CN105482110B - A kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method - Google Patents
A kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method Download PDFInfo
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- CN105482110B CN105482110B CN201511018217.6A CN201511018217A CN105482110B CN 105482110 B CN105482110 B CN 105482110B CN 201511018217 A CN201511018217 A CN 201511018217A CN 105482110 B CN105482110 B CN 105482110B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
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Abstract
A kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method, by PVDF and CoFe2O4Powder is added in hydrochloric acid, adds aniline after well mixed, 30 60min are stirred under ice bath, is naturally cooling to subzero, ammonium persulfate solution is added dropwise, drop stirs 8 10h after finishing in ice-water bath, obtains mixed solution；Mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, is obtained black product, black product is dried.The present invention use In-situ reaction method, ammonium persulfate induce aniline formed long chain when and CoFe2O4,BaSr0.6Ti0.4O3Powder generation is compound, is advantageous to dielectric loss and magnetic loss reaches matching, make its absorbing property more preferable.Composite produced by the present invention has excellent absorbing property, and maximum reflection loss reaches 27.4dB, and the preparation technology of the composite is simple.
Description
Technical field
The invention belongs to materials science field, is related to a kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method.
Background technology
With science and technology and electronics industry development, the harm getting worse of electromagnetic radiation, at the same have magnetic loss with
The NEW TYPE OF COMPOSITE absorbing material of electrical loss turns into the focus of current research.Traditional electromagnetic shielding material, mainly by electricity
Magnetic wave is reflected to reach the purpose of shielding.But the electromagnetic wave reflected still can be to the normal work of extraneous electronic device
And the health of human body has an impact.Therefore, it is necessary to according to EM theory and the interaction principle of material and electromagnetic wave,
The compound of a variety of different fillers is carried out, there is high-selenium corn to electromagnetic wave to develop, the electromagnetic shielding material of low albedo, that is, inhale
Wave material.At present, absorbing material towards being " thin, light, wide, strong ", that is, require the coating layer thickness of absorbing material is thin, than important
Gently, the direction that absorption band wants wide is developed.But density is a bottle item of ferrite application scope greatly, therefore actual total
Find the microwave ferrite absorbing material that absorption frequency range is wide, absorbent properties are good and cost is low and seem very urgent.Improve ferrite
The absorbing property of absorbing material, match materials thickness and the application in low frequency field are reduced, mainly there are two kinds of approach at present：One
It is the sandwich construction by preparing material, makes full use of absorbing property of the different materials under different frequency range, make composite wave-absorbing material
Material obtains optimum organization to greatest extent, so as to meet that multiband, more mechanism absorb, meets modern society to the comprehensive of absorbing material
Close performance requirement.Second, by improving material electromagnetic parameter value the methods of ion substitution, preparation technology, increase loss is applied with being thinned
Thickness degree.
CoFe2O4For absorbing material because its is cheap, absorbing property is good, still has in the case of low frequency, thickness of thin preferably
Absorbing property, be one of more ripe absorbing material of current research, be still widely used so far from the fifties.CoFe2O4It
Caused by dielectric is due to caused by the self poling effect of molecule, and magnetic is then the natural resonance of material, wherein natural resonance is
Ferrite inhales the main mechanism of ripple, and research finds that ferritic absorbing property and composition, technique, shape and frequency used are close
It is related.In terms of electric property, the resistivity of Ferrite Material is larger, there is higher dielectric properties；In terms of magnetic property, iron oxygen
Body has obvious ferrimagnetism, in high frequency with higher magnetic conductivity.In recent years, with multi-disciplinary crossing research, inhale
Wave material has bigger space in the selection of material, particularly with the compound of different qualities material, absorbing material
Absorbing property has bigger raising.What PANI (aniline) and PVDF (poly- two vinylidene) was faced as electromagnetic-wave absorbent
Problem is PANI and PVDF and its composite is played maximum wave-sucking performance.On the one hand, improve PANI and PVDF and
The microwave electrical loss of its composite；On the other hand, preferable microwave absorption is reached with reference to magnetic loss.Come for absorbing material
Say, carried out the research of conduction high polymer radar absorbing in succession both at home and abroad, and have been achieved for certain progress.But
From the point of view of current application, simple magnetic loss type or dielectric loss type can not all fully meet the needs of application, Jiang Junjun
Et al. prepare polyaniline/CoFe with coordination-oxidation polymerization-hydro-thermal method2O4Nano-complex and its absorbing property is have studied, ground
Study carefully and find that compound is in multilevel hierarchy, wherein CoFe2O4For cubic, average grain diameter is less than 20mm, when composite thickness is
During 2mm, maximum reflection loss is -16.71dB at 16.01GHz.
The developing direction of following absorbing material is to integrate the compound suction ripple material of magnetic loss and electrical loss as can be seen here
Material.It is compound to prepare organic/inorganic polynary nanometer composite, due to the presence of its skin effect, quantum effect and synergy,
The Effective Regulation to composite electricity, magnetic property can be achieved, having can not substitute than single polymer or inorganic nano material
Advantage, be one of desirable route of the light, wideband of exploitation, high-efficiency electromagnetic absorbing material.
The content of the invention
It is an object of the invention to provide a kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method, the absorbing material
With excellent absorbing property, maximum reflection loss reaches -27.4dB, and preparation technology is simple.
To achieve the above object, the present invention is achieved through the following technical solutions：
A kind of PANI/CoFe2O4/ PVDF absorbing materials, reaction synthesis expression formula is PANI/xCoFe2O4/ (1-x) PVDF,
Wherein x is 0.1~0.9.
Reaction synthesis expression formula is PANI/xCoFe2O4/ (1-x) PVDF, wherein x are 0.3~0.9.
Reaction synthesis expression formula is PANI/xCoFe2O4/ (1-x) PVDF, wherein x are 0.6~0.9.
A kind of PANI/CoFe2O4The preparation method of/PVDF absorbing materials, comprises the following steps：
1) by PVDF and CoFe2O4Powder is added in hydrochloric acid, adds aniline after well mixed, 30- is stirred under ice bath
60min, be naturally cooling to it is subzero, be added dropwise ammonium persulfate solution, drop finish after 8-10h is stirred in ice-water bath, obtain mixed solution；
Wherein, PVDF and CoFe2O4The mass ratio of powder is (1-x)：X, x are 0.1~0.9, aniline and PVDF, CoFe2O4Powder it is total
The ratio of quality is (1~1.5):1；The mol ratio of ammonium persulfate and aniline in ammonium persulfate solution is (1~1.5):1；
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing obtains PANI/CoFe after drying2O4/ PVDF absorbing material absorbing materials.
The concentration of hydrochloric acid is 1~2mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
It is well mixed to be carried out under ultrasound.
Rate of addition is that 3s to 5s one drips.
Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid, concentration 0.21mol/L.
The drying is in vacuum drying chamber, and 18-24h is dried under the conditions of 60 DEG C.
Compared with prior art, the device have the advantages that：The present invention prepares doped hydrochloride using chemical oxidization method
Electrically conductive polyaniline, situ aggregation method prepare conductive PANI/CoFe2O4/ PVDF composites, obtain conductive, magnetic simultaneously
With the composite of nano effect.In addition, the method that the present invention uses In-situ reaction, ammonium persulfate induces aniline and forms long molecule
When chain and CoFe2O4, BaSr0.6Ti0.4O3Powder generation is compound, is advantageous to dielectric loss and magnetic loss reaches matching, make it
Absorbing property is more preferable.Composite produced by the present invention has excellent absorbing property, and maximum reflection loss reaches -27.4dB, should
The preparation technology of composite is simple.With CoFe2O4The reduction of content, saturation magnetization are gradually reduced 15.9-2.9emu/
G, remanent magnetization are also gradually reduced 7.9-1.5emu/g；Work as CoFe2O4Content be 90%, PVDF contents be 10% when, inhale ripple
Performance is best, and absorption maximum can reach -27.4dB, and below -10dB absorption band width is 3.4GHz (7.2~10.6GHz).
PANI/CoFe prepared by the present invention2O4/ PVDF absorbing materials can be used for absorbing material and electrostatic shielding materials, possess good
While inhaling wave energy, have both the features such as light weight, thickness of thin, broadband, compatibility are good and corrosion resistance is strong.
Brief description of the drawings
Fig. 1 is that concentration of hydrochloric acid is 2mol/mL, and aniline and ammonium persulfate mol ratio are 1:1, stirring gained powder under condition of ice bath
Body PANI XRD.
Fig. 2 is PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 90%, PVDF
Mass percent be 10% when composite granule XRD spectrum.
Fig. 3 is PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 70%, PVDF
Mass percent be 30% when composite granule XRD spectrum.
Fig. 4 is PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 50%, PVDF
Mass percent be 50% when composite granule XRD spectrum.
Fig. 5 is PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 30%, PVDF
Mass percent be 90% when composite granule XRD spectrum.
Fig. 6 is PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 10%, PVDF
Mass percent be 90% when composite granule XRD spectrum.
Fig. 7 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 90%,
The hysteresis curve of composite granule when PVDF mass percent is 10%.
Fig. 8 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 70%,
The hysteresis curve of composite granule when PVDF mass percent is 30%.
Fig. 9 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 50%,
The hysteresis curve of composite granule when PVDF mass percent is 50%.
Figure 10 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 30%,
The hysteresis curve of composite granule when PVDF mass percent is 70%.
Figure 11 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 10%,
The hysteresis curve of composite granule when PVDF mass percent is 90%.
Figure 12 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 90%,
The reflection loss figure of composite granule when PVDF mass percent is 10%.
Figure 13 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 70%,
The reflection loss figure of composite granule when PVDF mass percent is 30%.
Figure 14 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 50%,
The reflection loss figure of composite granule when PVDF mass percent is 50%.
Figure 15 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 30%,
The reflection loss figure of composite granule when PVDF mass percent is 70%.
Figure 16 is to work as PANI：(CoFe2O4+ PVDF) mass ratio=1:When 1, CoFe2O4Mass percent be 10%,
The reflection loss figure of composite granule when PVDF mass percent is 90%.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
The present invention is by aniline and ammonium persulfate according to mol ratio 1：1, it is added in 50mL 2mol/L hydrochloric acid, Ran Hou
8-10h is stirred under condition of ice bath, obtains PANI, wherein, aniline 1g；XRD tests are carried out to PANI, referring to Fig. 1, from Fig. 1
As can be seen that the PANI angles of diffraction of synthesis are about at 22,27 degree or so, and it is consistent with standard PANI peak, illustrate of the invention real
It is consistent with standard PANI peak to apply the PANI in a 1-7.
Embodiment 1
1) by PVDF and CoFe2O4Powder is added in 2mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
30min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 3s mono- drips, in ice after drop is complete
Stirred in water bath 10h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-
x)：X, x are mass percent, and x is 0.9, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1:1；Ammonium persulfate
The mol ratio of ammonium persulfate and aniline in solution is 1:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid,
Concentration is 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 18h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
Figure it is seen that CoFe2O4, PANI and PVDF characteristic diffraction peak, represent there be depositing for three in composite granule
.
From figure 7 it can be seen that coercive field is 1709.1 (Oe), saturation magnetization is 15.9 (emu/g), and remanent magnetization is strong
Spend for 7.9 (emu/g).
It can be recognized from fig. 12 that the absorption maximum of composite thick 3mm can reach -27.4dB, below -10dB absorption
Frequency bandwidth is 3.4GHz (7.2~10.6GHz).
Embodiment 2
1) by PVDF and CoFe2O4Powder is added in 2mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
30min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 4s mono- drips, in ice after drop is complete
Stirred in water bath 8h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-x)：
X, x are mass percent, and x is 0.7, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1:1；Ammonium persulfate solution
In ammonium persulfate and aniline mol ratio be 1:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid, concentration
For 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 20h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
As can be seen from Figure 3 CoFe2O4, PANI and PVDF characteristic diffraction peak, represent there be depositing for three in composite granule
.
As can be seen from Figure 8 coercive field is 1685.2 (Oe), and saturation magnetization is 13.3 (emu/g), remanent magnetization
Intensity is 6.5 (emu/g).
As can be seen from Figure 13, the absorption maximum of composite thick 3mm can reach -21.7dB, below -10dB absorption
Frequency bandwidth is 3.3GHz (8.1~11.4GHz).
Embodiment 3
1) by PVDF and CoFe2O4Powder is added in 2mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
30min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 5s mono- drips, in ice after drop is complete
Stirred in water bath 9h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-x)：
X, x are mass percent, and x is 0.5, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1:1；Ammonium persulfate solution
In ammonium persulfate and aniline mol ratio be 1:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid, concentration
For 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 22h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
As can be seen from Figure 4 CoFe2O4, PANI and PVDF characteristic diffraction peak, represent there be depositing for three in composite granule
.
As can be seen from Figure 9 coercive field is 1709.1 (Oe), and saturation magnetization is 10.1 (emu/g), remanent magnetization
Intensity is 4.9 (emu/g).
It is seen from figure 14 that the absorption maximum of composite thick 3mm can reach -15.9dB, below -10dB absorption
Frequency bandwidth is 3.1GHz (7.4~10.5GHz).
Embodiment 4
1) by PVDF and CoFe2O4Powder is added in 2mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
30min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 3s mono- drips, in ice after drop is complete
Stirred in water bath 8h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-
x)：X, x are mass percent, and x is 0.3, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1:1；Ammonium persulfate is molten
The mol ratio of ammonium persulfate and aniline in liquid is 1:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid, dense
Spend for 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 24h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
As can be seen from Figure 5 CoFe2O4, PANI and PVDF characteristic diffraction peak, represent there be depositing for three in composite granule
.
As can be seen from Figure 10 coercive field is 1609.3 (Oe), and saturation magnetization is 6.9 (emu/g), remanent magnetization
Intensity is 3.3 (emu/g).
It can be seen from fig. 15 that the absorption maximum of composite thick 3mm can reach -15.8dB, below -10dB absorption
Frequency bandwidth is 5.2GHz (10.9~16.1GHz).
Embodiment 5
1) by PVDF and CoFe2O4Powder is added in 2mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
30min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 4s mono- drips, in ice after drop is complete
Stirred in water bath 10h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-
x)：X, x are mass percent, and x is 0.1, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1:1；Ammonium persulfate is molten
The mol ratio of ammonium persulfate and aniline in liquid is 1:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid, dense
Spend for 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 21h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
As can be seen from Figure 6 CoFe2O4, PANI and PVDF characteristic diffraction peak, represent there be depositing for three in composite granule
.
As can be seen from Figure 11 coercive field is 1671.5 (Oe), and saturation magnetization is 2.9 (emu/g), remanent magnetization
Intensity is 1.5 (emu/g).
As can be seen from Figure 16, the absorption maximum of composite thick 3mm can reach -17.5dB, below -10dB absorption
Frequency bandwidth is 3.5GHz (7.4~10.9GHz).
Embodiment 6
1) by PVDF and CoFe2O4Powder is added in 1mol/L hydrochloric acid, and aniline is added after being well mixed under ultrasound,
45min is stirred under ice bath, is naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 4s mono- drips, in ice after drop is complete
Stirred in water bath 8.5h, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is (1-
x)：X, x are mass percent, and x is 0.4, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1.2:1；Ammonium persulfate
The mol ratio of ammonium persulfate and aniline in solution is 1.5:1；Ammonium persulfate solution is made by dissolving ammonium persulfate into hydrochloric acid
, concentration 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 23h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
Embodiment 7
1) by PVDF and CoFe2O4Powder is added in 1.5mol/L hydrochloric acid, and benzene is added after being well mixed under ultrasound
Amine, 60min is stirred under ice bath, be naturally cooling to subzero, dropwise addition ammonium persulfate solution, rate of addition is that 5s mono- drips, after drop finishes
9.5h is stirred in ice-water bath, obtains mixed solution；Wherein, PVDF (poly- two vinylidene) and CoFe2O4The mass ratio of powder is
(1-x)：X, x are mass percent, and x is 0.8, aniline and PVDF, CoFe2O4The ratio of the gross mass of powder is 1.5:1；Over cure
The mol ratio of ammonium persulfate and aniline in acid ammonium solution is 1.3:1；Ammonium persulfate solution is by dissolving ammonium persulfate into hydrochloric acid
In be made, concentration 0.21mol/L；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black is produced
Thing dries 20h under the conditions of 60 DEG C, obtains PANI/CoFe in vacuum drying chamber2O4/ PVDF absorbing material absorbing materials.
The sorbing material of the present invention has excellent absorbing property, and maximum reflection loss reaches -27.4dB.The composite
Preparation technology is simple.With CoFe2O4The reduction of content, saturation magnetization are gradually reduced 15.9-2.9emu/g, remanent magnetization
Intensity is also gradually reduced 7.9-1.5emu/g；Work as CoFe2O4Content be 90%, PVDF contents be 10% when, absorbing property is best,
Absorption maximum can reach -27.4dB, and below -10dB absorption band width is 3.4GHz (7.2~10.6GHz).
Claims (6)
- A kind of 1. PANI/CoFe2O4The preparation method of/PVDF absorbing materials, it is characterised in that comprise the following steps：1) by PVDF and CoFe2O4Powder is added in hydrochloric acid, adds aniline after well mixed, 30-60min is stirred under ice bath, Be naturally cooling to it is subzero, be added dropwise ammonium persulfate solution, drop finish after 8-10h is stirred in ice-water bath, obtain mixed solution；Wherein, PVDF and CoFe2O4The mass ratio of powder is (1-x)：X, x are 0.1~0.9, aniline and PVDF, CoFe2O4The gross mass of powder Ratio be (1~1.5):1；The mol ratio of ammonium persulfate and aniline in ammonium persulfate solution is (1~1.5):1；2) mixed solution is filtered, is washed repeatedly with ultra-pure water until filtrate is in colourless, obtain black product, black product is done PANI/CoFe is obtained after dry2O4/ PVDF absorbing materials.
- A kind of 2. PANI/CoFe according to claim 12O4The preparation method of/PVDF absorbing materials, it is characterised in that institute It is 1~2mol/L to state concentration of hydrochloric acid；PVDF、CoFe2O4The gross mass of powder and the ratio of hydrochloric acid are 2g：50mL.
- A kind of 3. PANI/CoFe according to claim 12O4The preparation method of/PVDF absorbing materials, it is characterised in that mixed Conjunction is uniformly carried out under ultrasound.
- A kind of 4. PANI/CoFe according to claim 12O4The preparation method of/PVDF absorbing materials, it is characterised in that drop Acceleration is that 3s to 5s one drips.
- A kind of 5. PANI/CoFe according to claim 12O4The preparation method of/PVDF absorbing materials, it is characterised in that mistake Ammonium sulfate is made by dissolving ammonium persulfate into hydrochloric acid, concentration 0.21mol/L.
- A kind of 6. PANI/CoFe according to claim 12O4The preparation method of/PVDF absorbing materials, it is characterised in that institute It is in vacuum drying chamber to state drying, and 18-24h is dried under the conditions of 60 DEG C.
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| CN201511018217.6A CN105482110B (en) | 2015-12-29 | 2015-12-29 | A kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method |
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| CN105482110A CN105482110A (en) | 2016-04-13 |
| CN105482110B true CN105482110B (en) | 2017-11-10 |
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