CN103193473A - Preparation method of microwave absorbing material with three-dimensional ordered macroporous structure - Google Patents
Preparation method of microwave absorbing material with three-dimensional ordered macroporous structure Download PDFInfo
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- CN103193473A CN103193473A CN2013101381650A CN201310138165A CN103193473A CN 103193473 A CN103193473 A CN 103193473A CN 2013101381650 A CN2013101381650 A CN 2013101381650A CN 201310138165 A CN201310138165 A CN 201310138165A CN 103193473 A CN103193473 A CN 103193473A
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Abstract
The invention discloses a preparation method of a microwave absorbing material with a three-dimensional ordered macroporous structure. The preparation method comprises the following steps of: adding nickel nitrate (or cobalt nitrate) and ferric nitrate according to a molar ratio of 1:2 into a mixed solution of ethylene glycol and methanol and uniformly dissolving; then adding polymethyl methacrylate (PMMA) serving as a hard template and soaking for a period of time; and finally calcining to remove a template so as to acquire the microwave absorbing material with the three-dimensional ordered macroporous structure. The material has good degree of crystallization and shape; and electromagnetic waves are mainly absorbed by the material in high-frequency regions, and the absorption effect is good.
Description
Technical field
The invention belongs to the synthetic field of inorganic chemical, particularly a kind of structure of microwave absorbing material and preparation method relate in particular for absorbing electromagnetic material structure and preparation method
Background technology
In recent years, the develop rapidly of hertzian wave technology, the pollution that electromagnetic radiation produces has become a big important arch-criminal of harm environment and HUMAN HEALTH, so begun to have caused attention widely.In military field, microwave absorbing material can reduce the radar wave emission cross section of weaponry effectively simultaneously, realizes radar invisible, improves viability and the penetration ability of weaponry.The main mechanism of action of absorbing material is after making incident electromagnetic wave touch material, can enter in the material to greatest extent, and by the conversion of energy so rapidly attenuation loss fall.
Ferrite is a kind of traditional magnetic material, it has higher resistivity and magnetic loss characteristic preferably, therefore be widely used as radio-radar absorber, but be subject to the snoek effect, the magnetic loss of spinel type ferrite absorbing material can have significantly decline in the range of frequency of mega hertz.So the research for microwave absorbing material focuses on high-frequency range now.For example, patent CN101914821A discloses a kind of Ni-Zn ferrite and SiO
2The preparation method of composite nano-fiber material, it is by control microstructure of product and pattern, thereby realized the controlled of electromagnetic performance, it has then overcome traditional ferrite powder resonant frequency to the absorption of electromagnetic wave performance and has crossed low and shortcoming such as the snoek limit is lower; Patent CN102214509A discloses the preparation method of a kind of novel (FeCo) N microwave absorbing material, it carries out mechanical alloying for 50%-95% by mass percentage with carbonyl iron dust and cobalt powder, nitriding treatment is carried out to the material of alloying in the back, having obtained nitrogen content is (FeCo) N microwave absorbing material of mass percent 0.08%-2.10%, this material has the low remanent magnetism of higher saturation magnetization and coercive force, so absorbing property is preferably arranged; It is SmMe that patent CN1240659C discloses a kind of chemical formula
xFe
1-xO
3, wherein Me is one or both in Mn, Co or the Ni element, the span of x is 0.05-0.75.When this material is 1mm at thickness, the reflection of electromagnetic wave in 2-18GHz range of frequency decay minimum value has been reached-15dB, and advantage such as it is wide to have the wave frequency of suction, and synthetic method is simple, and production cost is low.
Summary of the invention
Purpose of the present invention is at synthetic a kind of ferrite with three-dimensional ordered macroporous structure, and showed good microwave absorbing effect.
The technical solution used in the present invention: adopt the hard template pickling process, may further comprise the steps: soluble ferric iron salt and nickel salt (or cobalt salt) are dissolved in the solvent, and the back adds template dipping for some time, after suction filtration obtains solid and puts into retort furnace and calcine then, obtains product.
What described segment template agent was used is polymethylmethacrylate (PMMA) microballoon.PMMA synthesizes according to bibliographical information, and particle diameter is very unified.By centrifugal and method sedimentation, make the PMMA microballoon closely arrange accumulation, form the colloid crystal template.
What the soluble metal salt of described part adopted is iron nitrate and nickelous nitrate (or Xiao Suangu).
The solvent of described part is the mixed solvent of ethylene glycol and methyl alcohol.
Preparation comprises the following steps
(a) according to bibliographical information, polymethylmethacrylate (PMMA) the microsphere template agent of preparation uniform particle diameter;
(b) nickelous nitrate (or Xiao Suangu) and iron nitrate are dissolved in the mixing solutions of ethylene glycol and methyl alcohol as precursor solution;
(c) a certain amount of PMMA microsphere template is immersed in the precursor solution, dipping for some time, back suction filtration obtains solid;
(d) solid that obtains after the drying is calcined to remove template under air, obtain having the spinel type ferrite of three-dimensional ordered macroporous structure at last.
Beneficial effect of the present invention: adopt the present technique route to prepare ferrite wave-absorbing material, have advantages such as raw material sources are extensive, reaction process simple, simple operation.In addition, the present invention has overcome traditional ferrite wave-absorbing material not good shortcoming of assimilation effect in high-frequency range.The template PMMA microballoon that adopts among the present invention is synthetic easy and particle diameter is controlled.The ferrite that the present invention synthesizes is traditional spinel crystal formation, and has macroporous structure.Ferrite wave-absorbing material among the present invention is three-dimensional order to be arranged, thereby has improved the absorption of electromagnetic wave performance.
Description of drawings
Fig. 1 is three-dimensional ordered macroporous ferritic X-ray diffractogram
Fig. 2 is three-dimensional ordered macroporous ferritic sem photograph
Fig. 3 is three-dimensional ordered macroporous ferritic N
2The adsorption desorption thermoisopleth
Fig. 4 is three-dimensional ordered macroporous ferrite microwave absorbing figure
Embodiment
Hard template method is synthesized three-dimensional ordered macroporous ferritic embodiment:
(1) is that 1: 2 nickelous nitrate (or Xiao Suangu) and iron nitrate is dissolved in the mixed solvent of 10mL ethylene glycol and methyl alcohol with mol ratio, is stirred to and obtains precursor solution after even;
(2) will flood some hours in 2g polymethylmethacrylate (PMMA) the microsphere template agent adding precursor solution;
(3) flooded after, remove excessive solution, with the solid Air drying 24h of gained;
The above-mentioned solid that obtains is calcined to remove template in retort furnace, concrete steps are: under air atmosphere, rise to 550 ℃ or 600 ℃ by room temperature, keep several hrs, treat that template is removed fully after, be down to room temperature, can obtain having the ferrite wave-absorbing material of three-dimensional ordered macroporous structure.XRD referring to accompanying drawing 1 characterizes, in 2 θ=30.31 °, 35.42 °, 43.66 °, 53.8 °, 57.51 °, 63.15 ° of (220) that correspond respectively to face-centred cubic structure, (311), (400), (422), (511) and (440) crystal face meets the structure (JCPDS No.10-325) of nickel (or cobalt) hercynite fully.
Shown in accompanying drawing 2, adopt the synthetic ferrite of hard template method to have very complete three-dimensional ordered macroporous structure, can see that the aperture of macroporous structure is unusual homogeneous also, this is relevant with our uniform particle diameter of selected template.Our material is behind the calcining template agent removing, and slightly shrink in the aperture.
By accompanying drawing 3 as can be known, adopting the synthetic ferritic nitrogen adsorption desorption thermoisopleth of hard template method is typical III type thermoisopleth, have H3 type hysteresis loop, thermoisopleth has one section very significantly lifting after p/p0＞0.8, and this illustrates eurypyloue existence in our material.Hole wall with ferrite wave absorbing agent of three-dimensional ordered macroporous structure is piled up by many small-particles and is formed, thereby the size in the thickness of hole wall and aperture is all controlled, we by the preparation different-grain diameter polymethylmethacrylate (PMMA) template or select different microspheric template for use, can prepare the ferrite wave-absorbing material with different pore wall thicknesses and pore size.
By accompanying drawing 4 as can be known, the absorption bandwidth of ferrite wave absorbing agent with three-dimensional ordered macroporous structure is narrower, and when thickness was 3.5mm, the maximum reflection loss value of material of the present invention can be less than-20dB.And this ferrite wave absorbing agent concentrates in the high-frequency region for absorption of electromagnetic wave, and absorption peak is between 11GHz-18GHz.Than other ferrite-type microwave absorbing materials, the present invention has narrow frequency microwave absorbing property efficiently.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. preparation method with ferrite-type microwave absorbing material of three-dimensional ordered macroporous structure, may further comprise the steps: nickelous nitrate (or Xiao Suangu) and iron nitrate are dissolved in ethylene glycol and the methanol mixed solvent, form precursor solution, the back adds template and floods, remove template at last, can obtain the ferrite wave absorbing agent.
2. a kind of ferrite wave-absorbing material with three-dimensional ordered macroporous structure according to claim 1 is characterized in that: adopt polymethylmethacrylate (PMMA) microballoon to do template, template is synthetic according to bibliographical information.
3. a kind of Ni ferrite absorbing material with three-dimensional ordered macroporous structure according to claim 1, it is characterized in that: this ferrite wave absorbing agent is nickel (or cobalt) hercynite type, have the macroporous structure of three-dimensional order simultaneously, pore size is even, and certain specific surface area is arranged.
4. a kind of Ni ferrite absorbing material with three-dimensional ordered macroporous structure according to claim 3, it is characterized in that: this absorbing material concentrates in the high-frequency region for absorption of electromagnetic wave, has remedied the deficiency of conventional iron oxysome wave absorbing agent.When thickness is 3.5mm, this absorbing material high frequency treatment have a great reflection loss value (＜-20dB), this means that hertzian wave has＞99% loss in this frequency.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103756635A (en) * | 2013-11-21 | 2014-04-30 | 张宇 | Preparation method of mesoporous silica foam based composite wave-absorbing material |
| CN106145919A (en) * | 2016-07-05 | 2016-11-23 | 陕西科技大学 | A kind of preparation method of three-dimensional netted ferrite microwave absorbing material |
| CN107098691A (en) * | 2017-05-16 | 2017-08-29 | 天长市中德电子有限公司 | A kind of wave filter soft magnetic ferrite and preparation method thereof |
| CN109650933A (en) * | 2019-01-28 | 2019-04-19 | 陕西科技大学 | A kind of porous C o3O4/Al2SiO5Low-density inhales wave mode complex phase ceramic and preparation method thereof |
| CN110299540A (en) * | 2019-07-02 | 2019-10-01 | 陕西科技大学 | A kind of NiCo of three-dimensional netted hierarchical porous structure2O4The preparation method of elctro-catalyst |
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| CN102190483A (en) * | 2010-03-01 | 2011-09-21 | 中国科学院生态环境研究中心 | Three-dimensional micro-nano material composed of nano CoFe2O4 and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103756635A (en) * | 2013-11-21 | 2014-04-30 | 张宇 | Preparation method of mesoporous silica foam based composite wave-absorbing material |
| CN106145919A (en) * | 2016-07-05 | 2016-11-23 | 陕西科技大学 | A kind of preparation method of three-dimensional netted ferrite microwave absorbing material |
| CN107098691A (en) * | 2017-05-16 | 2017-08-29 | 天长市中德电子有限公司 | A kind of wave filter soft magnetic ferrite and preparation method thereof |
| CN107098691B (en) * | 2017-05-16 | 2020-07-10 | 天长市中德电子有限公司 | Soft magnetic ferrite material for filter and preparation method thereof |
| CN109650933A (en) * | 2019-01-28 | 2019-04-19 | 陕西科技大学 | A kind of porous C o3O4/Al2SiO5Low-density inhales wave mode complex phase ceramic and preparation method thereof |
| CN109650933B (en) * | 2019-01-28 | 2021-03-30 | 陕西科技大学 | Porous Co3O4/Al2SiO5Low-density wave-absorbing type complex phase ceramic and preparation method thereof |
| CN110299540A (en) * | 2019-07-02 | 2019-10-01 | 陕西科技大学 | A kind of NiCo of three-dimensional netted hierarchical porous structure2O4The preparation method of elctro-catalyst |
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Application publication date: 20130710 |