CN106633547B - A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and preparation method thereof - Google Patents

A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and preparation method thereof Download PDF

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CN106633547B
CN106633547B CN201611162387.6A CN201611162387A CN106633547B CN 106633547 B CN106633547 B CN 106633547B CN 201611162387 A CN201611162387 A CN 201611162387A CN 106633547 B CN106633547 B CN 106633547B
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pvdf
powder
composite material
flaky powder
bafe
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CN106633547A (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

A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and preparation method thereof, PVDF powder is added in acetone, PVDF solution is obtained after dissolution, and the Ba for having orientation in (001) direction is then added3Co2Fe24O41Flaky powder is uniformly mixed, obtains composite mortar；Composite mortar is cast, Z- type ferrite flaky powder/PVDF Wave suction composite material is obtained.The present invention uses casting technique, and material dispersion is uniformly and the thickness of film is uniform, and prepares casting slurry nontoxicity used, will not cause harm to the human body.Present device is simple, process stabilizing, can operate continuously, and high production efficiency reduces costs, it can be achieved that increasingly automated, material compactness and has good uniformity, and preparation method is simple.

Description

A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and preparation method thereof
Technical field
The invention belongs to materials science field, be related to a kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and Preparation method.
Background technique
With the rapid development of electronic technology, radar and the communication technology, electromagenetic wave radiation is had become after noise pollution, atmosphere Another big public hazards after pollution, water pollution, solid waste pollution.The electromagnetic interference (EMI) that electromagenetic wave radiation generates not only can The normal operation of various electronic equipments is influenced, and also harmful to the health of the mankind.Therefore, electricity of good performance is developed There is very urgent scientific meaning and reality to need for electromagnetic wave shielding material, evolution electromagnetic environment.Traditional absorbing material, which has, to be inhaled Wave energy power is weak, density is big, inhales the disadvantages of wave frequency band is narrow, is unable to satisfy 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 is expected preparative by the compound realization performance complement of multiple material function and optimization Can excellent Materials Inorganic magnetic powder-composite membrane of polymer material be Polymer-based Magnets research and application form it One it is main be exactly to take physically or chemically means system for ferrite and the polymeric matrixs such as terres rares permanent magnetic powder and resin are compound Film forming.
Absorbing material needs to meet two principles：Impedance matching, can be to the greatest extent when electromagnetic wave incident is to material surface Into material internal；Attenuation characteristic, the electromagnetic wave into material need effective decaying rapidly.Ferrite is research using more It is extensive a kind of, very much, the single ferritic reflection losses of the research of the multiple correlation of inorganic magnetic powder and organic matter It is small, frequency bandwidth is narrow, in order to improve its absorbing property, the method mainly taken be chemically composited method (there are two types of or it is two or more Ferrite either ferrite and conductive bluk recombination), preparation process is complicated, be easy to appear chemical reaction in recombination process, Interfacial effect is complicated.
Summary of the invention
The purpose of the present invention is to provide a kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and its preparation sides Method, and absorbing material obtained, due to interfacial effect and impedance optimization, which has excellent absorbing property, Maximum reflection loss reaches -31.03dB, and preparation process is simple.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material, includes the following steps：
Step 1：PVDF powder is added in acetone, PVDF solution is obtained after dissolution, is then added and has in (001) direction There is the Ba of orientation3Co2Fe24O41Flaky powder is uniformly mixed, obtains composite mortar；Wherein, by mass percentage, in (001) Direction has the Ba of orientation3Co2Fe24O41The mass ratio of flaky powder and PVDF powder is (5%~20%)：(80%~ 95%)；
Step 2：Composite mortar is cast, Z- type ferrite flaky powder/PVDF Wave suction composite material is obtained.
Further improvement of the invention is that the temperature of acetone is 40~50 DEG C.
Further improvement of the invention is that the mass ratio of PVDF powder and acetone is 1:4.
Further improvement of the invention is, when curtain coating is cast 200-250 μm of height of scraper.
Further improvement of the invention is that (001) direction has the Ba of orientation3Co2Fe24O41Flaky powder by with Lower process preparation：
Step 1：It 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 kept the temperature at 1150~1200 DEG C, obtains BaFe12O19Presoma；
Step 2：By Fe2O3And BaCl2.2H2O mixing, is then added BaFe12O19Presoma, after ball milling mixing is uniform, 6~10h is kept the temperature at 1200~1250 DEG C, obtains the BaFe that there is orientation in (001) direction12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2.2H2The 5~10% of O gross mass； BaCl2.2H2The additional amount of O is Fe2O32~3 times of quality；
Step 3：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to molar ratio:1 is mixed It closes, while fused salt is added, be uniformly mixed, at 1250~1300 DEG C, keep the temperature 6~10h, obtain having in (001) direction and take To Ba3Co2Fe24O41Flaky powder is denoted as (001) Ba3Co2Fe24O41Flaky powder.
Further improvement of the invention is that fused salt is NaCl in step 1, and the quality of NaCl is BaCO3With Fe2O3Always 1~2 times of quality.
Further improvement of the invention is that 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.
Further improvement of the invention is, random Ba2Co2Fe12O22Powder is prepared by the following method：
By chemical formula formula by Ba2Co2Fe12O22Analytically pure CoO, BaCO3、Fe2O3By ball milling 20~mix for 24 hours after preparation Close uniformly, then dry, be sieved, briquetting, then through 1230~1270 DEG C pre-burning 3~6 hours, blocks of solid is obtained, then by block Shape solid smashes it through 120 meshes and obtains Ba2Co2Fe12O22Powder.
A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material, which is characterized in that the chemical table of the composite material It is x (001) Ba up to formula3Co2Fe24O41/ (1-x) PVDF, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and 5%≤x≤20%.
Compared with prior art, the present invention uses 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 is capable of providing dielectric loss, so that composite material not only has magnetic loss, but also has dielectric loss, meets impedance matching, reach To excellent wave-absorbing effect.The present invention passes through molten-salt growth method first and is prepared for (001) Ba3Co2Fe24O41Then flaky powder passes through Mechanical mixture progress two is compound after organic matter dissolves PVDF powder, wherein x is (001) Ba3Co2Fe24O41The matter of flaky powder Measure percentage, after tape casting, excellent (001) Ba of absorbing property is made in and 5%≤x≤35%3Co2Fe24O41Flaky powder Fill the absorbing material of PVDF matrix.The present invention uses casting technique, and material dispersion is uniformly and the thickness of film is uniform, and makes Standby casting slurry used is non-toxic, will not cause harm to the human body.Present device is simple, process stabilizing, can operate continuously, High production efficiency reduces costs, it can be achieved that increasingly automated, material compactness and has good uniformity, and preparation method letter It is single.
The uniformity of curtain coating thick film produced by the present invention is preferable, is laid in flaky powder uniformly 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 1.57emu/g, absorbing property is best, and absorption maximum can reach -21.2dB, -10dB with Under absorption band width be 4GHz.
Further, sheet Ba is prepared using molten-salt growth method in the present invention3Co2Fe24O41, pass through the tape casting conducive to the later period and prepare x(001)Ba3Co2Fe24O41/ (1-x) PVDF absorbing material, the absorbing material good dispersion of the method preparation, thickness is uniform, causes Close property is good and can generate on a large scale.
Detailed description of the invention
Fig. 1 is (001) Ba of molten-salt growth method preparation3Co2Fe24O41Flaky powder, 1300 DEG C of resulting XRD diagram of sintering.
Fig. 2 is to work as Ba3Co2Fe24O41Mass percent when to be 5%, PVDF mass percent be 95%, curtain coating gained is multiple The SEM of condensation material schemes.
Fig. 3 is to work as Ba3Co2Fe24O41Mass percent when to be 20%, PVDF mass percent be 80%, curtain coating gained The SEM of composite material schemes.
Fig. 4 is to work as Ba3Co2Fe24O41Mass percent when to be 5%, PVDF mass percent be 95%, curtain coating gained is multiple The hysteresis loop of condensation material.
Fig. 5 is to work as Ba3Co2Fe24O41Mass percent when to be 20%, PVDF mass percent be 80%, curtain coating gained The hysteresis loop of composite material.
Fig. 6 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percent be 95%, when with a thickness of 2mm, The reflection loss figure of curtain coating gained composite material.
Fig. 7 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percent be 95%, when with a thickness of 3mm, The reflection loss figure of curtain coating gained composite material.
Fig. 8 is to work as Ba3Co2Fe24O41Mass percent be 5%, PVDF mass percent be 95%, when with a thickness of 4mm, The reflection loss figure of curtain coating gained composite material.
Fig. 9 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percent be 90%, with a thickness of 2mm When, the reflection loss figure of curtain coating gained composite material.
Figure 10 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percent be 90%, with a thickness of 3mm When, the reflection loss figure of curtain coating gained composite material.
Figure 11 is to work as Ba3Co2Fe24O41Mass percent be 10%, PVDF mass percent be 90%, with a thickness of 4mm When, the reflection loss figure of curtain coating gained composite material.
Figure 12 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percent be 85%, with a thickness of 2mm When, the reflection loss figure of curtain coating gained composite material.
Figure 13 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percent be 85%, with a thickness of 3mm When, the reflection loss figure of curtain coating gained composite material.
Figure 14 is to work as Ba3Co2Fe24O41Mass percent be 15%, PVDF mass percent be 85%, with a thickness of 4mm When, the reflection loss figure of curtain coating gained composite material.
Figure 15 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percent be 80%, with a thickness of 2mm When, the reflection loss figure of curtain coating gained composite material.
Figure 16 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percent be 80%, with a thickness of 3mm When, the reflection loss figure of curtain coating gained composite material.
Figure 17 is to work as Ba3Co2Fe24O41Mass percent be 20%, PVDF mass percent be 80%, with a thickness of 4mm When, the reflection loss figure of curtain coating gained composite material.
Specific embodiment
By specific embodiment, the present invention is described in detail with reference to the accompanying drawing.
The Ba obtained after curtain coating3Co2Fe24O41Flaky powder/PVDF Wave suction composite material is film, by film together with film strips It is put into vacuum oven, under conditions of 200 DEG C, dry 5min, then ice-water bath chilling 2min, vacuum drying at 200 DEG C In the process, PVDF has the process of a phase transformation, while by way of the chilling in ice bath 2min, is conducive to demoulding and densification； Then it dries, lamination, is tested after hot pressing.Wherein, the temperature of hot pressing is 150~180 DEG C, and pressure is 0.5~1MPa, pressure maintaining Time is 30s~1min.
In the present invention compression moulding be specifically will the casting films that fold as in mold, hot pressing and pressure maintaining one minute.
Embodiment 1
(1) by BaCO3, Fe2O3, after NaCl is accurately weighed with electronic balance, it is placed in ball grinder, is sufficiently mixed Even, taking-up is dried for standby.Wherein BaCO3, Fe2O3Quality summation and NaCl mass ratio be 1:1, BaCO3With Fe2O3Amount press According to by chemical general formula BaFe12O19It is weighed；Material used in ball milling, ball, the mass ratio of alcohol are 1：2：1, the revolving speed of ball mill For 500r/min, ball milling 18h, temperature is that 7h is placed at 98 DEG C in an oven, takes out mixed powder, crosses 60 meshes.
(2) prepared raw material is obtained into BaFe in 1150 DEG C of pre-burning 4h12O19Presoma, then with heat ultrapure water into Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines at 1200 DEG C Then the ultrapure water of heat is added in 10h, ultrasonic disperse washs, and filtering is dried to obtain sheet (001) BaFe12O19Flaky powder, It is denoted as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The additional amount of O is Fe2O32 times of quality；BaFe12O19Forerunner The quality of body is BaCl2.2H2O、Fe2O3And BaFe12O19The 5% of presoma gross mass.
(4) chemical general formula Ba is pressed2Co2Fe12O22, by BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, placement Ball milling for 24 hours, is then dried in ball grinder, sieving, briquetting, and 6h is then kept the temperature at 1230 DEG C into phase, 120 mesh sieve is crossed, obtains To random Ba2Co2Fe12O22Powder is denoted as Co2Y。
The random Ba that will be obtained2Co2Fe12O22Powder and above-mentioned (001) BaFe prepared12O19Powder is according to molar ratio It is 1:1 mixing, adds NaCl, electric stirring mixing 12h, and the quality that NaCl is added is equal to random Ba2Co2Fe12O22Powder with (001)BaFe12O19Powder quality summation makes oxide carry out abundant fused salt reaction, then with heat in 1250 DEG C of heat preservation 10h Ultrapure water is washed, and until sodium chloride is washed clean, filtering is dry, obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) acetone that 1g PVDF powder is poured into 4g stirs 3h, until liquid is clear in the environment of 50 DEG C of magnetic agitations Clearly, it is completely dissolved PVDF powder, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composite material：Into the 1g PVDF solution being uniformly dissolved (001) Ba of 0.05g is added3Co2Fe24O41Flaky powder obtains composite mortar by electric stirring 8h；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing material, scraper Height be adjusted to 200mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=5%.
(8) it by the thick film of tape casting, is put into 200 DEG C of vacuum oven at once, in ice-water bath chilling after 5min 2min。
(9) dry after demoulding, by thick film lamination, hot pressing cyclization, 150 DEG C of heating temperature, pressurize 0.5MPa, pressure maintaining 60s.
(001) Ba of preparation is proved after tested3Co2Fe24O41/ PVDF absorbing material, flaky powder are spread in PVDF, There is excellent absorbing property in the range of 2-18GHz.
It will be seen from figure 1 that the Ba of preparation3Co2Fe24O41No miscellaneous phase generates, the oriented growth on (001) direction.
Figure it is seen that the Ba of preparation3Co2Fe24O41Random powder is generated without miscellaneous phase.
From fig. 4, it can be seen that the composite material of preparation has apparent ferromagnetism, saturation magnetization 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, - 10dB absorption band width below 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, - 10dB absorption band width below 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, - 10dB absorption band width below is 1.8GHz (9.0~10.8GHz).
Embodiment 2
A kind of Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, the chemical expression of the absorbing material are x (001)Ba3Co2Fe24O41/ (1-x) PVDF, wherein x is (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x= 10%.
Above-mentioned Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, includes the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl is accurately weighed with electronic balance, it is placed in ball grinder, it is sufficiently mixed It closes uniformly, taking-up is dried for standby.Wherein raw material BaCO3, Fe2O3Quality summation and NaCl mass ratio be 1:1.4, BaCO3With Fe2O3Amount according to press chemical general formula BaFe12O19It is weighed；Material used in ball milling, ball, the mass ratio of alcohol are 1：2：1, ball The revolving speed of grinding machine is 500r/min, ball milling 18h, and temperature is that 7h is placed at 98 DEG C in an oven, takes out mixed powder, crosses 60 mesh Sieve.
(2) prepared raw material is obtained into BaFe in 1170 DEG C of pre-burning 3.5h12O19Presoma.Then with the ultrapure water of heat It is washed, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then in 1220 DEG C of calcining 9h Obtain sheet (001) BaFe12O19Then the ultrapure water of heat is added in flaky powder, ultrasonic disperse washs, and filtering is dried to obtain Sheet (001) BaFe12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The additional amount of O is Fe2O32.2 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 7%.
(4) chemical general formula Ba is pressed2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, It is placed on ball milling 23h in ball grinder, is then dried, is sieved, then briquetting keeps the temperature 5h into phase at 1240 DEG C, crosses 120 meshes Son obtains random Ba2Co2Fe12O22Powder is denoted as Co2Y, the random Ba that will be obtained2Co2Fe12O22It powder and above-mentioned prepares (001)BaFe12O19(as template) is 1 according to molar 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, heat preservation 9h makes oxide carry out abundant fused salt reaction, is then washed with the ultrapure water of heat, until sodium chloride is washed clean, mistake Filter, it is dry, obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) acetone that 0.95g PVDF powder is poured into 3.8g stirs 4h, until liquid in the environment of 48 DEG C of magnetic agitations Body clarification, is completely dissolved PVDF powder, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composite material：To the 0.95g PVDF solution being uniformly dissolved According to be added 0.1g (001) Ba3Co2Fe24O41Flaky powder obtains composite mortar by electric stirring 9h；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing material, scraper Height be adjusted to 220mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=10%.
(8) it by the thick film of tape casting, is put into 200 DEG C of vacuum oven at once, in ice-water bath chilling after 5min 2min。
(9) dry after demoulding, by thick film lamination, hot pressing cyclization, 160 DEG C of heating temperature, pressurize 0.6MPa, pressure maintaining 50s.
(001) Ba of preparation is proved after tested3Co2Fe24O41/ PVDF absorbing material, flaky powder are spread 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, - 10dB absorption band width below 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, - 10dB absorption band width below is 3.5GHz (10.0~13.5GHz).
Embodiment 3
Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, the chemical expression of the absorbing material are x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x is (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x=15%.
Above-mentioned Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, includes the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl is accurately weighed with electronic balance, it is placed in ball grinder, it is sufficiently mixed It closes uniformly, taking-up is dried for standby.Wherein raw material BaCO3, Fe2O3Quality summation and NaCl mass ratio be 1:1.6, BaCO3With Fe2O3Amount according to press chemical general formula BaFe12O19It is weighed；Material used in ball milling, ball, the mass ratio of alcohol are 1：2：1, ball The revolving speed of grinding machine is 500r/min, ball milling 18h, and temperature is that 7h is placed at 98 DEG C in an oven, takes out mixed powder, crosses 60 mesh Sieve.
(2) prepared raw material is obtained into BaFe in 1180 DEG C of pre-burning 3h12O19Presoma.Then with heat ultrapure water into Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then in 1240 DEG C of calcining 8h Obtain sheet (001) BaFe12O19Then the ultrapure water of heat is added in flaky powder, ultrasonic disperse washs, and filters, dry, obtains Sheet (001) BaFe12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The additional amount of O is Fe2O32.6 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 8%.
(4) chemical general formula Ba is pressed2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, It is placed on ball milling 21h in ball grinder, is then dried, is sieved, then briquetting keeps the temperature 4h into phase at 1250 DEG C, crosses 120 meshes Son obtains random Ba2Co2Fe12O22Powder is denoted as Co2Y, the random Ba that will be obtained2Co2Fe12O22It powder and above-mentioned prepares (001)BaFe12O19Powder is 1 according to molar 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, heat preservation 8h makes oxygen Compound carries out abundant fused salt reaction, is then washed with the ultrapure water of heat, and until sodium chloride is washed clean, filtering is dry, Obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) acetone that 0.9g PVDF powder is poured into 3.6g stirs 5h, until liquid in the environment of 44 DEG C of magnetic agitations Clarification, is completely dissolved PVDF powder, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composite material：To the 0.9g PVDF solution being uniformly dissolved According to be added 0.15g (001) Ba3Co2Fe24O41Flaky powder obtains composite mortar by electric stirring 10h；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing material, scraper Height be adjusted to 230mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=15%.
(8) it by the thick film of tape casting, is put into 200 DEG C of vacuum oven at once, in ice-water bath chilling after 5min 2min。
(9) dry after demoulding, by thick film lamination, hot pressing cyclization, 170 DEG C of heating temperature, pressurize 0.7MPa, pressure maintaining 40s. (001) Ba of preparation is proved after tested3Co2Fe24O41/ PVDF absorbing material, flaky powder is spread 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, - 10dB absorption band width below is 0.9GHz (6.2~7.1GHz).
As can be seen from Figure 13, thickness of composite material 3.0mm, in 6.9GHz, maximum reflection loss -20.5dB, - 10dB absorption band width below 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, - 10dB absorption band width below is 2.9GHz (6.8~7.3GHz) and (15.6~18GHz).
Embodiment 4
One kind (001) Ba3Co2Fe24O41Flaky powder fills the absorbing material and preparation method thereof of its random powder, special Sign is that the chemical expression of the absorbing material is x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x is (001) Ba3Co2Fe24O41The mass percent of flaky powder, and x=20%.
Above-mentioned (001) Ba3Co2Fe24O41The preparation method of/PVDF absorbing material, includes the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl is accurately weighed with electronic balance, it is placed in ball grinder, it is sufficiently mixed It closes uniformly, taking-up is dried for standby.Wherein raw material BaCO3, Fe2O3Quality summation and NaCl mass ratio be 1:2, BaCO3With Fe2O3Amount according to press chemical general formula BaFe12O19It is weighed；Material used in ball milling, ball, the mass ratio of alcohol are 1：2：1, ball The revolving speed of grinding machine is 500r/min, ball milling 18h, and temperature is that 7h is placed at 98 DEG C in an oven, takes out mixed powder, crosses 60 mesh Sieve.
(2) prepared raw material is obtained into BaFe in 1200 DEG C of pre-burning 2h12O19Presoma.Then with heat ultrapure water into Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2.2H2O and BaFe12O19Presoma ball milling mixing is uniform, then in 1250 DEG C of calcining 6h Obtain sheet (001) BaFe12O19Then the ultrapure water of heat is added in flaky powder, ultrasonic disperse washs, and filters, dry, obtains Sheet (001) BaFe12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2The additional amount of O is Fe2O33 times of quality；BaFe12O19The quality of presoma is BaCl2.2H2O、Fe2O3And BaFe12O19Presoma gross mass 10%.
(4) chemical general formula Ba is pressed2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, It is placed on ball milling in ball grinder for 24 hours, then to dry, be sieved, then briquetting keeps the temperature 3h into phase at 1260 DEG C, crosses 120 meshes Son obtains sheet (001) BaFe12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder.Wherein, BaCl2.2H2O's adds Entering amount is 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 prepared12O19Powder is 1 according to molar ratio:1 powder, NaCl electric stirring mixing 16h, the quality that NaCl is added are equal to Ba2Co2Fe12O22Powder and (001) BaFe12O19Powder quality 2 times of summation, at 1300 DEG C, heat preservation 6h makes oxide carry out abundant fused salt reaction, is then washed with the ultrapure water of heat, directly It is washed clean to sodium chloride, it filters, it is dry, obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) acetone that 0.85g PVDF powder is poured into 3.4g stirs 6h, until liquid in the environment of 40 DEG C of magnetic agitations Body clarification, is completely dissolved PVDF powder, obtains PVDF solution；
(6) x (001) Ba is prepared3Co2Fe24O41/ (1-x) PVDF composite material：To the 0.85gPVDF solution being uniformly dissolved According to be added 0.2g (001) Ba3Co2Fe24O41Flaky powder obtains composite mortar by electric stirring 12h；
(7) composite mortar is prepared into x (001) Ba by casting technique3Co2Fe24O41/ (1-x) PVDF absorbing material, scraper Height be adjusted to 250mm, obtain Ba3Co2Fe24O41Flaky powder/PVDF Wave suction composite material, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and x=20%.
(8) it by the thick film of tape casting, is put into 200 DEG C of vacuum oven at once, in ice-water bath chilling after 5min 2min。
(9) dry after demoulding, by thick film lamination, hot pressing cyclization, 180 DEG C of heating temperature, pressurize 1MPa, pressure maintaining 30s.
(001) Ba of preparation is proved after tested3Co2Fe24O41/ PVDF absorbing material, flaky powder are spread 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 is 2 μm of sheet or so, Ba3Co2Fe24O41Random powder Crystallite dimension is 50nm~80nm or so, Ba3Co2Fe24O41Content is less, and composite material compactness is good.
From fig. 5, it can be seen that the saturation magnetization of composite material is 5.05emu/g, remanent magnetization is 1.08emu/g, coercive field 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 3.0mm, in 13.2GHz, maximum reflection loss -21.3dB, - 10dB absorption band width below is 1.4GHz (12.8~14.2GHz).
As can be seen from Figure 17, thickness of composite material 4.0mm, in 11.5GHz, maximum reflection loss -20.0dB, - 10dB absorption band width below 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 it is with higher it is magnetic respectively to Anisotropic equivalent field, thus having higher natural resonant frequency sheet is the optimum shape of absorbent.It is found by Robert et al. Excellent magnetic property is shown in (001) direction after hexagonal barium ferrite oriented growth.PVDF has good dielectricity simultaneously Can, hexagonal barium ferrite is dispersed in PVDF matrix, forms composite material by way of tape casting later, be prepared Composite material both had magnetic loss but also with dielectric loss, so that composite material be made to have excellent absorbing property, was cast simultaneously PVDF while it being used as electromagnetic wave transparent material in the composite material obtained afterwards, can replace prior paraffin material, avoids paraffin and powder Non-uniform mixing.
The present invention prepares x (001) Ba by the tape casting3Co2Fe24O41/ (1-x) PVDF thick film, 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 mixing, curtain coating, hot pressing are then discharged out organic matter, are prepared in the present invention using molten-salt growth method (001)Ba3Co2Fe24O41Flaky powder prepares the thick film of directional profile using the tape casting, then anxious after vacuum drying Cold, demoulding is hot-forming to prepare Both ring sam.High production efficiency of the present invention, automatization level is high, can be mass-produced, and is made The absorbing property of composite material is excellent.

Claims (8)

1. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material, which is characterized in that including following step Suddenly：
Step 1：PVDF powder is added in acetone, PVDF solution is obtained after dissolution, be then added (001) direction have take To Ba3Co2Fe24O41Flaky powder is uniformly mixed, obtains composite mortar；Wherein, by mass percentage, in (001) direction Ba with orientation3Co2Fe24O41The mass ratio of flaky powder and PVDF powder is (5%~20%)：(80%~95%)；Its In, (001) direction has the Ba of orientation3Co2Fe24O41Flaky powder is prepared by following procedure：
Step 1)：It will be according to BaFe12O19In mol ratio weigh BaCO respectively3、Fe2O3And fused salt ball milling mixing is uniform, so 2~4h is kept the temperature at 1150~1200 DEG C afterwards, obtains BaFe12O19Presoma；
Step 2)：By Fe2O3And BaCl2.2H2O mixing, is then added BaFe12O19Presoma, after ball milling mixing is uniform, 1200 6~10h is kept the temperature at~1250 DEG C, obtains the BaFe that there is orientation in (001) direction12O19Flaky powder is denoted as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2.2H2The 5~10% of O gross mass； BaCl2.2H2The additional amount of O is Fe2O32~3 times of quality；
Step 3)：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to molar ratio:1 mixing, together When fused salt is added, be uniformly mixed, at 1250~1300 DEG C, keep the temperature 6~10h, obtain (001) direction have orientation Ba3Co2Fe24O41Flaky powder；
Step 2：Composite mortar is cast, Z- type ferrite flaky powder/PVDF Wave suction composite material is obtained.
2. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, the temperature of acetone is 40~50 DEG C.
3. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, the mass ratio of PVDF powder and acetone is 1:4.
4. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, 200-250 μm of height of scraper is cast when curtain coating.
5. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, fused salt is NaCl in step 1), and the quality of NaCl is BaCO3With Fe2O31~2 times of gross mass.
6. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, fused salt is NaCl in step 3), and the quality of NaCl is random Ba2Co2Fe12O22Powder and (001) BaFe12O19Piece 1~2 times of shape powder gross mass.
7. a kind of preparation method of Z- type ferrite flaky powder/PVDF Wave suction composite material according to claim 1, It is characterized in that, random Ba2Co2Fe12O22Powder is prepared by the following method：
By chemical formula Ba2Co2Fe12O22By analytically pure CoO, BaCO3、Fe2O3By ball milling 20~be uniformly mixed for 24 hours after preparation, Then dry, be sieved, briquetting, then through 1230~1270 DEG C pre-burning 3~6 hours, blocks of solid is obtained, then by blocks of solid powder 120 meshes are crossed after broken obtains Ba2Co2Fe12O22Powder.
8. Z- type ferrite flaky powder/PVDF Wave suction composite material that one kind is prepared method according to claim 1, special Sign is that the chemical expression of the composite material is x (001) Ba3Co2Fe24O41/ (1-x) PVDF, wherein x is (001) Ba3Co2Fe24O41The mass percent of sheet, and 5%≤x≤20%.
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