CN110104692A - One kind having anisotropic magnetic iron ore electromagnetic-wave absorbent and preparation method thereof - Google Patents
One kind having anisotropic magnetic iron ore electromagnetic-wave absorbent and preparation method thereof Download PDFInfo
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- CN110104692A CN110104692A CN201910410733.5A CN201910410733A CN110104692A CN 110104692 A CN110104692 A CN 110104692A CN 201910410733 A CN201910410733 A CN 201910410733A CN 110104692 A CN110104692 A CN 110104692A
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- iron ore
- magnetic iron
- regular hexagon
- wave absorbent
- electromagnetic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses one kind to have anisotropic magnetic iron ore electromagnetic-wave absorbent, and the crystal grain of the material is in regular hexagon laminated structure.The invention also discloses the preparation method of above-mentioned magnetic iron ore electromagnetic-wave absorbent, specifically: Na is added into the mixed solution containing iron chloride and magnesium chloride2Si3O7Solution and NaOH, after reaction, separating, washing product obtains the α-Fe in regular hexagon2O3；α-the Fe that will be obtained2O3It is heat-treated under the protection of the mixed atmosphere of hydrogen and argon gas, obtains that there is anisotropic regular hexagon magnetic iron ore electromagnetic-wave absorbent.Magnetic iron ore electromagnetic-wave absorbent crystal grain of the present invention structure in the form of sheets, each laminated structure morphological rules is in regular hexagon, and each laminated structure size uniformity, and the pattern of regular hexagon sheet makes material have big anisotropy, to enhance Fe3O4The interfacial polarization of particle, therefore increase material magnetic loss, absorbing property improves.
Description
Technical field
The present invention relates to one kind to have anisotropic magnetic iron ore electromagnetic-wave absorbent, further relates to above-mentioned with anisotropy
Magnetic iron ore electromagnetic-wave absorbent preparation method, belong to microwave absorbing material technical field.
Background technique
With the development of electromagnetic technique and the progress of Radar Technology, in industrial and military field to the need of electromagnetic wave absorption agent
It asks and increasingly increases.So far, most popular absorbing material includes carbon-based material, magnetic metal, ferrite and conducting polymer.
Wherein, ferrite have relatively suitable dielectric constant and magnetic conductivity, this makes it have better impedance matching, thus reach compared with
Wide attenuation bandwidth.For example, coke next spring seminar, University of the Inner Mongol, has synthesized (Cu using sol-gal process0.2Ni0.8)Fe2O4Point
Spar type ferrite, the obtained the maximum absorption of institute's frequency measurement section (8~12GHz) are -13.3dB (functional material, 2005,36 (2): 295-
297.).Zhang Weidong seminar, Northwestern Polytechnical University has prepared MoS using hydro-thermal reaction method2@Fe3O4@PANI composite wave-absorbing material
Material, when absorbent is with a thickness of 2.3mm, minimum reflection loss value can reach -40.91dB
(J.Mater.Sci.Mater.Electron.2017,28,15488).Tong Guoxiu seminar, Zhejiang Normal University passes through hydro-thermal method
Prepare the Fe of sea urchin shape3O4, minimum reflection loss value can reach -29.96dB, realizes in 3.76~8.15GHz wave band
Effective electromagnetic absorption (J.Alloys Compd.2011,509,4320).However existing research still remains and faces many problems:
1. traditional spheroidal filler cannot obtain preferable absorbing property due to easily causing magnetic conductivity lower with biggish demagnetizing factor；
2. existing flaky magnet mine preparation process is complicated, time-consuming, low yield, and pattern is irregular, and size is inhomogenous.Therefore a kind of work
Skill is simple, and the preparation method exploitation of product morphology rule obtained, the flaky magnet mine electromagnetic-wave absorbent of size uniformity has very much
It is necessary.
Summary of the invention
Goal of the invention: technical problem to be solved by the invention is to provide one kind, and there is anisotropic magnetic iron ore electromagnetism to inhale
Wave material, magnetic iron ore electromagnetic-wave absorbent crystal grain structure in the form of sheets, each laminated structure morphological rules are in regular hexagon,
And each laminated structure size uniformity, since the pattern of regular hexagon sheet makes material have big anisotropy, to enhance
Fe3O4The interfacial polarization of particle, therefore increase the magnetic loss of material, absorbing property improves.
The present invention also technical problems to be solved are to provide above-mentioned with anisotropic magnetic iron ore electromagnetic-wave absorbent
Preparation method, which can scale without the use of the organic solvent of severe toxicity without complicated synthesis device
Change and produces in enormous quantities.
In order to solve the above technical problems, the technical scheme adopted by the invention is as follows:
One kind having anisotropic magnetic iron ore electromagnetic-wave absorbent, and the crystal grain of the magnetic iron ore electromagnetic-wave absorbent is in the form of sheets
Structure, the shape of every crystal grain are regular hexagon.
Wherein, the inscribed circle diameter of every regular hexagon crystal grain is 1.75~1.8 μm.
The above-mentioned preparation method with anisotropic magnetic iron ore electromagnetic-wave absorbent, comprises the following steps:
Step 1, regular hexagon α-Fe is prepared2O3: Na is added into the mixed solution containing iron chloride and magnesium chloride2Si3O7
Solution and NaOH, after reaction, separating, washing product obtains the α-Fe in regular hexagon2O3；
Step 2, regular hexagon Fe is prepared3O4: the α-Fe that step 1 is obtained2O3It is protected in the mixed atmosphere of hydrogen and argon gas
Under be heat-treated, obtain that there is anisotropic regular hexagon magnetic iron ore electromagnetic-wave absorbent.
Wherein, in step 1, reaction temperature is 190~200 DEG C, and the reaction time is 3.5~4 hours.
Wherein, in step 2, in mixed atmosphere, the quality accounting of argon gas is 95%, and the quality accounting of hydrogen is 5%.
Wherein, in step 2, heat treatment temperature is 750~800 DEG C, and heat treatment time is 1.5~2 hours.
Compared with prior art, technical solution of the present invention has the beneficial effect that
Preparation method of the present invention is with Na2Si3O7With MgCl2·6H2O passes through Na as surfactant2Si3O7With
MgCl2·6H2O additional amount controls the partial size and thickness of magnetic iron ore microplate, obtains the regular hexagon thin slice with big L/D ratio,
Finally obtained magnetic iron ore microplate size uniformity, regular shape；The regular hexagon of rule assigns Fe3O4The big anisotropy of microplate,
To improve the magnetic loss of material, the Fe finally made3O4Microplate shows excellent electromagnetic property；In addition, prepared by the present invention
Method and process is simple, at low cost, it can be achieved that scale is produced in enormous quantities.
Detailed description of the invention
Fig. 1 is α-Fe made from the embodiment of the present invention 12O3With Fe3O4X ray diffracting spectrum；
Fig. 2 a~Fig. 2 d is α-Fe made from the embodiment of the present invention 12O3The SEM photograph of particle；
Fig. 3 is Fe made from the embodiment of the present invention 13O4The SEM photograph of particle；
Fig. 4 a is Fe made from embodiment 13O4The complex dielectric permittivity of particle and the graph of relation of frequency；
Fig. 4 b is Fe made from embodiment 13O4The complex permeability of particle and the graph of relation of frequency；
Fig. 4 c is Fe made from embodiment 13O4The dielectric loss of particle and the graph of relation of frequency；
Fig. 4 d is Fe made from embodiment 13O4The magnetic loss of particle and the graph of relation of frequency；
Fig. 5 is Fe made from the embodiment of the present invention 13O4The reflection loss figure of particle；
The molar ratio and regular hexagon thin slice inscribed circle diameter (d) and regular hexagon sheet thickness that Fig. 6 is different Fe and Si
(t) graph of relation.
Specific embodiment
Below in conjunction with attached drawing, technical scheme is described further, but the scope of protection of present invention is simultaneously
It is not limited to this.
Embodiment 1
The present invention has the preparation method of anisotropic magnetic iron ore electromagnetic-wave absorbent, specifically includes the following steps:
Step 1, regular hexagon α-Fe is prepared2O3Microplate: by 2.7032gFeCl3·6H2O and 0.051g MgCl2·6H2O
It is dissolved in 30mL distilled water, obtains the mixed solution containing iron chloride and magnesium chloride；Then, in above-mentioned mixed solution and dripping
The Na of 0.041mL2Si3O7Solution (Na2Si3O7The mass percentage concentration of solution is 10%), to add 5.2g sodium hydroxide, is stirred
After 30 minutes, mixed material is put into baking oven, keeps the temperature 4 hours at 200 DEG C；α-Fe is obtained after centrifugation, washing, drying2O3
Microplate；
Step 2, regular hexagon Fe is prepared3O4Microplate: the α-Fe that step 1 is obtained2O3Microplate is placed in quartz ampoule, in matter
In the mixed atmosphere for measuring the hydrogen that percentage composition is 5% and the argon gas composition that mass percentage is 95%, calcined at 800 DEG C
2 hours.
Embodiment 2
Na2Si3O7With MgCl2·6H2O is as surfactant to above-mentioned α-Fe2O3The research side of the influence of microplate pattern
Method specifically includes the following steps:
Step 1, different Na are added in preparation2Si3O7With MgCl2·6H2Regular hexagon α-the Fe of O amount2O3Microplate: by 0.1mol
FeCl3·6H2The MgCl of O and 0~0.02mol2·6H2O is dissolved in 30mL distilled water, is obtained containing iron chloride and magnesium chloride
Mixed solution；Then, in above-mentioned 0~0.02mol of mixed solution and dripping Na2Si3O7Solution (Na2Si3O7The concentration of solution
Mixed material is put into baking oven, keeps the temperature 4 at 200 DEG C 10%), to add 1.3mol sodium hydroxide after stirring 30 minutes
Hour；It is obtained after centrifugation, washing, drying and adds different Na2Si3O7With MgCl2·6H2α-the Fe of O amount2O3Microplate.
Step 2, the different amounts of MgCl of above-mentioned addition is calculated2·6H2O and Na2Si3O7Obtained regular hexagon α-Fe2O3It is micro-
The draw ratio of piece, draw ratio are inscribed diameter of a circle divided by thickness (d/t)；According to α-Fe2O3The SEM photograph of particle obtains positive six
The ratio of side shape thin slice inscribed circle diameter (d) and hexagonal foil thickness (t), to make the molar ratio and just of different Fe and Si
The graph of relation of hexagonal foil inscribed circle diameter (d) and regular hexagon sheet thickness (t).Draw ratio is bigger, respectively to different
Property is better, and the absorbing property of composite material obtained is better.
MgCl2And Na2SiO3It will form a kind of silicate, this silicate after reaction system is added as surfactant
The surface that regular hexagon crystal grain can be adhered to can prevent intercrystalline aggregation, and it is promoted to grow along a certain crystal face, improve crystal grain
Draw ratio.
Fig. 1 is α-Fe made from the embodiment of the present invention 12O3With Fe3O4X ray diffracting spectrum, it will be seen from figure 1 that institute
α-the Fe of preparation2O3With Fe3O4Crystallinity is high, purity is high.
Fig. 2 a~Fig. 2 d is α-Fe made from embodiment 12O3The SEM photograph of particle can be seen that α-from Fig. 2 a~Fig. 2 b
Fe2O3Microplate size uniformity, morphological rules；It can be seen that α-Fe from Fig. 2 c2O3Microplate is regular hexagon, and regular hexagon is inscribed
Circular diameter is about 1.8 μm；It can be seen that α-Fe from Fig. 2 d2O3The thickness of microplate is about 120nm.
Fig. 3 is Fe obtained made from embodiment 13O4The SEM photograph of particle, from figure 3, it can be seen that Fe3O4Microplate size
Uniform, morphological rules, the inscribed circle diameter of regular hexagon are about 1.8 μm.
Fig. 4 a is Fe made from embodiment 13O4(compactedness is the graph of relation of the complex dielectric permittivity of particle and frequency
70wt%).It can be seen that possessing more appropriate complex dielectric permittivity.
Fig. 4 b is Fe made from embodiment 13O4(compactedness is the graph of relation of the complex permeability of particle and frequency
70wt%).It can be seen that possessing higher complex permeability.Illustrate that platelet morphology increases the anisotropy (major diameter of material
Than), to improve its magnetic conductivity.
Fig. 4 c is Fe made from embodiment 13O4(compactedness is the graph of relation of the dielectric loss of particle and frequency
70wt%).
Fig. 4 d is Fe made from embodiment 13O4(compactedness is the graph of relation of the magnetic loss of particle and frequency
70wt%).It can be seen that possessing higher magnetic loss.Illustrate that the magnetic loss of above-mentioned absorbing material increases.
Fig. 5 is Fe made from embodiment 13O4The reflection loss figure of particle.As can be seen that it possesses excellent electromagnetic absorption
Characteristic.Under 5mm thickness, reflection loss peak is -41.67dB.
Fig. 6 is that embodiment 2 obtains the molar ratio and regular hexagon thin slice inscribed circle diameter (d), thickness (t) of different Fe and Si
Graph of relation.As can be seen that the increase of the molar ratio with Fe and Si, regular hexagon thin slice inscribed circle diameter (d) can subtract
Small, the draw ratio (d/t) of regular hexagon thin slice will increase.Illustrate Na2Si3O7With MgCl2·6H2The addition of O will affect α Fe2O3
The growth of crystal grain can control α-Fe2O3The pattern and size of crystal grain.
Electromagnetic-wave absorbent of the invention has the pattern of regular hexagon sheet, on the one hand makes it have biggish respectively to different
Property, enhance Fe3O4The interfacial polarization of particle, so that the magnetic loss of absorbing material be made to increase, absorbing property is improved；On the other hand,
Since the demagnetizing factor of flaky material is smaller, to make sheet absorbing material Effective permeability with higher, absorbing property compared with
It is good.It is preparation method simple process of the invention, at low cost, without complicated synthesis device, without using the chemical reagent of severe toxicity,
It is suitable for large-scale industrial production.
Claims (6)
1. one kind has anisotropic magnetic iron ore electromagnetic-wave absorbent, it is characterised in that: the magnetic iron ore electromagnetic-wave absorbent
Structure, the shape of every crystal grain are regular hexagon to crystal grain in the form of sheets.
2. according to claim 1 have anisotropic magnetic iron ore electromagnetic-wave absorbent, it is characterised in that: every positive six
The inscribed circle diameter of side shape crystal grain is 1.75~1.8 μm.
3. a kind of preparation method described in claim 1 with anisotropic magnetic iron ore electromagnetic-wave absorbent, feature exist
In comprising the following steps:
Step 1, regular hexagon α-Fe is prepared2O3: Na is added into the mixed solution containing iron chloride and magnesium chloride2Si3O7Solution
And NaOH, after reaction, separating, washing product obtains the α-Fe in regular hexagon2O3；
Step 2, regular hexagon Fe is prepared3O4: the α-Fe that step 1 is obtained2O3The mixed atmosphere of hydrogen and argon gas protection under into
Row heat treatment, obtains having anisotropic regular hexagon magnetic iron ore electromagnetic-wave absorbent.
4. the preparation method according to claim 3 with anisotropic magnetic iron ore electromagnetic-wave absorbent, feature exist
In: in step 1, reaction temperature is 190~200 DEG C, and the reaction time is 3.5~4 hours.
5. the preparation method according to claim 3 with anisotropic magnetic iron ore electromagnetic-wave absorbent, feature exist
In: in step 2, in mixed atmosphere, the quality accounting of argon gas is 95%, and the quality accounting of hydrogen is 5%.
6. the preparation method according to claim 3 with anisotropic magnetic iron ore electromagnetic-wave absorbent, feature exist
In: in step 2, heat treatment temperature is 750~800 DEG C, and heat treatment time is 1.5~2 hours.
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Application publication date: 20190809 |