CN104003706A - Method for preparing nano ferrite composite wave absorber - Google Patents
Method for preparing nano ferrite composite wave absorber Download PDFInfo
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- CN104003706A CN104003706A CN201410241402.0A CN201410241402A CN104003706A CN 104003706 A CN104003706 A CN 104003706A CN 201410241402 A CN201410241402 A CN 201410241402A CN 104003706 A CN104003706 A CN 104003706A
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Abstract
The invention relates to a method for preparing a nano ferrite composite wave absorber. According to the method, mesoporous foamed silicon oxide is taken as a hard template to prepare nano ferrite. The method comprises the following specific steps; 1) adding the mesoporous foamed silicon oxide into an acid solution of an inorganic metal salt, and stirring uniformly; 2) transferring an obtained mixture liquid into a high-pressure reaction kettle for hydrothermal crystallization reaction; 3) filtering an obtained product, washing with water and drying so as to prepare nano powder, and calcining the dried nano powder at high temperature; 4) adding SiO2 powder and attapulgite powder into the obtained calcined powder, granulating and forming so as to prepare the nano ferrite composite wave absorber. The method has the advantages that firstly, the nano ferrite is a multielement metallic oxide material and has properties of ferroelectric, electromagnetic and dielectric semiconductors; 2) by adopting the method, a series of different nano ferrites can be obtained through different proportioning of mass of metal salt substances.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material technical field, be specifically related to a kind of preparation method of nanometer ferrite composite wave-absorbing body.
Background technology
Electromagenetic wave radiation has become the another large public hazards after sound pollution, topsoil, water pollution, solid waste pollution.The electromagnetic interference that electromagenetic wave radiation produces not only affects the normal operation of various electronicss, and also has very large harm to healthy.The microminiaturization of electronic technology, the development of integrated and high frequencyization make electromagnetic compatibility problem increasingly outstanding, and anti-electromagnetic interference more and more draws attention as the core content of electromagnetic compatibility.Absorbing material technology is as a kind of conventional anti-electromagnetic interference means, useless and harmful electromagnetic energy absorption that electromagnetic pollution can be produced, conversion and attenuate, become the focus of the technical field researchs such as the stealthy and civilian anti-electromagnetic radiation of various countries' military equipment.
In existing absorbing material, ferrite and metal-powder, because of its good effect and lower cost, become the main component of absorbing material.But it is larger that traditional technology is prepared the size of ferrite particle, generally at micron order.
Document 1: Chen Tingli, nanometer zinc ferrite ZnFe
2o
4preparation and the research of performance, University Of Suzhou, 2012.This Research Literature is with zinc nitrate, iron nitrate, and urea, ammoniacal liquor etc. are raw material, utilize sol-gel method and coprecipitation method to prepare nanometer zinc ferrite presoma, and by calcining, prepare the nanometer zinc ferrite iron particle of spinel type.
Document 2: Xu Guocai, the preparation and application of nanometer zinc ferrite, it utilizes monocrystalline ferric acetyl acetonade and a hydration zinc acetylacetonate is raw material, hydrolysis obtains ZnFe
2o
4nano crystal material.
Document 3: Guo Ruiqian, the magnetic research of element doping M type barium ferrite ultra-micro powder, it utilizes sol-gel self-propagating high-temperature synthesis to prepare rare earth doped barium ferrite ultra-micro powder.
Document 4: Chen Xirong, hydrothermal method is synthesized nickel-zinc ferrite technical study, and it take single nickel salt, ferrous sulfate, zinc sulfate and sodium hydroxide as raw material, adopts hydrothermal synthesis method to prepare nanometer Ni
1-xzn
xfe
2o
4ferrite powder.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanometer ferrite absorbing material.
The technical solution that realizes the object of the invention is: a kind of preparation method of nanometer ferrite composite wave-absorbing body, and its concrete preparation process is:
1) mesoporous foam silicon oxide is joined in the acid solution of inorganic metal salt, stir;
2) step 1) gained mixed solution is transferred to and in autoclave, carries out hydrothermal crystallizing reaction;
3) by step 2) products therefrom filters, washes and be dried, and makes nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination;
4) will in the calcined powder of step 3) gained, add SiO
2powder and attapulgite powder, after granulating, moulding, make nanometer ferrite composite wave-absorbing body.
Preferably, the mass ratio of the mesoporous foam silicon oxide described in step 1) and inorganic metal salt is (2～4): 1, and the mass ratio of inorganic metal salt and acid solution is 1:20, the solute massfraction of acid solution is 10%.
Preferably, the specific surface area of the mesoporous foam silicon oxide described in step 1) is 600～1000m
2/ g, aperture is 20～50nm, described inorganic metal salt is metal chloride or nitrate or vitriol.
Further, step 2) described hydrothermal crystallizing temperature of reaction is 130～150 ℃, and the reaction times is 12～24 hours.
Further, the nanometer powder described in step 3) is multi-element metal oxide, with general formula, is expressed as AB
xfe
10-xo
16, 0≤x≤1, wherein, A is Mg, Ba, Mn or Zn, B is Nd or Ni.
Further, the SiO described in step 4)
2mass ratio 1:(1～3 of powder and attapulgite powder), described SiO
2mass ratio 1:(4～6 of powder and mesoporous foam silicon oxide).
Preferably, described multi-element metal oxide is MnFe
10o
16.
Preferably, described multi-element metal oxide is MgNd
0.4fe
9.6o
16.
Preferably, described multi-element metal oxide is BaNd
0.2fe
9.8o
16.
Preferably, described multi-element metal oxide is ZnSmFe
9o
16.
The invention has the advantages that: 1) nanometer ferrite is multi-element metal oxide material, have ferroelectric, ferromagnetic, dielectric semiconductor property; 2) take mesoporous foam silicon oxide as matrix, by means of the ultra-large aperture of mesopore silicon oxide foam materials and the special construction of three-dimensional communication, thereby obtain the orderly nanometer ferrite that distributes, this nanometer ferrite has the characteristic of nano-meter characteristic and the 3 D pore canal of material concurrently; 3) the nano-attapulgite powder that the present invention adds in moulding process, can not only reduce the reunion of nano-powder, improves the conjugation of powder, can play the effect of doping in sintering process simultaneously; 4) the present invention can pass through the different proportionings of metal-salt amount of substance, obtains a series of different nanometer ferrites.
Embodiment
Below by example, further describe feature of the present invention, but the present invention is not limited to following example.
Embodiment 1
Get x=0, prepare nanometer Mn ferrite.
1) take 0.1667 gram of manganous nitrate, 1.333 gram ferric sulfate, join in the salpeter solution that 28.5 milliliters of massfractions are 10%, then add 3 grams of mesoporous foam silicon oxide powders, stir, then being transferred to liner is that in 25 milliliters of reactors of tetrafluoroethylene, transfer amount is about 80% of reactor volume.By reactor sealing, put into 130 ℃ of loft drier and react 12 hours, naturally cool to room temperature, gained mixed solution is filtered, washed and is dried, make nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination, obtain multi-element metal oxide MnFe
10o
16.
2) by the calcined powder multi-element metal oxide MnFe of gained
10o
160.5 gram of SiO of middle interpolation
2powder and 0.5 gram of attapulgite powder, after granulating, moulding, make nanometer Mn ferrite composite wave-absorbing body.
Embodiment 2
Get x=1, prepare nanometer Zn ferrite.
1) take 0.1234 gram of zinc sulfate, 0.2578 gram of samaric nitrate, 1.1188 gram iron(ic) chloride, join in the sulphuric acid soln that 28 milliliters of massfractions are 10%, then add 6 grams of mesoporous foam silicon oxide powders, stir, being then transferred to liner is that in 25 milliliters of reactors of tetrafluoroethylene, transfer amount is about 80% of reactor volume.By reactor sealing, put into 150 ℃ of loft drier and react 24 hours, naturally cool to room temperature, gained mixed solution is filtered, washed and is dried, make nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination, obtain multi-element metal oxide ZnSmFe
9o
16.
2) by the calcined powder multi-element metal oxide ZnSmFe of gained
9o
161 gram of SiO of middle interpolation
2powder and 3 grams of attapulgite powder, after granulating, moulding, make nanometer Zn ferrite composite wave-absorbing body.
Embodiment 3
Get x=0.4, prepare nanometer Mg ferrite.
1) take 0.0874 gram of magnesium sulfate, 0.1419 gram of neodymium nitrate, 1.2606 gram iron(ic) chloride, join in the hydrochloric acid soln that 27.9 milliliters of massfractions are 10%, then add 3.6 grams of mesoporous foam silicon oxide powders, stir, being then transferred to liner is that in 25 milliliters of reactors of tetrafluoroethylene, transfer amount is about 80% of reactor volume.By reactor sealing, put into 135 ℃ of loft drier and react 16 hours, naturally cool to room temperature, gained mixed solution is filtered, washed and is dried, make nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination, obtain multi-element metal oxide MgNd
0.4fe
9.6o
16.
2) by the calcined powder multi-element metal oxide MgNd of gained
0.4fe
9.6o
161.25 grams of SiO of middle interpolation
2powder and 2.5 grams of attapulgite powder, after granulating, moulding, make nanometer Mg ferrite composite wave-absorbing body.
Embodiment 4
Get x=0.2, prepare nanometer Ba ferrite.
1) take 0.2022 gram of nitrate of baryta, 0.0678 gram of neodymium nitrate, 1.2300 gram iron(ic) chloride, join in the hydrochloric acid soln that 27.9 milliliters of massfractions are 10%, then add 5.1 grams of mesoporous foam silicon oxide powders, stir, being then transferred to liner is that in 25 milliliters of reactors of tetrafluoroethylene, transfer amount is about 80% of reactor volume.By reactor sealing, put into 145 ℃ of loft drier and react 20 hours, naturally cool to room temperature, gained mixed solution is filtered, washed and is dried, make nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination, obtain multi-element metal oxide BaNd
0.2fe
9.8o
16.
2) by the calcined powder multi-element metal oxide BaNd of gained
0.2fe
9.8o
161.02 grams of SiO of middle interpolation
2powder and 2.55 grams of attapulgite powder, after granulating, moulding, make nanometer Ba ferrite composite wave-absorbing body.
Claims (10)
1. a preparation method for nanometer ferrite composite wave-absorbing body, is characterized in that: concrete preparation process is:
1) mesoporous foam silicon oxide is joined in the acid solution of inorganic metal salt, stir;
2) step 1) gained mixed solution is transferred to and in autoclave, carries out hydrothermal crystallizing reaction;
3) by step 2) products therefrom filters, washes and be dried, and makes nanometer powder, and the nanometer powder after drying is carried out to high-temperature calcination;
4) will in the calcined powder of step 3) gained, add SiO
2powder and attapulgite powder, after granulating, moulding, make nanometer ferrite composite wave-absorbing body.
2. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 1, it is characterized in that: the mass ratio of the mesoporous foam silicon oxide described in step 1) and inorganic metal salt is (2～4): 1, the mass ratio of inorganic metal salt and acid solution is 1:20, and the solute massfraction of acid solution is 10%.
3. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 1, is characterized in that: the specific surface area of the mesoporous foam silicon oxide described in step 1) is 600～1000m
2/ g, aperture is 20～50nm, described inorganic metal salt is metal chloride or nitrate or vitriol.
4. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 1, is characterized in that: step 2) described hydrothermal crystallizing temperature of reaction is 130～150 ℃, the reaction times is 12～24 hours.
5. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 1, is characterized in that: the nanometer powder described in step 3) is multi-element metal oxide, with general formula, is expressed as AB
xfe
10-xo
16, 0≤x≤1, wherein, A is Mg, Ba, Mn or Zn, B is Nd or Sm.
6. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 1, is characterized in that: the SiO described in step 4)
2mass ratio 1:(1～3 of powder and attapulgite powder), described SiO
2mass ratio 1:(4～6 of powder and mesoporous foam silicon oxide).
7. the preparation method of a kind of nanometer ferrite composite wave-absorbing body according to claim 5, is characterized in that: described multi-element metal oxide is MnFe
10o
16.
8. the preparation method of a kind of nanometer ferrite absorbing material according to claim 5, is characterized in that: described multi-element metal oxide is MgNd
0.4fe
9.6o
16.
9. the preparation method of a kind of nanometer ferrite absorbing material according to claim 5, is characterized in that: described multi-element metal oxide is BaNd
0.2fe
9.8o
16.
10. the preparation method of a kind of nanometer ferrite absorbing material according to claim 5, is characterized in that: described multi-element metal oxide is ZnSmFe
9o
16.
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Cited By (3)
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| CN104496454A (en) * | 2015-01-19 | 2015-04-08 | 陈吉美 | Preparation method of nanometer ferrite particle |
| CN105702405A (en) * | 2016-04-29 | 2016-06-22 | 湖北工程学院 | Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method |
| CN107690271A (en) * | 2017-08-30 | 2018-02-13 | 兰州理工大学 | Rear-earth-doped barium ferrite magnetoelectric composites preparation method |
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| CN104003706B (en) | 2016-04-13 |
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