CN107660111A - A kind of preparation method of amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material - Google Patents
A kind of preparation method of amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material Download PDFInfo
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- CN107660111A CN107660111A CN201610518745.6A CN201610518745A CN107660111A CN 107660111 A CN107660111 A CN 107660111A CN 201610518745 A CN201610518745 A CN 201610518745A CN 107660111 A CN107660111 A CN 107660111A
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- ferrite
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- molten drop
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Abstract
The invention discloses a kind of preparation method of amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material.Using autoreaction extinguishing method, first with Fe+Fe2O3+Li2CO3+ ZnO is main reaction system, with Bi2O3For fluxing agent, KClO4For nutritional agents, sucrose is carburization agent, and epoxy resin is binding agent, prepares high energy reunion powder.Then fusing is allowed to using the injection of self- propagating flame gun and concurrently gives birth to SHS process reaction, produce atomized droplet, rapid quench realizes that very large super cooling degree cools down into the 15wt.%NaCl aqueous solution, on the one hand suppress the formation of nucleus and grow up, on the other hand make sucrose, gas caused by Epoxy burns have little time to escape and be retained in inside molten drop, ultimately form the amorphous li Zn ferrite cenosphere with hollow structure.Present device is simple, technique is flexible, cost is cheap, can obtain amorphous structure, while traditional lithium-zinc-ferrite lighting is realized, effectively improves its low frequency absorbing property, has certain application potential in military and civilian industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material, belong to electromagnetism
Field of functional materials.
Background technology
Stealth technology is the development and extension of conventional camouflage technological direction high-tech, existence and work for modern armament
The influence of war ability constantly increases, and this requires to apply the absorbing material that can largely absorb high band radar wave, therefore, both at home and abroad
Main research fund and human resources is focused primarily upon in high frequency absorbing material (8-20GHz) research and development, and the research is increasingly
Maturation, and the research of below 8GHz low-frequency wave-absorbing material then lacks relatively, is not only difficult to meet military big wavelengths of electromagnetic
Shielding demand, the significant problem hidden danger of civilian aspect also be present.
Lithium-zinc-ferrite raw material is cheap, and wide material sources, simple production process are stable, in having rectangular hysteresis loop, being in
The features such as temperature, remanent magnetism are low to stress sensitivity, temperature stability is good, good gyromagnet and square material is not only, and it is a kind of
The soft magnetic ferrite applied in 0.5-8GHz low-frequency ranges, current domestic loyal, Jiang Hong et al. that had a surplus have studied lithium zinc
After ferritic preparation and absorbing property, external Gruskova et al. have studied the substitution of the elements such as lithium-zinc-ferrite Ti, Bi, Mn
Low frequency absorbing property.As other ferrites, lithium-zinc-ferrite similarly has that frequency band is narrow, density is big, matching thickness is big, low
Frequency absorbs the features such as ripple performance is difficult to regulation and control, it is difficult to meets the suction ripple requirement of modern stealthy field " thin, light, wide, strong ".
Compared with traditional crystalline material, non-crystalline material resistivity is high, has high saturation magnetization, is that one kind has
Low frequency inhales the novel wave-absorbing material of ripple potentiality.This patent is intended to prepare amorphous li Zn ferrite by special process method hollow
Microballon, while the traditional lithium-zinc-ferrite density of solution is big, it is effectively improved its low frequency absorbing property.
The content of the invention
The technical problems to be solved by the invention are to found amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material
Preparation method.For this method using the raw material of low cost, easy equipment and easy technique, the low frequency for preparing lighting inhales ripple
The amorphous li Zn ferrite cenosphere of excellent performance.
To achieve these goals, the present invention uses following technical scheme：
1 with Fe powder, Li2CO3Powder, ZnO powder, Fe2O3Powder, KClO4Powder, Bi2O3Powder, sucrose and epoxy resin are prepared for raw material
Function reunion powder.
Reunion powder is introduced into the oxyacetylene torch field of self- propagating spray gun and carries out meltallizing by 2, makes reunion powder in flight course
Rapid that self-propagating reaction occurs, exothermic heat of reaction makes system temperature along with the double action of high temperature oxyacetylene torch (about 3500K)
More than reaction product fusing point and form molten drop, while the organic matter such as epoxy resin and sucrose high-temp combustion produces a large amount of gases.
3 will realize that very large super cooling degree cools down in the molten drop injection 15wt.%NaCl aqueous solution, make gas have little time to escape and protect
Stay in inside molten drop, final fabricated in situ has the amorphous state microballon of hollow-core construction.Because NaCl can be separated out on molten drop surface
And burst, steam blanket is destroyed, the cooling of molten drop is entered the bubble boiling stage in advance, when significantly shorten the cooling of molten drop
Between, and then the cooldown rate of its molten drop is greatly improved, molten drop is formd very large super cooling degree in cooling procedure, cause crystallization to drive
Power increases, while the formation of nucleus and grows up and receive obvious suppression, and the formation for amorphous state cenosphere provides heating power
And dynamic conditions.In this experiment, self-propagating reaction is lighted by the high temperature of flame field, reaction one is ignited, can be certainly
I maintains, and provides energy without the external world, flame field only plays a part of melting reunion powder and promoting melting drop.
The amorphous li Zn ferrite cenosphere of acquisition such as is successively filtered, collected, being dried at the step by 4, and is used
Ultrasonic disperse avoids its reunion, finally obtains finished product.
Above-mentioned amorphous li Zn ferrite cenosphere finished product is carried out electromagnetic parameter survey by 5 on network vector analyzer
It is fixed, and reflectance curve is calculated by matlab softwares, obtain low frequency absorbing property.
The present invention can pass through the group of adjustment during amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material is prepared
Poly- powder size, the liquid dissolved drip of volume-tunable is obtained, the final amorphous state cenosphere absorbing material for obtaining size tunable；It can lead to
Cross and select suitable foaming agent, adjust the modes such as its addition, progress are suitably modified and a variety of foaming agents are compound, adjust its hair
Tolerance, realize the regulation and control to hollow-core construction.Present device is simple, technique is flexible, strong adaptability, reaction raw materials and manufacture are run
Cost is cheap.Method involved in the present invention can be applied to the system of low-frequency wave-absorbing material required in military and civilian industry
It is standby.
Brief description of the drawings
Fig. 1 is the general principle figure that the technology of the present invention prepares amorphous li Zn ferrite cenosphere.
Fig. 2 is that amorphous li Zn ferrite cenosphere SEM made from the technology of the present invention schemes.
Fig. 3 is amorphous li Zn ferrite cenosphere XRD analysis figure made from the technology of the present invention.
Fig. 4 is amorphous li Zn ferrite cenosphere transmission electron microscope SEAD figure made from the technology of the present invention.
Fig. 5 is that amorphous li Zn ferrite cenosphere suction ripple sample reflects under different-thickness made from the technology of the present invention
Rate curve map.
Embodiment
In order to be better understood from the present invention, present disclosure will be further elucidated by the following examples.Following examples
Invention rather than limitation of the invention further are intended to illustrate, those skilled in the art is according to the content of the invention described above
Some nonessential modifications and adaptations are made, belong to the scope of the present invention.
The determination of 1 raw material proportioning：Used raw material using molar ratio computing as：Fe powder 0.94mol, Fe2O3Powder 0.705mol,
Li2CO3Powder 0.175mol, ZnO powder 0.3mol, KClO4Powder 0.47mol, Bi2O3Powder 0.01mol, sucrose 0.35mol, epoxy resin
0.4mol。
2 preparations containing the powder that can reunite：
(1) it is standby by above-mentioned various raw materials balance precise；
(2) load weighted raw material is sequentially placed into ball grinder, adds suitable alcohols, ball milling 6-8h；
(3) pour into container to be placed under agitator after the completion of ball milling and stir, then epoxy resin is poured into beaker and added
Alcohol stirs, until epoxy resin is stirred into emulsion form, slowly pours into container, stirs 1-2h；
(4) material being stirred is put into oven for drying, temperature is maintained at 110-120 DEG C, time 2-3h；
(5) after the completion of drying, oven temperature is adjusted to 190-210 DEG C and is carbonized, time 4-6h；
(6) after the completion of being carbonized, blocking material is taken out, is put into Universalpulverizer and crushes, it is 40- that screening, which obtains particle diameter,
70 μm of reunion powder is stand-by.
3 flame reaction meltallizings and cooling：
(1) oxygen, acetylene, nitrogen sebific duct are connected to each corresponding interface of flame gun exactly respectively, check that each interface is
Whether no gas leakage, muzzle block with feed opening；
(2) after inspection is errorless, the reunion powder that step 2 is prepared introduces blanking device, and regulation oxygen pressure is 0.5-
0.6MPa, acetylene 0.11MPa, after nitrogen is 0.4-0.5MPa, igniting, holding flame is micro-carbon flame, opens blanking device, right
Container equipped with 15wt.%NaCl solution carries out meltallizing, and inclination angle is 45 °, at the same time opens cooling system to meltallizing product
Cooled down.
The acquisition of 4 amorphous li Zn ferrite cenosphere absorbing materials：
(1) after treating step 3 meltallizing, emptying cooling medium, meltallizing product is collected；
(2) meltallizing product is dried, and it is disperseed to prevent from reuniting in ultrasonic disperse instrument, final sieving obtains certain particle diameter
Amorphous li Zn ferrite cenosphere absorbing material.
Particle diameter, pattern, phase structure and the suction ripple of amorphous li Zn ferrite cenosphere absorbing material prepared by the present invention
Performance is as follows：Particle diameter distribution is uniform, concentrates on 40 μm or so, includes solid, single hole and porous type various structures, and small part
Irregular particle.Cenosphere surface smoother, occur without obvious crystal grain.XRD curve substrates are higher, without sharp diffraction
Peak, only exist " steamed bun peak " of widthization, it was demonstrated that material is amorphous state；Transmission electron microscope SEAD pattern is to disperse
Halo, without it is any sign periodic structure spot and bright and sharp striped, further testimonial material be amorphous state.This is hollow micro-
Pearl low frequency absorbing property is good：Best match thickness is 2mm, and under the thickness, the minimum reflectivity of sample is -29.8dB, right
It is 7.1GHz to answer frequency, and the absorption band less than -10dB is 5.3-10.3GHz, and bandwidth reaches 5GHz.
Claims (4)
1. amorphous li Zn ferrite cenosphere absorbing material, it is characterised in that using autoreaction extinguishing method, select specific
Lithium-zinc-ferrite reaction system, good fluidity, the function reunion state powder of uniform component are prepared, and introduce the spray of self- propagating flame
Rifle, SHS reactions occur during meltallizing, under exothermic heat of reaction and the double action of flame high temperature, the reaction fusing life of reunion powder
Into ceramic droplet, while gas is produced, subsequently enter and supper-fast solidification is realized in the 15wt.%NaCl aqueous solution, gas is come not
And effusion is retained in inside molten drop, finally gives the amorphous li Zn ferrite cenosphere absorbing material with hollow structure,
It is the efficient low-frequency wave-absorbing material of a kind of novel light.
2. reaction system according to claim 1, it is characterised in that amorphous li zinc-iron is prepared using autoreaction extinguishing method
Oxysome cenosphere low-frequency wave-absorbing material, used composition of raw materials and mol ratio are：
。
3. reaction system according to claim 1, it is characterised in that carried out from the 15wt.%NaCl aqueous solution to molten drop cold
But, because under the concentration conditions, the cooldown rate of NaCl solution is maximum, when continuing to increase concentration to 20.wt%, cooldown rate meeting
Drastically reduce.When the high temperature molten drop that autoreaction extinguishing method obtains enters the solution, NaCl can be separated out and burst on molten drop surface,
Steam blanket is destroyed, the cooling of molten drop is entered the bubble boiling stage in advance, significantly shorten the cool time of molten drop, Jin Erji
The cooldown rate of its molten drop is improved greatly, molten drop is formd very large super cooling degree in cooling procedure, is caused crystallization driving force to increase,
The formation of nucleus simultaneously and grow up and receive obvious suppression, these provide thermodynamics and kineticses condition for the formation of amorphous.
4. specific lithium-zinc-ferrite reaction system according to claim 1, it is characterised in that addition Bi2O3It can suppress
Crystal grain is grown up, and crystal boundary inside ferrite be present, inner ion spreads difficulty to plane of crystal, therefore the volatilization of lithium ion is by larger
Restriction, ensure there is enough lithium ion to participate in SHS reactions.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113305293A (en) * | 2021-04-13 | 2021-08-27 | 河北工业职业技术学院 | Preparation method of amorphous hollow microsphere electromagnetic wave absorption material |
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Application publication date: 20180202 |