CN106410426A - Silicon oil magnetic fluid absorbing material based on carboxy siloxane and preparation method - Google Patents
Silicon oil magnetic fluid absorbing material based on carboxy siloxane and preparation method Download PDFInfo
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- CN106410426A CN106410426A CN201611049481.0A CN201611049481A CN106410426A CN 106410426 A CN106410426 A CN 106410426A CN 201611049481 A CN201611049481 A CN 201611049481A CN 106410426 A CN106410426 A CN 106410426A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
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Abstract
The invention provides a silicone oil magnetic fluid absorbing material based on carboxy siloxane and a preparation method. The material comprises a magnetic fluid composite coating and a semiconductor coating in turn. The magneti c fluid composite coating comprises Fe3O4 nanoparticles, graphene, carboxy siloxane, dimethyl silicone oil, epoxy resin, ethylenediamine and carbonyl nickel powder, and carbonyl iron powder or iron-based alloy magnetic powder high permeability alloy powder. The semiconductor coating comprises epoxy resin, ethylenediamine and semiconductor SiC powder. The absorbing material provided by the invention contains a silicone oil magnetic fluid with excellent stability. The silicone oil magnetic fluid is combined with the magnetic fluid composite coating prepared with epoxy resin, ethylenediamine and high permeability alloy powder and the semiconductor coating containing semiconductor SiC powder, so as to form the absorbing material. The absorbing material has the advantages of light mass, thin thickness, high magnetic fluid solid content, high saturation magnetization, excellent magnetic anisotropy, excellent absorbing performance and simple preparation method, and is suitable for industrialization production.
Description
Technical field
The invention belongs to absorbing material technical field is and in particular to a kind of silicone oil magnetic fluid based on carboxyl siloxanes inhales ripple
Material and preparation method.
Background technology
With the fast development of electronic science and technology, electronic countermeasure and antielectronic countermeasures technique become the intersection point of information war,
Electromagnetic-wave absorbent is one of material with fastest developing speed and most widely used in information war stealth material.Electromagnetic-wave absorbent can
So that electromagnetic wave is consumed by the absorption of itself and the effect of decay, reduce to the reflection of electromagnetic wave and scattering, reduce target with
The contrast of the radiation of environment or anti-spectrum reflection differences, reduce the detectivity of target, reach stealthy mesh within the specific limits
's.Additionally, with the editor of other communication systems such as electronics, electrical equipment, also along with more coming the more in daily life
Electromagnetic radiation, excessive electromagnetic radiation all can produce serious threat to the health of the mankind and environment, and therefore absorbing material is to state
Anti- cause and the healthy of people all have important effect.
Magnetic liquid, also known as magnetic fluid, magnetic colloid, ferromagnetic fluids, it is that have nano level magnetic-particle to pass through carboxylic
The dispersion of the interfacial agent height such as base, amido, hydroxyl, aldehyde radical and sulfenyl, be suspended in water, mineral oil, lipid, organic silicone oil,
In the carrier fluid such as fluorine ether oil and mercury, the temperature colloidal dispersion of formation, this colloidal dispersion is not subject to gravity, centrifugal force or high-intensity magnetic field
Impact, can keep system and magnetic stability for a long time.Magnetic liquid belongs to nano wave-absorbing material, has high electromagnetic absorption energy
Power, have that suction wave frequency bandwidth, density is low concurrently, thickness of thin, compatible good the advantages of, but the stability of magnetic liquid directly affects suction
The performance of wave material, in addition some privileged sites of plant equipment also the high temperature resistant aspect of absorbing material is had higher will
Ask.
A kind of method preparing absorbing material using magnetic fluid disclosed in Chinese patent CN 103753881B, by chemistry altogether
After four oxidation three body magnetic nanoparticles of precipitation method preparation are processed through OP-7 surfactant, with oleic acid, kerosene or silicone oil
Be mixed to get ferroferric oxide magnetic fluid, then by ferroferric oxide magnetic fluid and epoxy resin, ethylenediamine, magnetic alloy powder, half
Conductor powder, as raw material, forms composite coating and coated semiconductor respectively, but the composite of the method preparation applies
In layer, ferroferric oxide magnetic fluid magnetic temperature stability is not good, easily causes separation of solid and liquid, directly affects its absorbing property.The present invention
Applicant will be silicone-modified through carboxyl for four oxidation three body magnetic nanoparticle surfaces, then mix with dimethicone and Graphene
Close and prepare the splendid magnetic fluid of stability, the absorbing material of preparation has excellent wave absorbtion based on this magnetic fluid
Can, and light weight, thickness of thin, high temperature resistant, meet the requirement of multiple fields.
Content of the invention
The technical problem to be solved in the present invention be provide a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes and
Preparation method, includes magnetic fluid composite coating and coated semiconductor successively, magnetic fluid composite coating include Fe3O4 nano particle,
Graphene, carboxyl siloxanes, dimethicone, epoxy resin, ethylenediamine and carbonyl nickel powder, carbonyl iron dust or ferrous alloy magnetic
Property powder Alperm powder, coated semiconductor includes epoxy resin, ethylenediamine and semiconductor SiC powder.This absorbing material
Light weight, thickness of thin, magnetic fluid saturation magnetization is high, has excellent magnetic anisotropy, has excellent absorbing property,
And preparation method is simple, suitable industrialized production.
For solving above-mentioned technical problem, the technical scheme is that：
A kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes, the described silicone oil magnetic fluid based on carboxyl siloxanes
Absorbing material includes magnetic fluid composite coating and coated semiconductor, and described magnetic fluid composite coating includes Graphene MODIFIED Fe 3O4
Magnetic fluid, epoxy resin, ethylenediamine and Alperm powder, described coated semiconductor includes epoxy resin, ethylenediamine and half
Conductor SiC powder, described Graphene MODIFIED Fe 3O4 magnetic fluid includes Fe3O4 nano particle, Graphene, carboxyl siloxanes and two
Methyl-silicone oil, the chemical formula of described carboxyl siloxanes is (CH3)3SiO[(CH3)2SiO]x[(CH3)2SiO]ySi CH3)3.
Preferred as technique scheme, described Alperm powder is carbonyl nickel powder, carbonyl iron dust or iron-based
Alloy Magnaglo.
The present invention also provides a kind of preparation method of the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes, including following
Step：
(1) according to mol ratio Fe3+:Fe2+For 1-2:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C surpass
In the there-necked flask of pure water, it is continually fed into rare gas simultaneously in reaction system and discharges air, stir complete to solid particle
After dissolving, according to Fe3+Mol ratio with NaOH is 1:4-10, is rapidly added excessive sodium hydrate aqueous solution, enters simultaneously
Row strong agitation, stirs 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature is adjusted
To 40-70 DEG C, reacting liquid pH value is adjusted to 5-7, then according to Fe3O4Nano magnetic particle with the mass ratio of carboxyl siloxanes is
1-10:1, add carboxyl siloxanes, stir 5-10h, carry out separation of solid and liquid with magnet, and repeatedly clear with ultra-pure water and absolute ethyl alcohol
Wash and obtain dark thick thing, dark thick thing centrifugal drying is ground, obtain the magnetic-particle of carboxyl siloxanes cladding；
(2) disperse graphene in formation graphene dispersing solution in dimethicone, add carboxyl silicon prepared by step (1)
The magnetic-particle of oxygen alkane cladding, mixes at 80-100 DEG C, ultrasonic disperse, obtains MODIFIED Fe 3O4 magnetic fluid, by modification
Fe3O4 magnetic fluid is stirred with epoxy resin, ethylenediamine and Alperm powder, eliminates bubble, forms mixed solution, will
Mixed solution uniform application, on aluminium alloy sheet, adjusts the state of mixing liquid, solidification, forms magnetic fluid composite coating；
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Conductor liquid, the magnetic fluid composite coating surface that semiconductor droplets uniform application is prepared in step (2), solidification, formed and partly lead
Body coating, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Preferred as technique scheme, in described step (1), the chemical formula of carboxyl siloxanes is (CH3)3SiO
[(CH3)2SiO]x[(CH3)2SiO]ySi CH3)3, in shallow bale of straw or limpid liquid, viscosity is 2500cSt, refractive index
Content for 1.408, COOH is 1.3%.
Preferred as technique scheme, in described step (1), the technique that centrifugal drying grinds is：The speed of centrifugation
For 2000rpm, the time of centrifugation is 30min, and the temperature being dried is 40-70 DEG C, and the time is 8-10h, and the equipment of grinding is agate
Mortar, the time of grinding is 30-60min.
Preferred as technique scheme, in described step (2), Graphene and Fe in MODIFIED Fe 3O4 magnetic fluid3O4's
Mass ratio is 1:3-10.
Preferred as technique scheme, in described step (2), MODIFIED Fe 3O4 magnetic fluid, asphalt mixtures modified by epoxy resin in mixed solution
The materials of fat, ethylenediamine and Alperm powder are than for 1ml：0.1-0.8g：0.01-0.1g:0.05-0.2g.
Preferred as technique scheme, in described step (2), the method for adjustment is：By magnet from vertical direction by
, just the phenomenon of magnetic anisotropy to mixing liquid in the lower surface of the remote and nearly aluminium alloy sheet of proximity.
Preferred as technique scheme, in described step (3), component in semiconductor droplets, in percentage terms, bag
Include epoxy resin 45-70%, ethylenediamine 5-15%, semiconductor SiC powder is 15-45%, total amount is 100%.
Preferred as technique scheme, in described step (3), the silicone oil magnetic fluid based on carboxyl siloxanes inhales ripple material
In material, magnetic fluid composite coating and the gross thickness of coated semiconductor are 0.5-0.8mm, magnetic fluid composite coating and coated semiconductor
Thickness be 1:1-2.
Compared with prior art, the invention has the advantages that：
(1) contain in the magnetic fluid composite coating based on the silicone oil magnetic fluid absorbing material of carboxyl siloxanes of present invention preparation
There are Fe3O4 magnetic-particle and the Graphene of carboxyl siloxanes cladding, carboxyl siloxanes one end has and silicone oil identical silica knot
Structure, the carboxyl of the other end can carry out chemisorbed with four oxidation three body nano particles well, makes fundamentally to solve magnetic
Dispersion in organic silicone oil dispersant for the grain and stable problem, the magnetic liquid therefore prepared can keep homogeneous steady for a long time
Fixed, stability is splendid, in addition the presence of Graphene, makes magnetic liquid have excellent mechanics and electric conductivity, can be used as magnetic current
The antisettling agent of body, antiwear additive and lubricant, on the basis of not reducing saturation magnetization, reduce solid content, drop further
The density of low magnetic fluid, improves stability, with dimethicone as carrier fluid, makes magnetic fluid have excellent heat resistance, enter
One step improves the range of absorbing material.
(2) present invention preparation the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes in magnetic fluid composite bed be
In the presence of additional stabilizing magnetic field, magnetic fluid is mixing cured with materials such as resins, make the absorption length of magnetic fluid composite bed big
Big increase, absorption band broadening, absorbing property improves, and adds one layer of carbon containing semiconductor again on the surface of magnetic fluid composite bed
The coated semiconductor of SiClx, improves the absorbing property of material further, had therefore both contained carbon in the absorbing material of present invention preparation
The resistor-type absorbing material such as SiClx and graphite, and contain magnetic fluid and Alperm powder magnetic media type absorbing material,
Absorbing material prepared by the present invention is made to have the wave-absorbing mechanism of complexity, the absorbing material light weight of preparation, thickness of thin, absorption band
Width, absorption length is long, and absorbing property is excellent.
(3) all contain epoxy resin in the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes of present invention preparation, lead to
Cross intensity, toughness, heat resistance and the corrosion resistance that epoxy resin cure gives magnetic fluid composite bed and semiconductor composite layer, improve
The suitable application area of absorbing material.
(4) preparation method of the present invention is simple, product cost low it is adaptable to industrialized production, the absorbing material of preparation
Can be excellent, economic worth is high, and the market competitiveness is strong.
Specific embodiment
To describe the present invention, the illustrative examples of the here present invention and explanation below in conjunction with specific embodiment in detail
It is used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1：
(1) according to mol ratio Fe3+:Fe2+For 1:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C ultrapure
In the there-necked flask of water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir after being completely dissolved to solid particle,
According to Fe3+Mol ratio with NaOH is 1:4, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with the speed of 500rpm
Degree strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature is adjusted to 40
DEG C, reacting liquid pH value is adjusted to 5, then according to Fe3O4Nano magnetic particle is 1 with the mass ratio of carboxyl siloxanes:1, add carboxylic
Radical siloxane, stirs 5h with the speed of 100rpm, carries out separation of solid and liquid with magnet, and be cleaned multiple times with ultra-pure water and absolute ethyl alcohol
To pH be neutrality, obtain dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum drying chamber with
40 DEG C are dried 8h, grind 30min with agate mortar, obtain the magnetic-particle of carboxyl siloxanes cladding.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 5ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 80 DEG C, ultrasonic disperse, obtaining saturation magnetization is 48emu/
The MODIFIED Fe of g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:3, by the MODIFIED Fe of 1ml3O4Magnetic fluid and 0.1g
The Alperm powder of epoxy resin, the ethylenediamine of 0.01g and 0.05g stir, eliminate bubble, form mixing molten
Liquid, by mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to aluminium alloy sheet from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in lower surface, solidification, forms magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 45%, ethylenediamine 10%, semiconductor
SiC powder is 45%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.5mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
1, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Embodiment 2：
(1) according to mol ratio Fe3+:Fe2+For 2:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C ultrapure
In the there-necked flask of water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir after being completely dissolved to solid particle,
According to Fe3+Mol ratio with NaOH is 1:10, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with 1000rpm's
Speed strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature adjust to
70 DEG C, reacting liquid pH value is adjusted to 5-7, then according to Fe3O4Nano magnetic particle is 1-10 with the mass ratio of carboxyl siloxanes:
1, add carboxyl siloxanes, 10h is stirred with the speed of 500rpm, carries out separation of solid and liquid with magnet, and with ultra-pure water and anhydrous second
It is neutrality that alcohol is cleaned multiple times to pH, obtains dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum
10h is dried with 70 DEG C in drying box, grinds 60min with agate mortar, obtain the magnetic-particle of carboxyl siloxanes cladding.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 10ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 100 DEG C, ultrasonic disperse, obtaining saturation magnetization is
The MODIFIED Fe of 57emu/g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:10, by the MODIFIED Fe of 1ml3O4Magnetic fluid
Stir with the Alperm powder of the epoxy resin of 0.8g, the ethylenediamine of 0.1g and 0.2g, eliminate bubble, form mixing
Solution, by mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to aluminium alloy sheet from vertical direction
Lower surface, the phenomenon of magnetic anisotropy just occurs to mixing liquid, solidification, formed magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 70%, ethylenediamine 15%, semiconductor
SiC powder is 15%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.8mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
2, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Embodiment 3：
(1) according to mol ratio Fe3+:Fe2+For 1.5:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C surpass
In the there-necked flask of pure water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir and be completely dissolved to solid particle
Afterwards, according to Fe3+Mol ratio with NaOH is 1:6, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with 800rpm's
Speed strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature adjust to
55 DEG C, reacting liquid pH value is adjusted to 6, then according to Fe3O4Nano magnetic particle is 3 with the mass ratio of carboxyl siloxanes:1, add
Carboxyl siloxanes, stirs 7h with the speed of 200rpm, carries out separation of solid and liquid with magnet, and repeatedly clear with ultra-pure water and absolute ethyl alcohol
Being washed till pH is neutrality, obtains dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum drying chamber
9h is dried with 50 DEG C, grinds 40min with agate mortar, obtain the magnetic-particle of carboxyl siloxanes cladding.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 8ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 90 DEG C, ultrasonic disperse, obtaining saturation magnetization is 51emu/
The MODIFIED Fe of g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:8, by the MODIFIED Fe of 1ml3O4Magnetic fluid and 0.5g
The Alperm powder of epoxy resin, the ethylenediamine of 0.3g and 0.1g stir, eliminate bubble, form mixed solution,
By mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to the following table of aluminium alloy sheet from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in face, solidification, forms magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 55%, ethylenediamine 12%, semiconductor
SiC powder is 33%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.6mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
1.5, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Embodiment 4：
(1) according to mol ratio Fe3+:Fe2+For 1.2:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C surpass
In the there-necked flask of pure water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir and be completely dissolved to solid particle
Afterwards, according to Fe3+Mol ratio with NaOH is 1:5, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with 800rpm's
Speed strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature adjust to
55 DEG C, reacting liquid pH value is adjusted to 5-7, then according to Fe3O4Nano magnetic particle is 8 with the mass ratio of carboxyl siloxanes:1, plus
Enter carboxyl siloxanes, 8h is stirred with the speed of 250rpm, carries out separation of solid and liquid with magnet, and multiple with ultra-pure water and absolute ethyl alcohol
Cleaning to pH is neutrality, obtains dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum drying chamber
In 10h is dried with 50 DEG C, grind 50min with agate mortar, obtain carboxyl siloxanes cladding magnetic-particle.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 7ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 90 DEG C, ultrasonic disperse, obtaining saturation magnetization is 54emu/
The MODIFIED Fe of g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:6, by the MODIFIED Fe of 1ml3O4Magnetic fluid and 0.2g
The Alperm powder of epoxy resin, the ethylenediamine of 0.04g and 0.07g stir, eliminate bubble, form mixing molten
Liquid, by mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to aluminium alloy sheet from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in lower surface, solidification, forms magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 65%, ethylenediamine 8%, semiconductor
SiC powder is 27%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.7mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
1, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Embodiment 5：
(1) according to mol ratio Fe3+:Fe2+For 2:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C ultrapure
In the there-necked flask of water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir after being completely dissolved to solid particle,
According to Fe3+Mol ratio with NaOH is 1:8, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with the speed of 1000rpm
Degree strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature is adjusted to 60
DEG C, reacting liquid pH value is adjusted to 5, then according to Fe3O4Nano magnetic particle is 7 with the mass ratio of carboxyl siloxanes:1, add carboxylic
Radical siloxane, stirs 8h with the speed of 300rpm, carries out separation of solid and liquid with magnet, and be cleaned multiple times with ultra-pure water and absolute ethyl alcohol
To pH be neutrality, obtain dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum drying chamber with
55 DEG C are dried 10h, grind 45min with agate mortar, obtain the magnetic-particle of carboxyl siloxanes cladding.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 10ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 100 DEG C, ultrasonic disperse, obtaining saturation magnetization is
The MODIFIED Fe of 49emu/g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:3, by the MODIFIED Fe of 1ml3O4Magnetic fluid
Stir with the Alperm powder of the epoxy resin of 0.3g, the ethylenediamine of 0.07g and 0.08g, eliminate bubble, formed mixed
Close solution, by mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to aluminum alloy thin from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in the lower surface of plate, solidification, forms magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 65%, ethylenediamine 15%, semiconductor
SiC powder is 20%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.8mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
1, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
Embodiment 6：
(1) according to mol ratio Fe3+:Fe2+For 1:1, by FeCl3·7H2O、FeSO4·6H2O be added to fill 70 DEG C ultrapure
In the there-necked flask of water, it is continually fed into nitrogen simultaneously in reaction system and discharges air, stir after being completely dissolved to solid particle,
According to Fe3+Mol ratio with NaOH is 1:5, it is rapidly added excessive sodium hydrate aqueous solution, simultaneously with the speed of 700rpm
Degree strong agitation 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature is adjusted to 65
DEG C, reacting liquid pH value is adjusted to 6.5, then according to Fe3O4Nano magnetic particle is 8 with the mass ratio of carboxyl siloxanes:1, add
Carboxyl siloxanes, stirs 6h with the speed of 200rpm, carries out separation of solid and liquid with magnet, and repeatedly clear with ultra-pure water and absolute ethyl alcohol
Being washed till pH is neutrality, obtains dark thick thing, by dark thick thing with 2000rpm centrifugation 30min, in vacuum drying chamber
10h is dried with 65 DEG C, grinds 40min with agate mortar, obtain the magnetic-particle of carboxyl siloxanes cladding.
(2) by weight, the graphene dispersion of 1g is formed graphene dispersing solution in the dimethicone of 8ml, plus
Enter the magnetic-particle of carboxyl siloxanes cladding, mix at 90 DEG C, ultrasonic disperse, obtaining saturation magnetization is 52emu/
The MODIFIED Fe of g3O4Magnetic fluid, wherein Graphene and Fe3O4Mass ratio be 1:6, by the MODIFIED Fe of 1ml3O4Magnetic fluid and 0.4g
The Alperm powder of epoxy resin, the ethylenediamine of 0.08g and 0.15g stir, eliminate bubble, form mixing molten
Liquid, by mixed solution uniform application on aluminium alloy sheet, magnet is drawn near close to aluminium alloy sheet from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in lower surface, solidification, forms magnetic fluid composite coating.
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form half
Component in conductor liquid, wherein semiconductor droplets, in percentage terms, including epoxy resin 55%, ethylenediamine 12%, semiconductor
SiC powder is 33%, by semiconductor droplets uniform application in magnetic fluid composite coating surface, solidifies, forms coated semiconductor, magnetic
Fluid composite coating is 0.6mm with the gross thickness of coated semiconductor, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:
2, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
After testing, the reflection of electromagnetic wave of the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes of embodiment 1-6 preparation
Rate, frequency bandwidth result as follows：
As shown in the above, the silicone oil magnetic fluid absorbing material density based on carboxyl siloxanes of present invention preparation is little,
Coating is frivolous, and absorbing property is excellent, and heat resistance is good, and performance is stable for a long time.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes it is characterised in that：Described based on carboxyl siloxanes
Silicone oil magnetic fluid absorbing material includes magnetic fluid composite coating and coated semiconductor, and described magnetic fluid composite coating includes Graphene
MODIFIED Fe 3O4 magnetic fluid, epoxy resin, ethylenediamine and Alperm powder, described coated semiconductor includes epoxy resin, second
Diamines and semiconductor SiC powder, described Graphene MODIFIED Fe 3O4 magnetic fluid includes Fe3O4 nano particle, Graphene, carboxyl silicon
Oxygen alkane and dimethicone, the chemical formula of described carboxyl siloxanes is (CH3)3SiO[(CH3)2SiO]x[(CH3)2 SiO]ySi
CH3)3.
2. a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 1 it is characterised in that：Institute
Stating Alperm powder is carbonyl nickel powder, carbonyl iron dust or ferrous alloy Magnaglo.
3. a kind of preparation method of the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes is it is characterised in that include following walking
Suddenly：
(1) according to mol ratio Fe3+:Fe2+For 1-2:1, by FeCl3·7H2O、FeSO4·6H2O is added to and fills 70 DEG C of ultra-pure waters
There-necked flask in, be continually fed into in reaction system simultaneously rare gas discharge air, stir and be completely dissolved to solid particle
Afterwards, according to Fe3+Mol ratio with NaOH is 1:4-10, is rapidly added excessive sodium hydrate aqueous solution, carries out strong simultaneously
Strong stirring, stirs 30min, obtains Fe3O4Nano magnetic particle solution, by Fe3O4Nano magnetic particle solution temperature adjust to
40-70 DEG C, reacting liquid pH value is adjusted to 5-7, then according to Fe3O4Nano magnetic particle is 1- with the mass ratio of carboxyl siloxanes
10:1, add carboxyl siloxanes, stir 5-10h, carry out separation of solid and liquid with magnet, and be cleaned multiple times with ultra-pure water and absolute ethyl alcohol
Obtain dark thick thing, dark thick thing centrifugal drying is ground, obtain the magnetic-particle of carboxyl siloxanes cladding；
(2) disperse graphene in formation graphene dispersing solution in dimethicone, add carboxyl siloxanes prepared by step (1)
The magnetic-particle of cladding, mixes at 80-100 DEG C, ultrasonic disperse, obtains MODIFIED Fe 3O4 magnetic fluid, by MODIFIED Fe 3O4
Magnetic fluid is stirred with epoxy resin, ethylenediamine and Alperm powder, eliminates bubble, forms mixed solution, will mix
Solution uniform application, on aluminium alloy sheet, adjusts the state of mixing liquid, solidification, forms magnetic fluid composite coating；
(3) ethylenediamine and semiconductor SiC powder will be sequentially added in epoxy resin, stir, eliminate bubble, form semiconductor
Liquid, the magnetic fluid composite coating surface that semiconductor droplets uniform application is prepared in step (2), solidification, form semiconductor and apply
Layer, magnetic fluid composite coating and coated semiconductor constitute the silicone oil magnetic fluid absorbing material based on carboxyl siloxanes.
4. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (1), the chemical formula of carboxyl siloxanes is (CH3)3SiO[(CH3)2SiO]x[(CH3)2 SiO]ySi
CH3)3, in shallow bale of straw or limpid liquid, viscosity is 2500cSt, and refractive index is the content of 1.408, COOH is 1.3%.
5. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (1), the technique that centrifugal drying grinds is：The speed of centrifugation is 2000rpm, and the time of centrifugation is
30min, the temperature being dried is 40-70 DEG C, and the time is 8-10h, and the equipment of grinding is agate mortar, and the time of grinding is 30-
60min.
6. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (2), Graphene and Fe in MODIFIED Fe 3O4 magnetic fluid3O4Mass ratio be 1:3-10.
7. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (2), MODIFIED Fe 3O4 magnetic fluid, epoxy resin, ethylenediamine and Alperm in mixed solution
The materials of powder are than for 1ml：0.1-0.8g：0.01-0.1g:0.05-0.2g.
8. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (2), the method for adjustment is：Magnet is drawn near close to aluminium alloy sheet from vertical direction
, just the phenomenon of magnetic anisotropy to mixing liquid in lower surface.
9. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (3), component in semiconductor droplets, in percentage terms, including epoxy resin 45-70%, second two
Amine 5-15%, semiconductor SiC powder is 15-45%, and total amount is 100%.
10. the preparation method of a kind of silicone oil magnetic fluid absorbing material based on carboxyl siloxanes according to claim 3, its
It is characterised by：In described step (3), based on magnetic fluid composite coating in the silicone oil magnetic fluid absorbing material of carboxyl siloxanes and half
The gross thickness of conductor coatings is 0.5-0.8mm, and magnetic fluid composite coating is 1 with the thickness of coated semiconductor:1-2.
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| CN107393675A (en) * | 2017-07-14 | 2017-11-24 | 四川大学 | A kind of fluorine ether acid@Fe3O4The preparation method of the compound fluorine ether oil based magnetic rheologic liquids of@GO |
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| CN110690579A (en) * | 2019-10-11 | 2020-01-14 | 陕西师范大学 | Preparation method of structural broadband wave-absorbing material based on 3D printing technology |
| CN110797666A (en) * | 2019-11-05 | 2020-02-14 | 南京邮电大学 | Wave absorber regulated and controlled by gravity field and frequency selection function reconfigurable device |
| CN110797666B (en) * | 2019-11-05 | 2021-03-16 | 南京邮电大学 | Wave absorber regulated and controlled by gravity field and frequency selection function reconfigurable device |
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