prior art, the invention has the following beneficial effects:
(1) the microporous magnetic medium composite ceramic wave-absorbing metamaterial realizes intrinsic negative electromagnetic parameters of the material by utilizing the synergy of the dielectric loss of the periodic array microporous ceramic and the magnetic loss of the nano ferrite, and has a wide-band stealth effect;
(2) the microporous magnetic medium composite ceramic wave-absorbing metamaterial has the advantages of relatively simple structure, mature preparation process, easily obtained raw materials, low cost, easy large-scale production and application, and great application potential in the engineering field.
Drawings
FIG. 1 is a schematic cross-sectional view of a microporous magnetic medium composite ceramic wave-absorbing metamaterial according to embodiment 1 of the present invention;
FIG. 2 is a diagram of a periodic array alumina microporous ceramic sample in a microporous magnetic medium composite ceramic wave-absorbing metamaterial according to embodiment 1 of the present invention;
FIG. 3 is an equivalent permeability diagram of a microporous magnetic medium composite ceramic wave-absorbing metamaterial according to embodiment 1 of the present invention;
fig. 4 is an equivalent dielectric constant diagram of the microporous magnetic medium composite ceramic wave-absorbing metamaterial provided in embodiment 1 of the invention.
Description of reference numerals:
1. periodic array microporous ceramics; 2. a nano magnetic ferrite.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
With reference to fig. 1 and 2, an embodiment 1 of the present invention provides a microporous magnetic medium composite ceramic wave-absorbing metamaterial structure, including periodic array microporous ceramic 1 and nano magnetic ferrite 2, where a hole of the periodic array microporous ceramic 1 is a square hole, and the nano magnetic ferrite 2 is embedded in the hole of the periodic array microporous ceramic 1; the aperture of the periodic array microporous ceramic is 400 microns, the thickness of the periodic array microporous ceramic is 1.0mm, and the embedding depth of the nano magnetic ferrite is 0.5 mm; the periodic array microporous ceramic is alumina microporous ceramic which can be purchased from the market, the relative dielectric constant of the alumina microporous ceramic is 10, and the dielectric loss tangent value is 0.1;
the preparation method of the microporous magnetic medium composite ceramic wave-absorbing metamaterial comprises the following steps:
s1: the pretreatment of the alumina microporous ceramic comprises the following steps: dissolving 0.2g of ammonium fluoride in 50mL of deionized water, adding 2mL of hydrofluoric acid with the mass concentration of 40% into the completely dissolved ammonium fluoride, uniformly stirring to obtain a mixed solution, transferring the mixed solution into a 100mL volumetric flask, and performing constant volume to obtain a coarsening solution; adding the coarsening liquid into the alumina microporous ceramic, wherein the alumina microporous ceramic comprises the following steps: roughening solution 1 g: 2mL, performing ultrasonic treatment for 30min at room temperature, and washing with deionized water for 2-3 times; adding 0.125g of palladium chloride into 20mL of concentrated hydrochloric acid, completely dissolving the palladium chloride in 25mL of deionized water to obtain a solution a, weighing 30g of sodium chloride, dissolving the sodium chloride in 125mL of deionized water to obtain a solution b, mixing the solution a and the solution b to obtain a solution c, weighing 7.5g of stannous chloride, dissolving the stannous chloride in the deionized water to obtain a solution d, adding the solution d into the solution c, transferring the obtained mixed solution to a 250mL volumetric flask, and performing constant volume to obtain a sensitizing solution; adding the sensitizing solution into the coarsened alumina microporous ceramic, wherein the alumina microporous ceramic comprises the following components in percentage by weight: sensitizing solution is 1 g: 2mL, performing ultrasonic treatment for 30min at room temperature, washing with deionized water for 2-3 times, and drying;
s2: mixing 0.2moL/L cobalt chloride aqueous solution, 0.4moL/L ferric chloride aqueous solution and 0.6moL/L sodium citrate aqueous solution in proportion, wherein the total volume is 500 mL. Adjusting the pH of the mixed solution to 10.5 by using sodium hydroxide to prepare an in-situ synthetic solution; fixing the pretreated alumina microporous ceramic in a lining of a 1000mL hydrothermal reaction kettle, pouring in-situ synthetic liquid into the lining of the hydrothermal reaction kettle, wherein the alumina microporous ceramic: 1g of in-situ synthesis solution: 10mL, placing the container in an oven, keeping the temperature at 150 ℃, and reacting for 6 h;
s3: and (4) taking out the alumina microporous ceramic reacted in the step (S2), washing the surface with water, and drying at 70 ℃ to obtain the microporous magnetic medium composite ceramic wave-absorbing metamaterial.
Example 2
The embodiment 2 of the invention provides a microporous magnetic medium composite ceramic wave-absorbing metamaterial structure, which comprises periodic array microporous ceramic and nano magnetic ferrite, wherein holes of the periodic array microporous ceramic are square holes, and the nano magnetic ferrite is embedded in the holes of the periodic array microporous ceramic; the aperture of the periodic array microporous ceramic is 600 mu m, the thickness of the periodic array microporous ceramic is 0.8mm, and the embedding depth of the nano magnetic ferrite is 1 mm; the periodic array microporous ceramic is alumina microporous ceramic which can be purchased from the market, the relative dielectric constant of the alumina microporous ceramic is 9, and the dielectric loss tangent value is 0;
the preparation method of the microporous magnetic medium composite ceramic wave-absorbing metamaterial comprises the following steps:
s1: the same as example 1;
s2: mixing 0.2moL/L cobalt chloride aqueous solution, 0.4moL/L ferric chloride aqueous solution and 0.6moL/L sodium citrate aqueous solution in proportion, wherein the total volume is 500 mL. Adjusting the pH of the mixed solution to 10.5 by using sodium hydroxide to prepare an in-situ synthetic solution; fixing the pretreated alumina microporous ceramic in a lining of a 1000mL hydrothermal reaction kettle, pouring in-situ synthetic liquid into the lining of the hydrothermal reaction kettle, wherein the alumina microporous ceramic: 1g of in-situ synthesis solution: 15mL, placing the container in an oven, keeping the temperature at 150 ℃, and reacting for 8 h;
s3: and preparing the microporous magnetic medium composite ceramic wave-absorbing metamaterial in the same way as the embodiment 1.
Example 3
The embodiment 3 of the invention provides a microporous magnetic medium composite ceramic wave-absorbing metamaterial, which comprises periodic array microporous ceramic and nano magnetic ferrite, wherein holes of the periodic array microporous ceramic are square holes, and the nano magnetic ferrite is embedded in the holes of the periodic array microporous ceramic; the aperture of the periodic array microporous ceramic is 1000 microns, the thickness of the periodic array microporous ceramic is 1.0mm, and the embedding depth of the nano magnetic ferrite is 2 mm; the periodic array microporous ceramic is alumina microporous ceramic which can be purchased from the market, the relative dielectric constant of the alumina microporous ceramic is 12.5, and the dielectric loss angle is 0.5;
the preparation method of the microporous magnetic medium composite ceramic wave-absorbing metamaterial comprises the following steps:
s1: the same as example 1;
s2: mixing 0.2moL/L cobalt chloride aqueous solution, 0.4moL/L ferric chloride aqueous solution and 0.6moL/L sodium citrate aqueous solution in proportion, wherein the total volume is 500 mL. Adjusting the pH value of the mixed solution to 11 by using sodium hydroxide to prepare in-situ synthetic solution; fixing the pretreated alumina microporous ceramic in a lining of a 1000mL hydrothermal reaction kettle, pouring in-situ synthetic liquid into the lining of the hydrothermal reaction kettle, wherein the alumina microporous ceramic: 1g of in-situ synthesis solution: 12mL, placing the container in an oven, keeping the temperature at 150 ℃, and reacting for 10 h;
s3: and preparing the microporous magnetic medium composite ceramic wave-absorbing metamaterial in the same way as the embodiment 1.
The microporous magnetic medium composite ceramic wave-absorbing metamaterial in the embodiment 1 is subjected to an absorption characteristic test, as shown in fig. 3 and 4, the equivalent permeability of the material is shown in fig. 3, and it can be observed that the equivalent permeability gradually rises to a maximum positive value on the right side of 7.46GHz, steeply falls to a minimum negative value at 9.36GHz, slowly rises after 12.6GHz, the equivalent permeability at 7.46GHz generates a magnetic resonance, and then to a broadband negative value at 9.36GHz, which is a typical ferromagnetic resonance; then the equivalent magnetic conductivity at 13.28GHz generates a magnetic resonance again, and then the equivalent magnetic conductivity at 14.96GHz is a broadband negative value; fig. 4 shows the equivalent dielectric constant of the material, and it can be observed that the equivalent dielectric constant generates a weak electrical resonance at 3.38GHz, gradually rises to a maximum positive value at the right side of 3.38GHz, steeply falls to a minimum negative value at 3.83GHz, and then slowly rises to a positive value, and generates a strong electrical resonance at 5.09GHz, and then becomes a broadband negative value at 13.80GHz, which is a typical electrical resonance; the equivalent dielectric constant at 14.58GHz and 21.68GHz is electrically resonated again, and the equivalent dielectric constant sequentially reaches 15.37 GHz and 23.21GHz to be broadband negative values. It can be seen that the electric resonance and the ferromagnetic resonance of the periodic array microporous ceramic in this embodiment 1 cooperate with each other, so that the wave-absorbing bandwidth can be significantly expanded, and the multi-band negative electromagnetic parameters of the material can be realized.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (8)
1. A microporous magnetic medium composite ceramic wave-absorbing metamaterial is characterized by comprising periodic array microporous ceramics and nano magnetic ferrite, wherein holes of the periodic array microporous ceramics are square holes, and the nano magnetic ferrite is embedded in the holes of the periodic array microporous ceramics;
the aperture of the periodic array microporous ceramic is 0.4-1000 mu m, and the thickness of the periodic array microporous ceramic is 0.8-3.5 mm; the embedding depth of the nano magnetic ferrite is 0.5-2 mm;
the preparation method of the microporous magnetic medium composite ceramic wave-absorbing metamaterial comprises the following steps:
s1: carrying out in-situ synthesis pretreatment on the periodic array microporous ceramic through coarsening, sensitizing, cleaning and drying processes;
the roughening process is to immerse the periodic array microporous ceramic into roughening liquid, wherein the periodic array microporous ceramic comprises the following steps: roughening solution 1 g: 2-5 mL, performing ultrasonic treatment for 30min at room temperature, and washing with deionized water for 2-3 times;
the sensitization process is that the periodic array microporous ceramic is immersed into the sensitization liquid, and the periodic array microporous ceramic: sensitizing solution is 1 g: 2-5 mL, performing ultrasonic treatment for 30min at room temperature, and washing with deionized water for 2-3 times;
s2: fixing the pretreated periodic array microporous ceramic in a lining of a hydrothermal reaction kettle, pouring in-situ synthetic liquid into a container, and preparing the periodic array microporous ceramic: 1g of in-situ synthesis solution: 10-15 mL, and adjusting the pH value of the in-situ synthesis solution to 8.0-11.0 by using sodium hydroxide; ultrasonically vibrating for 30min, covering the reaction kettle, placing the reaction kettle in an oven, keeping the temperature at 149.5-150.5 ℃, and reacting for 6-10 h;
s3: and taking out the cooled periodic array microporous ceramic after the reaction of S2, washing the surface with water, and drying at 70 ℃ to obtain the microporous magnetic medium composite ceramic wave-absorbing metamaterial.
2. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 1, wherein the periodic array microporous ceramic is an alumina microporous ceramic.
3. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 2, wherein the alumina microporous ceramic has a relative dielectric constant of 9-12.5 and a dielectric loss tangent of 0-0.5.
4. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 1, wherein the nano magnetic ferrite is Co Fe2O4、Ni Fe2O4Either one or both.
5. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 1, wherein the roughening solution in step S1 is a mixed solution of hydrofluoric acid with a mass concentration of 40%, ammonium chloride and deionized water, and the ratio of hydrofluoric acid: ammonium chloride: deionized water 20 mL: 2 g: 1L of the compound.
6. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 1, wherein the sensitizing solution in the step S1 is a mixed solution of palladium chloride, stannous chloride, sodium chloride, 36% by mass of concentrated hydrochloric acid and deionized water, and the ratio of the palladium chloride: stannous chloride: sodium chloride: concentrated hydrochloric acid: deionized water 0.5 g: 30g of: 120 g: 80mL of: 1L of the compound.
7. The microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 1, wherein the in-situ synthesis solution in step S2 is a mixed solution consisting of iron salt, cobalt salt or nickel salt, and sodium citrate, and the cobalt salt or nickel salt: iron salt: the molar ratio of sodium citrate is 1: 2: 55.5.
8. the microporous magnetic medium composite ceramic wave-absorbing metamaterial according to claim 7, wherein the iron salt is ferric chloride, the cobalt salt is cobalt chloride, and the nickel salt is nickel chloride.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6162532A (en) * | 1998-07-31 | 2000-12-19 | International Business Machines Corporation | Magnetic storage medium formed of nanoparticles |
| CN101503613A (en) * | 2009-02-18 | 2009-08-12 | 安徽大学 | Microwave absorbing material with periodic nanostructure and preparation thereof |
| CN102424570A (en) * | 2011-09-01 | 2012-04-25 | 上海大学 | Preparation method of NiFe2O4 magnetic material |
| CN102770009A (en) * | 2011-05-04 | 2012-11-07 | 深圳光启高等理工研究院 | Wave-absorbing metamaterial |
| CN103319208A (en) * | 2013-05-20 | 2013-09-25 | 合肥工业大学 | Al3O3 ceramic substrate metallization process |
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| CN102952367B (en) * | 2011-08-31 | 2015-08-26 | 深圳光启高等理工研究院 | A kind of metamaterial substrate and preparation method thereof |
| CN106220211B (en) * | 2016-07-26 | 2019-03-05 | 中国人民解放军国防科学技术大学 | A kind of composite material of silicon carbide microwave-absorbing ceramic and preparation method thereof based on Meta Materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6162532A (en) * | 1998-07-31 | 2000-12-19 | International Business Machines Corporation | Magnetic storage medium formed of nanoparticles |
| CN101503613A (en) * | 2009-02-18 | 2009-08-12 | 安徽大学 | Microwave absorbing material with periodic nanostructure and preparation thereof |
| CN102770009A (en) * | 2011-05-04 | 2012-11-07 | 深圳光启高等理工研究院 | Wave-absorbing metamaterial |
| CN102424570A (en) * | 2011-09-01 | 2012-04-25 | 上海大学 | Preparation method of NiFe2O4 magnetic material |
| CN103319208A (en) * | 2013-05-20 | 2013-09-25 | 合肥工业大学 | Al3O3 ceramic substrate metallization process |
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