CN102807840A - Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material - Google Patents

Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material Download PDF

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CN102807840A
CN102807840A CN2012102939123A CN201210293912A CN102807840A CN 102807840 A CN102807840 A CN 102807840A CN 2012102939123 A CN2012102939123 A CN 2012102939123A CN 201210293912 A CN201210293912 A CN 201210293912A CN 102807840 A CN102807840 A CN 102807840A
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composite wave
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CN102807840B (en
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李巧玲
景红霞
叶云
杨晓峰
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North University of China
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North University of China
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Abstract

The invention discloses a preparation method for a nanometer Fe3O4-SrFe12O19 compound wave absorption material. The preparation method comprises the steps as follows: completely dispersing SrFe12O19 in water to prepare a dispersion solution; dissolving FeCl3.6H2O and FeCl2.4H2O in the water to prepare a water solution; uniformly mixing the required amount of the dispersion solution and the water solution; heating and stirring under the pH value of 11-12; and cooling, washing and drying to obtain the nanometer Fe3O4-SrFe12O19 compound wave absorption material. The maximum reflectance of the nanometer Fe3O4-SrFe12O19 compound wave absorption material in the frequency range of 0-6 GHz reaches -17.7 dB and is superior to -5 dB, the frequency width is 1.3 GHz, the frequency domain of 2.13-3.43 GHz is covered, the absorption capability in the low frequency band can be improved and the absorption frequency band can be widened.

Description

Nanometer Fe 3O 4-SrFe 12O 19The preparation method of composite wave-suction material
Technical field
The present invention relates to absorbing material, particularly relate to a kind of preparation method who has the thin type composite wave-suction material of absorbing property in low-frequency range.
Background technology
In recent years; Develop rapidly along with the military radar Detection Techniques; And the promoting the use of of civilian calutron such as mobile phone, microwave oven, the absorbing material that can be used for stealthy design of weaponry and daily electromagnetic radiation protection field has received attention and further investigation more and more widely.China compares with west advanced country the research of absorbing material; Obtained certain breakthrough in some research direction; Obtained very big progress like 4～18GHz wave band, some absorbing material gets into the application stage, but waits development research at the employed slim absorbing material of 2～4GHz frequency range.
Ferrite Material is an a kind of pair of composite dielectric, and under electromagnetic field effect, Ferrite Material has magnetic loss and two kinds of functions of dielectric loss, thereby is a kind of good absorbing material.But there are shortcomings such as absorption band is narrow, absorption intensity is low in single Ferrite Material, makes it can't satisfy increasingly high application requiring.And nano composite material possibly be the desirable approach that addresses this problem, and it provides a new approach for development high-performance novel material with the performance that improves current material, becomes an important directions of novel material research.Nanometer Fe 3O 4With its significant magnetosensitive, gas-sensitive property and surface effects etc., great application prospect is arranged at aspects such as high density magnetic recording material, air humidity dependent sensor spare, magnetic fluid matrix material, absorbing material, catalyzer.
About Fe 3O 4--SrFe 12O 19The preparation of matrix material and performance, existing at home and abroad report." Fe 3O 4The preparation of/strontium ferrites composite wave-suction material and performance " (Yan Fangliang etc., magneticsubstance and device, 2009,40 (2): 25-29) disclose a kind of Fe of using 3O 4With SrFe 12O 19The compound composite wave-suction material that obtains in 2～18GHz scope, is worked as Fe 3O 4Content is 40%, when thickness of sample remains on the 2.4mm left and right sides, maximum loss reaches-23.2dB at the 14.5GHz place ,-5dB bandwidth is 7.7GHz.The Fe of this report 3O 4/ strontium ferrites composite wave-suction material is the matrix material that adopts the physical blending method to prepare, and its defective is: nanoparticle is prone to reunite Fe in 1) the preparation process 3O 4With SrFe 12O 19In system, be difficult to be uniformly dispersed, composite structure has uncertainty; 2) 0～6GHz scope internal loss less (＞-5db), absorption band is also narrower in addition.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of nanometer Fe is provided 3O 4-SrFe 12O 19The preparation method of composite wave-suction material is with the nanometer Fe of preparing method's preparation of the present invention 3O 4-SrFe 12O 19Composite wave-suction material can improve the receptivity in low-frequency range, widens absorption band.
Nanometer Fe provided by the invention 3O 4-SrFe 12O 19The preparation method of composite wave-suction material may further comprise the steps:
1) with SrFe 12O 19Be dispersed in fully and process dispersion liquid in the water;
2) with FeCl 36H 2O and FeCl 24H 2O is according to Fe 3+With Fe 2+Mol ratio be that the ratio of 1:3～4 is dissolved in the water, process the aqueous solution;
3) according to Fe 3O 4With SrFe 12O 19Mass ratio be the dose relationship of 1:0.1～0.4, the dispersion liquid and the aqueous solution of requirement is even, obtain mixed solution;
4) pH value to 11～12 of mixed solution are regulated in heating mixed solution to 30～40 ℃, continue to be heated to 50 ℃, stirring reaction 2～3h;
5) cooling to neutral, obtains nanometer Fe with the reaction product washing after the drying 3O 4-SrFe 12O 19Composite wave-suction material.
Wherein, can adopt following at least a method, or adopt two kinds of methods simultaneously, with SrFe 12O 19Be dispersed in the water fully:
A) stir 10～50min not being higher than under 50 ℃ the temperature;
B) power ultrasonic with 100～120w is handled 0.5～1h in ultrasonic apparatus.
Fig. 1 is the nanometer Fe of different mass ratio 3O 4-SrFe 12O 19The X-ray diffraction analysis collection of illustrative plates of composite wave-suction material.Can find out its each diffraction peak and Fe from the curve a of XRD figure 3O 4PDF standard card (PDF No.19-0629) fits like a glove, and shows that this material is the Fe of pure cube inverse spinel structure 3O 4Can find out its each diffraction peak and SrFe from curve d 12O 19PDF standard card (PDF No.24-1207) fits like a glove, and shows that products therefrom is the SrFe of pure hexaplanar magnetoplumbite structure 12O 19When M(Fe 3O 4): M(SrFe 12O 19Obtain curve b during)=1:0.1, its each diffraction peak and Fe 3O 4The diffraction peak position is identical, but diffraction intensity weakens relatively; When M(Fe 3O 4): M(SrFe 12O 19Obtain curve c during)=1:0.3, its each main diffraction peak and Fe 3O 4The diffraction peak position is identical, and diffraction intensity further weakens, but also SrFe is arranged 12O 19Diffraction peak occur, just diffraction intensity a little less than, show that the magnetoplumbite phase composition in the sample structure increases, the spinel phase composition reduces.
Fig. 2 is the transmission electron microscope collection of illustrative plates of different samples.Can find out Fe from the figure a of TEM figure 3O 4Be the spheroidal particle of particle diameter between 10～15nm; Figure b can find out SrFe 12O 19Be the rod-shpaed particle between diameter 500～700nm; Figure c then can find out Fe 3O 4Cover SrFe equably 12O 19The surface forms one deck coating layer.
With the nanometer Fe for preparing 3O 4-SrFe 12O 19After composite wave-suction material grinds, as sticker, mix, behind 50～70 ℃ of consolutes, inject the cylindrical die that thickness of sample is 3mm fast, obtain sample after solidifying and be used to test absorbing property according to the mass ratio of absorbing material: paraffin=7:3 with paraffin.
Fig. 3 is the nanometer Fe of different mass ratio 3O 4-SrFe 12O 19The absorption curve figure of composite wave-suction material.Can find out, in 0～6GHz scope, Fe 3O 4-SrFe 12O 19The whole absorbent capacity of matrix material is than pure Fe 3O 4Or SrFe 12O 19Raising is all arranged, and effectively absorption band is widened.And, along with SrFe 12O 19The increase of consumption, Fe 3O 4-SrFe 12O 19The suction crest of matrix material moves to high frequency region, and near SrFe 12O 19Suction crest shape and position.Wherein, when M(Fe 3O 4): M(SrFe 12O 19During)=1:0.3, the absorbing property of product is best, and its maximum absorption peak is-17.7dB, is superior to-5dB frequency range 1.3GHz, has covered 2.13～3.43GHz frequency domain.
The present invention has following advantage:
1) the present invention adopts interfacial to prepare nanometer Fe 3O 4-SrFe 12O 19Composite wave-suction material, particle is not reunited in the preparation process, but Fe 3O 4Cover SrFe equably 12O 19The surface forms nucleocapsid structure.
2) nanometer Fe of the inventive method preparation 3O 4-SrFe 12O 19In the composite wave-suction material, because Fe 3O 4Mix, natural resonance loss and the domain wall resonance loss of material are increased, thereby the absorbing property of matrix material is greatly improved, effectively absorption band is widened, and has improved the absorbing property of single-material preferably.In 0～6GHz band limits, the maximum reflectivity of composite wave-suction material reaches-17.7dB, is superior to-5dB frequency range 1.3GHz, has covered 2.13～3.43GHz frequency domain, than Fe 3O 4And SrFe 12O 19Maximum absorption peak improve 247% and 185% respectively, frequency band is widened 1.12GHz and 0.40GHz respectively.
Description of drawings
Fig. 1 is the nanometer Fe of different mass ratio 3O 4-SrFe 12O 19The X-ray diffraction analysis collection of illustrative plates of composite wave-suction material.
Among the figure, a does M(Fe 3O 4): M(SrFe 12O 19)=1:0; B does M(Fe 3O 4): M(SrFe 12O 19)=1:0.1; C does M(Fe 3O 4): M(SrFe 12O 19)=1:0.3; D does M(Fe 3O 4): M(SrFe 12O 19)=0:1.
Fig. 2 is for being the nanometer Fe of different mass ratio 3O 4-SrFe 12O 19The transmission electron microscope collection of illustrative plates of composite wave-suction material.
Among the figure, a does M(Fe 3O 4): M(SrFe 12O 19)=1:0; B does M(Fe 3O 4): M(SrFe 12O 19)=0:1; C does M(Fe 3O 4): M(SrFe 12O 19)=1:0.3.
Fig. 3 is the nanometer Fe of different mass ratio 3O 4-SrFe 12O 19The absorption curve figure of composite wave-suction material.
Among the figure, a does M(Fe 3O 4): M(SrFe 12O 19)=1:0; B does M(Fe 3O 4): M(SrFe 12O 19)=1:0.1; C does M(Fe 3O 4): M(SrFe 12O 19)=1:0.3; D does M(Fe 3O 4): M(SrFe 12O 19)=0:1.
Embodiment
Embodiment 1
1.SrFe 12O 19Preparation
Take by weighing 0.21g Sr (NO 3) 2With 4.65g Fe (NO 3) 39H 2O is dissolved in the 50mL zero(ppm) water, and heated and stirred when temperature reaches 80 ℃, adds the 2.62g Hydrocerol A to dissolving fully, mixes, and regulates pH value to 6 with ammoniacal liquor, continue to be heated to 70～80 ℃ stir 2h after, surplus solution is blotted with absorbent cotton.
The absorbent cotton of above-mentioned acquisition behind 90 ℃ of dry 12h, is put into 1050 ℃ retort furnace and calcined 2h, obtain SrFe after the cooling 12O 19Sample.
The SrFe for preparing 12O 19The XRD figure of sample is seen Fig. 1 d, and TEM figure sees Fig. 2 b.It is prepared into the absorbing material sample, test absorption curve such as Fig. 3 d.
2.Fe 3O 4-SrFe 12O 19The preparation of composite wave-suction material
Take by weighing 0.17g SrFe 12O 19In 200mL zero(ppm) water, 30 ℃ are stirred 20min on magnetic stirring apparatus, and it is scattered in the water fully.
Take by weighing 0.98g FeCl 36H 2O and 2.55g FeCl 24H 2O is in 100mL zero(ppm) water, after heated and stirred is dissolved extremely fully, with above-mentioned SrFe 12O 19Dispersion liquid mixes.The heated and stirred mixed solution when temperature reaches 35 ℃, is 12 to the pH value that wherein drips NaOH solution regulator solution.Continue to be heated to 50 ℃, stirring reaction 2h.Behind the naturally cooling, with product wash to the pH value be 7.At last, with the product natural air drying, obtain nanometer Fe 3O 4-SrFe 12O 19Composite wave-suction material, its XRD figure is seen Fig. 1 b.
3. inhale the preparation of ripple sample
With the nanometer Fe that makes 3O 4-SrFe 12O 19Composite wave-suction material mixes with the mass ratio of sticker paraffin by 7:3 after grinding, and behind 50～70 ℃ of consolutes, puts into the cylindrical die of thickness 3mm fast, obtains the absorbing material sample after solidifying, and tests its absorbing property, sees Fig. 3 b.
Embodiment 2
SrFe 12O 19Preparation with embodiment 1.
Take by weighing 0.52g SrFe 12O 19In 300mL zero(ppm) water, supersound process 0.5h under the 120W power is dispersed in the water it fully in ultrasonic apparatus.
Take by weighing 1.0g FeCl 36H 2O and 2.58g FeCl 24H 2O is in 100mL zero(ppm) water, after heated and stirred is dissolved extremely fully, with above-mentioned SrFe 12O 19Dispersion liquid mixes.The heated and stirred mixed solution when temperature reaches 38 ℃, is 12 to the pH value that wherein drips NaOH solution to solution.Continue to be heated to 50 ℃, stirring reaction 2.5h.Behind the naturally cooling, washed product to pH value is 7.At last, with the product natural air drying, obtain nanometer Fe 3O 4-SrFe 12O 19Composite wave-suction material.Its XRD figure is seen Fig. 1 c, and TEM figure sees Fig. 2 c.It is prepared into the absorption curve of testing behind the absorbing material sample sees Fig. 3 c.
Embodiment 3
SrFe 12O 19Preparation with embodiment 1.
Take by weighing 0.35g SrFe 12O 19Be dissolved in the 250mL zero(ppm) water, put into ultrasonic apparatus, supersound process 45min under the 110W power is dispersed in the water it fully.
Take by weighing 1.1g FeCl 36H 2O and 2.57g FeCl 24H 2O is dissolved in the 100mL zero(ppm) water, and be heated be stirred to fully dissolving after, with above-mentioned SrFe 12O 19Dispersion liquid mixes.This mixed solution of heated and stirred when temperature reaches 33 ℃, is 11 to wherein dripping NaOH solution to pH value of solution value.Continue to be heated to 50 ℃ of stirring reaction 3h, behind the naturally cooling, washed product pH value is 7.At last, product is dried in 80 ℃ of baking ovens, be nanometer Fe 3O 4-SrFe 12O 19Composite wave-suction material.
Embodiment 4
SrFe 12O 19Preparation with embodiment 1.
Take by weighing 0.69g SrFe 12O 19Be dissolved in the 350mL zero(ppm) water, 40 ℃ are stirred 20min on magnetic stirring apparatus, and it is scattered in the water fully.
Take by weighing 0.95g FeCl 36H 2O and 2.58g FeCl 24H 2O is dissolved in the 100mL zero(ppm) water, and be heated be stirred to fully dissolving after, with above-mentioned SrFe 12O 19Dispersion liquid mixes.This mixed solution of heated and stirred when temperature reaches 36 ℃, is 11 to wherein dripping NaOH solution to pH value of solution value.Continue to be heated to 50 ℃ of stirring reaction 2.5h, behind the naturally cooling, washed product pH value is 7.At last, product is dried in 80 ℃ of baking ovens, be nanometer Fe 3O 4-SrFe 12O 19Composite wave-suction material.

Claims (3)

1. nanometer Fe 3O 4-SrFe 12O 19The preparation method of composite wave-suction material may further comprise the steps:
1) with SrFe 12O 19Be dispersed in fully and process dispersion liquid in the water;
2) with FeCl 36H 2O and FeCl 24H 2O is according to Fe 3+With Fe 2+Mol ratio be that the ratio of 1:3～4 is dissolved in the water, process the aqueous solution;
3) according to Fe 3O 4With SrFe 12O 19Mass ratio be the dose relationship of 1:0.1～0.4, the dispersion liquid and the aqueous solution of requirement is even, obtain mixed solution;
4) pH value to 11～12 of mixed solution are regulated in heating mixed solution to 30～40 ℃, continue to be heated to 50 ℃, stirring reaction 2～3h;
5) cooling to neutral, obtains nanometer Fe with the reaction product washing after the drying 3O 4-SrFe 12O 19Composite wave-suction material.
2. nanometer Fe according to claim 1 3O 4-SrFe 12O 19The preparation method of composite wave-suction material is characterized in that adopting following at least a method, or adopts two kinds of methods simultaneously, with SrFe 12O 19Be dispersed in the water fully:
A) stir 10～50min not being higher than under 50 ℃ the temperature;
B) power ultrasonic with 100～120w is handled 0.5～1h in ultrasonic apparatus.
3. the nanometer Fe for preparing of claim 1 preparation method 3O 4-SrFe 12O 19Composite wave-suction material.
CN201210293912.3A 2012-08-17 2012-08-17 Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material Expired - Fee Related CN102807840B (en)

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CN105645479A (en) * 2015-12-29 2016-06-08 陕西科技大学 RGO/BaFe12O19/CoFe2O4 (reduced graphene oxide/barium ferrite/cobalt ferrite) composite powder and preparation method
CN105802578A (en) * 2016-03-22 2016-07-27 苏州捷德瑞精密机械有限公司 Electromagnetic-wave-absorbing composite material and preparing method thereof
CN109130411A (en) * 2018-07-17 2019-01-04 佛山市南海区佳妍内衣有限公司 Underwear based on healthcare function
CN113329608A (en) * 2021-06-30 2021-08-31 东北大学秦皇岛分校 Preparation method of nano barium titanate/ferroferric oxide hybrid material with high wave-absorbing performance
CN114933800A (en) * 2022-05-13 2022-08-23 哈尔滨理工大学 Nano ferrite/liquid silicon rubber radar wave-absorbing composite material

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Cited By (6)

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CN105645479A (en) * 2015-12-29 2016-06-08 陕西科技大学 RGO/BaFe12O19/CoFe2O4 (reduced graphene oxide/barium ferrite/cobalt ferrite) composite powder and preparation method
CN105802578A (en) * 2016-03-22 2016-07-27 苏州捷德瑞精密机械有限公司 Electromagnetic-wave-absorbing composite material and preparing method thereof
CN105802578B (en) * 2016-03-22 2018-07-20 蒋吉平 A kind of electro-magnetic wave absorption composite material and preparation method
CN109130411A (en) * 2018-07-17 2019-01-04 佛山市南海区佳妍内衣有限公司 Underwear based on healthcare function
CN113329608A (en) * 2021-06-30 2021-08-31 东北大学秦皇岛分校 Preparation method of nano barium titanate/ferroferric oxide hybrid material with high wave-absorbing performance
CN114933800A (en) * 2022-05-13 2022-08-23 哈尔滨理工大学 Nano ferrite/liquid silicon rubber radar wave-absorbing composite material

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