CN106633547A - Z-shaped ferrite flaky powder/PVDF (polyvinylidene fluoride) wave absorption composite material and preparation method thereof - Google Patents

Z-shaped ferrite flaky powder/PVDF (polyvinylidene fluoride) wave absorption composite material and preparation method thereof Download PDF

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CN106633547A
CN106633547A CN201611162387.6A CN201611162387A CN106633547A CN 106633547 A CN106633547 A CN 106633547A CN 201611162387 A CN201611162387 A CN 201611162387A CN 106633547 A CN106633547 A CN 106633547A
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pvdf
flaky powder
powder
bafe
preparation
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CN106633547B (en
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林营
刘潇
戴菁菁
杨海波
韩宁
王幸
孙雨佳
高淑雅
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Xi'an Function Material Co., Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a Z-shaped ferrite flaky powder/PVDF (polyvinylidene fluoride) wave absorption composite material and a preparation method thereof. PVDF powder is added into acetone; after the dissolution, a PVDF solution is obtained; then, Ba3Co2Fe24O41 flaky powder with the orientation in the (001) direction is added; after uniform mixing, compound slurry is obtained; the compound slurry is subjected to tape casting; the Z-shaped ferrite flaky powder/PVDF wave absorption composite material is obtained. A tape casting process is used; the material dispersion is uniform; the membrane thickness is uniform; the prepared tape casting slurry has no toxicity and cannot cause harm to the human body. The equipment is simple; the process is stable; the continuous operation can be realized; the production efficiency is high; high-degree automation can be realized; the cost is reduced; the material compactness and the uniformity are good; the preparation method is simple.

Description

A kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials and preparation method thereof
Technical field
The invention belongs to material science, be related to a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials and Its preparation method.
Background technology
With developing rapidly for electronic technology, radar and the communication technology, electromagenetic wave radiation has become after noise pollution, air Another big public hazards after pollution, water pollution, solid waste pollution.The electromagnetic interference (EMI) that electromagenetic wave radiation is produced not only can The normal operation of various electronic equipments is affected, and also has harm to the healthy of the mankind.Therefore, electricity of good performance is developed Electromagnetic wave shielding material, evolution electromagnetic environment have very urgent scientific meaning and reality need.Traditional absorbing material has to be inhaled The shortcomings of wave energy power is weak, density big, suction wave frequency band is narrow, it is impossible to meet the requirement of novel wave-absorbing material " thin, light, wide, strong ".Cause This, while improving and optimizating traditional absorbing material, does one's utmost to explore the focus that advanced composite material (ACM) is current absorbing material research. Composite is that the trend of modern material development realizes that performance complement and optimization are expected preparative by the compound of multiple material function Can excellent Materials Inorganic magnetic-composite membrane of polymer material be Polymer-based Magnets research and the form applied it One main being exactly combined the polymeric matrix such as ferrite and terres rares permanent magnetic powder and resin takes physically or chemically means system Film forming.
Absorbing material needs to meet two principles：Impedance matching, electromagnetic wave incident is maximum to energy during material surface Into material internal；Attenuation characteristic, the electromagnetic wave into material needs rapid effectively decay.Ferrite is research using more It is extensive a kind of, the research of inorganic magnetic and the multiple correlation of organic matter a lot, its single ferritic reflection loss Little, frequency bandwidth is narrow, and in order to improve its absorbing property, the method mainly taken is that chemically composited method (has two or more Ferrite or ferrite and conductive bluk recombination), easily there is chemical reaction in its complicated process of preparation in recombination process, Interfacial effect is complicated.
The content of the invention
It is an object of the invention to provide a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials and its preparation side Method, and obtained absorbing material, due to interfacial effect and impedance optimization, the composite wave-suction material has excellent absorbing property, Maximum reflection loss reaches -31.03dB, and preparation process is simple.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of Z- type ferrites flaky powder/PVDF Wave suction composite materials, comprises the following steps：
Step 1：PVDF powders are added in acetone, PVDF solution is obtained after dissolving, be subsequently adding in (001) direction tool There is the Ba of orientation3Co2Fe24O41Flaky powder, is well mixed, and obtains composite mortar；Wherein, by mass percentage, in (001) Direction has the Ba of orientation3Co2Fe24O41Flaky powder is (5%～20%) with the mass ratio of PVDF powders：(80%～ 95%)；
Step 2：Composite mortar is cast, Z- type ferrites flaky powder/PVDF Wave suction composite materials are obtained.
The present invention's is further improved by, and the temperature of acetone is 40～50 DEG C.
The present invention's is further improved by, and PVDF powders are 1 with the mass ratio of acetone:4.
The present invention's is further improved by, and 200-250 μm of the height of scraper is cast during curtain coating.
The present invention's is further improved by, and (001) direction has the Ba of orientation3Co2Fe24O41Flaky powder by with It is prepared by lower process：
Step 1：Will be according to BaFe12O19In mol ratio weigh BaCO respectively3、Fe2O3And fused salt ball milling mixing is equal It is even, 2～4h is then incubated at 1150～1200 DEG C, obtain BaFe12O19Presoma；
Step 2：By Fe2O3And BaCl2.2H2O mixes, and is subsequently adding BaFe12O19Presoma, after ball milling mixing is uniform, 6～10h is incubated at 1200～1250 DEG C, the BaFe that there is orientation in (001) direction is obtained12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2.2H2The 5～10% of O gross masses； BaCl2.2H2The addition of O is Fe2O32～3 times of quality；
Step 3：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to mol ratio:1 mixes Close, at the same add fused salt, be uniformly mixed, at 1250～1300 DEG C, be incubated 6～10h, obtain (001) direction have take To Ba3Co2Fe24O41Flaky powder, is designated as (001) Ba3Co2Fe24O41Flaky powder.
The present invention's is further improved by, and fused salt is NaCl in step 1, and the quality of NaCl is BaCO3With Fe2O3Always 1～2 times of quality.
The present invention's is further improved by, and fused salt is NaCl in step 3, and the quality of NaCl is random Ba2Co2Fe12O22Powder and (001) BaFe12O191～2 times of flaky powder gross mass.
The present invention's is further improved by, random Ba2Co2Fe12O22Powder is prepared by the following method：
By chemical formula formula by Ba2Co2Fe12O22Analytically pure CoO, BaCO3、Fe2O3It is mixed by 20～24h of ball milling after preparation Close uniform, then dry, sieve, briquetting, then 1230～1270 DEG C of Jing pre-burnings 3～6 hours, blocks of solid is obtained, then by block Shape solid crosses 120 mesh sieves and obtains Ba after crushing2Co2Fe12O22Powder.
A kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials, it is characterised in that the chemical table of the composite It is x (001) Ba up to formula3Co2Fe24O41/ (1-x) PVDF, wherein x are (001) Ba3Co2Fe24O41The mass percent of sheet, and 5%≤x≤20%.
Compared with prior art, the present invention adopts hexad ferrite Ba3Co2Fe24O41As absorbing material, and sheet-shaped The absorbing property of looks is more excellent compared to graininess, while PVDF is not only as electromagnetic wave transparent material, but also is a kind of dielectric Material, using the teaching of the invention it is possible to provide dielectric loss so that composite had both had magnetic loss, and with dielectric loss, met impedance matching, reached To excellent wave-absorbing effect.The present invention is prepared for (001) Ba by molten-salt growth method first3Co2Fe24O41Flaky powder, then passes through Organic matter dissolving PVDF powders after mechanical mixture carry out two be combined, wherein, x be (001) Ba3Co2Fe24O41The matter of flaky powder Amount percentage, and 5%≤x≤35%, after flow casting molding, are obtained excellent (001) Ba of absorbing property3Co2Fe24O41Flaky powder The absorbing material of filling PVDF matrixes.The present invention adopts casting technique, and material dispersion is uniform and thickness of film is homogeneous, and makes Standby casting slurry used is non-toxic, and human body will not be damaged.Present device is simple, and process stabilizing can be operated continuously, Production efficiency is high, is capable of achieving increasingly automated, reduces cost, material compactness and has good uniformity, and preparation method letter It is single.
The uniformity of obtained curtain coating thick film of the invention preferably, makes flaky powder uniformly be laid on casting films band.When (001)Ba3Co2Fe24O41The mass fraction of flaky powder is 20%, and when mass fraction is 80%, saturation magnetization is 7.15emu/g, remanent magnetization is 1.57emu/g, and preferably, absorption maximum can reach -21.2dB to absorbing property, -10dB with Under absorption band width be 4GHz.
Further, sheet Ba is prepared using molten-salt growth method in the present invention3Co2Fe24O41, prepared by the tape casting beneficial to the later stage x(001)Ba3Co2Fe24O41/ (1-x) PVDF absorbing materials, absorbing material good dispersion prepared by the method, thickness is uniform, causes Close property is good and can generate on a large scale.
Description of the drawings
Fig. 1 is (001) Ba prepared by molten-salt growth method3Co2Fe24O41Flaky powder, the XRD obtained by 1300 DEG C of sintering.
Fig. 2 is to work as Ba3Co2Fe24O41Mass percent when to be 5%, PVDF mass percents be 95%, curtain coating gained is multiple The SEM figures of condensation material.
Fig. 3 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percents be 80% when, curtain coating gained The SEM figures of composite.
Fig. 4 is to work as Ba3Co2Fe24O41Mass percent when to be 5%, PVDF mass percents be 95%, curtain coating gained is multiple The hysteresis curve of condensation material.
Fig. 5 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percents be 80% when, curtain coating gained The hysteresis curve of composite.
Fig. 6 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percents be 95%, thickness be 2mm when, The reflection loss figure of curtain coating gained composite.
Fig. 7 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percents be 95%, thickness be 3mm when, The reflection loss figure of curtain coating gained composite.
Fig. 8 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percents be 95%, thickness be 4mm when, The reflection loss figure of curtain coating gained composite.
Fig. 9 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percents be 90%, thickness is 2mm When, the reflection loss figure of curtain coating gained composite.
Figure 10 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percents be 90%, thickness is 3mm When, the reflection loss figure of curtain coating gained composite.
Figure 11 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percents be 90%, thickness is 4mm When, the reflection loss figure of curtain coating gained composite.
Figure 12 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percents be 85%, thickness is 2mm When, the reflection loss figure of curtain coating gained composite.
Figure 13 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percents be 85%, thickness is 3mm When, the reflection loss figure of curtain coating gained composite.
Figure 14 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percents be 85%, thickness is 4mm When, the reflection loss figure of curtain coating gained composite.
Figure 15 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percents be 80%, thickness is 2mm When, the reflection loss figure of curtain coating gained composite.
Figure 16 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percents be 80%, thickness is 3mm When, the reflection loss figure of curtain coating gained composite.
Figure 17 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percents be 80%, thickness is 4mm When, the reflection loss figure of curtain coating gained composite.
Specific embodiment
Below in conjunction with the accompanying drawings by specific embodiment, the present invention is described in detail.
The Ba obtained after curtain coating3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials are film, by film together with film strips In being put into vacuum drying chamber, under conditions of 200 DEG C, 5min is dried, then ice-water bath chilling 2min, it is vacuum drying at 200 DEG C During, PVDF has the process of a phase transformation, while by way of the chilling in ice bath 2min, beneficial to the demoulding and densification； Then it is dried, lamination is tested after hot pressing.Wherein, the temperature of hot pressing be 150～180 DEG C, pressure be 0.5～1MPa, pressurize Time is 30s～1min.
In the present invention it is compressing specifically by the casting films folded as in mould, hot pressing and pressurize one minute.
Embodiment 1
(1) by BaCO3, Fe2O3, after NaCl electronic balances are accurately weighed, in being placed on ball grinder, it is sufficiently mixed It is even, take out dry for standby.Wherein BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1, BaCO3With Fe2O3Amount press According to pressing chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, the rotating speed of ball mill For 500r/min, ball milling 18h, in an oven to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh sieves to temperature.
(2) raw material prepared is obtained into BaFe in 1150 DEG C of pre-burning 4h12O19Presoma, is then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed totally.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then in 1200 DEG C of calcinings 10h, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing is filtered, and is dried to obtain sheet (001) BaFe12O19Flaky powder, It is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The addition of O is Fe2O32 times of quality；BaFe12O19Forerunner The quality of body is BaCl2.2H2O、Fe2O3And BaFe12O19The 5% of presoma gross mass.
(4) by chemical general formula Ba2Co2Fe12O22, by BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, placement The ball milling 24h in ball grinder, then dries, and sieves, briquetting, and 6h is then incubated at 1230 DEG C into phase, crosses 120 mesh sieve, obtains To random Ba2Co2Fe12O22Powder, is designated as Co2Y。
By the random Ba for obtaining2Co2Fe12O22Powder and above-mentioned (001) BaFe for preparing12O19Powder is according to mol ratio For 1:1 mixing, adds NaCl, and electric stirring mixing 12h, the quality that NaCl is added is equal to random Ba2Co2Fe12O22Powder with (001)BaFe12O19Powder quality summation, being incubated 10h at 1250 DEG C makes oxide carry out abundant fused salt reaction, then with heat Ultra-pure water is washed, and until sodium chloride is washed clean, is filtered, and is dried, and obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) 1g PVDF powders are poured into the acetone of 4g, in the environment of 50 DEG C of magnetic agitations, 3h is stirred, it is clear to liquid Clearly, it is completely dissolved PVDF powders, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composites：To in the 1g PVDF solution being uniformly dissolved Add (001) Ba of 0.05g3Co2Fe24O41Flaky powder, by electric stirring 8h, obtains composite mortar；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing materials, scraper Height be adjusted to 200mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=5%.
(8) by the thick film of flow casting molding, during 200 DEG C of vacuum drying chamber is put at once, in ice-water bath chilling after 5min 2min。
(9) after the demoulding, it is dried, by thick film lamination, hot pressing cyclization, 150 DEG C of heating-up temperature, pressurize 0.5MPa, pressurize 60s.
Jing tests prove (001) Ba for preparing3Co2Fe24O41/ PVDF absorbing materials, flaky powder spreads in PVDF, There is excellent absorbing property in the range of 2-18GHz.
It will be seen from figure 1 that the Ba for preparing3Co2Fe24O41Generate without dephasign, the oriented growth on (001) direction.
Figure it is seen that the Ba for preparing3Co2Fe24O41Random powder is generated without dephasign.
From fig. 4, it can be seen that the composite for preparing has obvious ferromagnetism, saturation magnetization is 6.3emu/g.
From fig. 6, it can be seen that thickness of composite material is 2.0mm, and in 10.5GHz, maximum reflection loss -11.3dB, - The absorption band width of below 10dB is 1.0GHz (10.4～11.0GHz).
From figure 7 it can be seen that thickness of composite material is 3.0mm, and in 10.2GHz, maximum reflection loss -31.8dB, - The absorption band width of below 10dB is 1.0GHz (10.0～11.0GHz).
From figure 8, it is seen that thickness of composite material is 4.0mm, and in 10.0GHz, maximum reflection loss -27.5dB, - The absorption band width of below 10dB is 1.8GHz (9.0～10.8GHz).
Embodiment 2
A kind of Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, the chemical expression of the absorbing material is x (001)Ba3Co2Fe24O41/ (1-x) PVDF, wherein x are (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x= 10%.
Above-mentioned Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, comprises the following steps：
(1) by raw material BaCO3, Fe2O3, it is fully mixed in being placed on ball grinder after NaCl electronic balances are accurately weighed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1.4, BaCO3With Fe2O3Amount according to pressing chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and in an oven to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature Sieve.
(2) raw material prepared is obtained into BaFe in 1170 DEG C of pre-burning 3.5h12O19Presoma.Then with the ultra-pure water of heat Washed, until sodium chloride is washed totally.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 9h at 1220 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing is filtered, is dried to obtain Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The addition of O is Fe2O32.2 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 7%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 23h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 5h into phase at 1240 DEG C, crosses 120 mesh sieves Son, obtains random Ba2Co2Fe12O22Powder, is designated as Co2Y, by the random Ba for obtaining2Co2Fe12O22Powder is prepared with above-mentioned (001)BaFe12O19(as template) is 1 according to mol ratio:1 mixing, adds NaCl electric stirring mixing 14h, and NaCl is added Quality be equal to Ba2Co2Fe12O22Powder and (001) BaFe12O191.2 times of flaky powder quality summation, at 1270 DEG C, insulation 9h makes oxide carry out abundant fused salt reaction, is then washed with the ultra-pure water of heat, until sodium chloride is washed clean, mistake Filter, is dried, and obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) 0.95g PVDF powders are poured into the acetone of 3.8g, in the environment of 48 DEG C of magnetic agitations, 4h is stirred, to liquid Body is clarified, and is completely dissolved PVDF powders, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composites：To the 0.95g PVDF solution being uniformly dissolved According to add 0.1g (001) Ba3Co2Fe24O41Flaky powder, by electric stirring 9h, obtains composite mortar；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing materials, scraper Height be adjusted to 220mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=10%.
(8) by the thick film of flow casting molding, during 200 DEG C of vacuum drying chamber is put at once, in ice-water bath chilling after 5min 2min。
(9) after the demoulding, it is dried, by thick film lamination, hot pressing cyclization, 160 DEG C of heating-up temperature, pressurize 0.6MPa, pressurize 50s.
Jing tests prove (001) Ba for preparing3Co2Fe24O41/ PVDF absorbing materials, flaky powder spreads in PVDF, There is excellent absorbing property in the range of 2-18GHz.
From fig. 9, it can be seen that thickness of composite material is 2.0mm, and in 18GHz, maximum reflection loss -17.1dB.
From fig. 10 it can be seen that thickness of composite material is 2.0mm, and in 11.9GHz, maximum reflection loss -16.3dB, - The absorption band width of below 10dB is 1.2GHz (11.2～12.4GHz).
It can be seen from figure 11 that thickness of composite material is 3.0mm, and in 11.6GHz, maximum reflection loss -16.5dB, - The absorption band width of below 10dB is 3.5GHz (10.0～13.5GHz).
Embodiment 3
Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, the chemical expression of the absorbing material is x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x are (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x=15%.
Above-mentioned Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, comprises the following steps：
(1) by raw material BaCO3, Fe2O3, it is fully mixed in being placed on ball grinder after NaCl electronic balances are accurately weighed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1.6, BaCO3With Fe2O3Amount according to pressing chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and in an oven to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature Sieve.
(2) raw material prepared is obtained into BaFe in 1180 DEG C of pre-burning 3h12O19Presoma.Then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed totally.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 8h at 1240 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing is filtered, is dried, obtains Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The addition of O is Fe2O32.6 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 8%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 21h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 4h into phase at 1250 DEG C, crosses 120 mesh sieves Son, obtains random Ba2Co2Fe12O22Powder, is designated as Co2Y, by the random Ba for obtaining2Co2Fe12O22Powder is prepared with above-mentioned (001)BaFe12O19Powder is 1 according to mol ratio:1 mixing, adds NaCl electric stirring mixing 16h, the quality that NaCl is added Equal to random Ba2Co2Fe12O22Powder and (001) BaFe12O191.4 times of powder quality summation, at 1260 DEG C, insulation 8h makes oxygen Compound carries out abundant fused salt reaction, is then washed with the ultra-pure water of heat, until sodium chloride is washed clean, filters, and is dried, Obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) 0.9g PVDF powders are poured into the acetone of 3.6g, in the environment of 44 DEG C of magnetic agitations, 5h is stirred, to liquid Clarification, is completely dissolved PVDF powders, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composites：To the 0.9g PVDF solution being uniformly dissolved According to add 0.15g (001) Ba3Co2Fe24O41Flaky powder, by electric stirring 10h, obtains composite mortar；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing materials, scraper Height be adjusted to 230mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=15%.
(8) by the thick film of flow casting molding, during 200 DEG C of vacuum drying chamber is put at once, in ice-water bath chilling after 5min 2min。
(9) after the demoulding, it is dried, by thick film lamination, hot pressing cyclization, 170 DEG C of heating-up temperature, pressurize 0.7MPa, pressurize 40s. Jing tests prove (001) Ba for preparing3Co2Fe24O41/ PVDF absorbing materials, flaky powder spreads in PVDF, in 2- There is excellent absorbing property in the range of 18GHz.
It can be recognized from fig. 12 that thickness of composite material is 2.0mm, and in 6.5GHz, maximum reflection loss -20.9dB, - The absorption band width of below 10dB is 0.9GHz (6.2～7.1GHz).
As can be seen from Figure 13, thickness of composite material is 3.0mm, in 6.9GHz, maximum reflection loss -20.5dB, - The absorption band width of below 10dB is 1.3GHz (6.2～7.5GHz).
It is seen from figure 14 that thickness of composite material is 4.0mm, and in 17.6GHz, maximum reflection loss -21.0dB, - The absorption band width of below 10dB is 2.9GHz (6.8～7.3GHz) and (15.6～18GHz).
Embodiment 4
One kind (001) Ba3Co2Fe24O41Flaky powder fills absorbing material of its random powder and preparation method thereof, and it is special Levy and be, the chemical expression of the absorbing material is x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x are (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x=20%.
Above-mentioned (001) Ba3Co2Fe24O41The preparation method of/PVDF absorbing materials, comprises the following steps：
(1) by raw material BaCO3, Fe2O3, it is fully mixed in being placed on ball grinder after NaCl electronic balances are accurately weighed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:2, BaCO3With Fe2O3Amount according to pressing chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and in an oven to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature Sieve.
(2) raw material prepared is obtained into BaFe in 1200 DEG C of pre-burning 2h12O19Presoma.Then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed totally.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 6h at 1250 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing is filtered, is dried, obtains Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The addition of O is Fe2O33 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 10%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 24h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 3h into phase at 1260 DEG C, crosses 120 mesh sieves Son, obtains sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2O's adds Enter amount for Fe2O32 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma is total The 5% of quality.Ba2Co2Fe12O22Powder and above-mentioned (001) BaFe for preparing12O19Powder is 1 according to mol ratio:1 powder, The quality that NaCl electric stirring mixing 16h, NaCl are added is equal to Ba2Co2Fe12O22Powder and (001) BaFe12O19Powder quality 2 times of summation, at 1300 DEG C, insulation 6h makes oxide carry out abundant fused salt reaction, is then washed with the ultra-pure water of heat, directly It is washed clean to sodium chloride, filter, it is dried, obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) 0.85g PVDF powders are poured into the acetone of 3.4g, in the environment of 40 DEG C of magnetic agitations, 6h is stirred, to liquid Body is clarified, and is completely dissolved PVDF powders, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composites：To the 0.85gPVDF solution being uniformly dissolved According to add 0.2g (001) Ba3Co2Fe24O41Flaky powder, by electric stirring 12h, obtains composite mortar；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing materials, scraper Height be adjusted to 250mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite materials, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=20%.
(8) by the thick film of flow casting molding, during 200 DEG C of vacuum drying chamber is put at once, in ice-water bath chilling after 5min 2min。
(9) after the demoulding, it is dried, by thick film lamination, hot pressing cyclization, 180 DEG C of heating-up temperature, pressurize 1MPa, pressurize 30s.
Jing tests prove (001) Ba for preparing3Co2Fe24O41/ PVDF absorbing materials, flaky powder spreads in PVDF, There is excellent absorbing property in the range of 2-18GHz.
From figure 3, it can be seen that (001) Ba3Co2Fe24O41Flaky crystalline grain be 2 μm or so of sheet, Ba3Co2Fe24O41Random powder Crystallite dimension is 50nm～80nm or so, Ba3Co2Fe24O41Content is less, and composite compactness is good.
From fig. 5, it can be seen that the saturation magnetization of composite is 5.05emu/g, remanent magnetization is 1.08emu/g, coercive field is 355.89Oe.
It can be seen from fig. 15 that thickness of composite material is 2.0mm, and in 18GHz, maximum reflection loss -10.5dB.
As can be seen from Figure 16, thickness of composite material is 3.0mm, in 13.2GHz, maximum reflection loss -21.3dB, - The absorption band width of below 10dB is 1.4GHz (12.8～14.2GHz).
As can be seen from Figure 17, thickness of composite material is 4.0mm, in 11.5GHz, maximum reflection loss -20.0dB, - The absorption band width of below 10dB is 3.8GHz (10.5～14.3GHz).
Hexagonal crystal system magnetic lead-type ferrite absorbing property is best, firstly because hexagonal crystal system magneto-plumbite type ferrite has piece Shape structure, and sheet is the optimum shape of absorbent；Secondly, hexagonal crystal system magneto-plumbite type ferrite have higher magnetic respectively to Different in nature equivalent field, thus have the optimum shape that higher natural resonant frequency sheet is absorbent.Found by Robert et al. Excellent magnetic property is shown after hexagonal barium ferrite oriented growth in (001) direction.Simultaneously PVDF has good dielectricity Can, hexagonal barium ferrite is dispersed in PVDF matrixes, forms composite by way of flow casting molding afterwards, is prepared Composite had both had magnetic loss but also with dielectric loss, so that composite has excellent absorbing property, while curtain coating PVDF can replace prior paraffin material simultaneously as electromagnetic wave transparent material in the composite for obtaining afterwards, it is to avoid paraffin and powder Uneven mixing.
The present invention prepares x (001) Ba by the tape casting3Co2Fe24O41/ (1-x) PVDF thick films, wherein, x is (001) Ba3Co2Fe24O41Mass percent, and 5%≤x≤20%, then by organic matter and orientation (001) Ba3Co2Fe24O41's Flaky powder and PVDF powder ball milling mixings, curtain coating, hot pressing is then discharged out organic matter, is prepared using molten-salt growth method in the present invention (001)Ba3Co2Fe24O41Flaky powder, using the tape casting the thick film of directional profile is prepared, then anxious after vacuum drying Cold, demoulding is hot-forming to prepare Both ring sam.Production efficiency of the present invention is high, and automatization level is high, can be mass-produced, and is obtained The absorbing property of composite is excellent.

Claims (9)

1. a kind of preparation method of Z- type ferrites flaky powder/PVDF Wave suction composite materials, it is characterised in that including following step Suddenly：
Step 1：PVDF powders are added in acetone, PVDF solution are obtained after dissolving, be subsequently adding (001) direction have take To Ba3Co2Fe24O41Flaky powder, is well mixed, and obtains composite mortar；Wherein, by mass percentage, in (001) direction Ba with orientation3Co2Fe24O41Flaky powder is (5%～20%) with the mass ratio of PVDF powders：(80%～95%)；
Step 2：Composite mortar is cast, Z- type ferrites flaky powder/PVDF Wave suction composite materials are obtained.
2. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 1, its It is characterised by, the temperature of acetone is 40～50 DEG C.
3. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 1, its It is characterised by, PVDF powders are 1 with the mass ratio of acetone:4.
4. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 1, its It is characterised by, 200-250 μm of the height of scraper is cast during curtain coating.
5. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 1, its It is characterised by, (001) direction has the Ba of orientation3Co2Fe24O41Flaky powder is prepared by procedure below：
Step 1：Will be according to BaFe12O19In mol ratio weigh BaCO respectively3、Fe2O3And fused salt ball milling mixing is uniform, so It is incubated 2～4h at 1150～1200 DEG C afterwards, obtains BaFe12O19Presoma；
Step 2：By Fe2O3And BaCl2·2H2O mixes, and is subsequently adding BaFe12O19Presoma, after ball milling mixing is uniform, 1200 6～10h is incubated at～1250 DEG C, the BaFe that there is orientation in (001) direction is obtained12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2·2H2The 5～10% of O gross masses； BaCl2·2H2The addition of O is Fe2O32～3 times of quality；
Step 3：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to mol ratio:1 mixing, while Fused salt is added, is uniformly mixed, at 1250～1300 DEG C, be incubated 6～10h, obtain that there is orientation in (001) direction Ba3Co2Fe24O41Flaky powder, is designated as (001) Ba3Co2Fe24O41Flaky powder.
6. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 5, its It is characterised by, fused salt is NaCl in step 1, and the quality of NaCl is BaCO3With Fe2O31～2 times of gross mass.
7. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 5, its It is characterised by, fused salt is NaCl in step 3, and the quality of NaCl is random Ba2Co2Fe12O22Powder and (001) BaFe12O19Sheet 1～2 times of powder gross mass.
8. the preparation method of a kind of Z- type ferrites flaky powder/PVDF Wave suction composite materials according to claim 1, its It is characterised by, random Ba2Co2Fe12O22Powder is prepared by the following method：
By chemical formula formula by Ba2Co2Fe12O22Analytically pure CoO, BaCO3、Fe2O3It is equal by 20～24h of ball milling mixing after preparation It is even, then dry, sieve, briquetting, then 1230～1270 DEG C of Jing pre-burnings 3～6 hours, blocks of solid is obtained, then will be block solid Body crosses 120 mesh sieves and obtains Ba after crushing2Co2Fe12O22Powder.
9. Z- type ferrites flaky powder/PVDF Wave suction composite materials that prepared by a kind of method according to claim 1, it is special Levy and be, the chemical expression of the composite is x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x are (001) Ba3Co2Fe24O41The mass percent of sheet, and 5%≤x≤20%.
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