CN109957274A - A kind of absorbent and preparation method thereof - Google Patents
A kind of absorbent and preparation method thereof Download PDFInfo
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- CN109957274A CN109957274A CN201711408086.1A CN201711408086A CN109957274A CN 109957274 A CN109957274 A CN 109957274A CN 201711408086 A CN201711408086 A CN 201711408086A CN 109957274 A CN109957274 A CN 109957274A
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- 239000002250 absorbent Substances 0.000 title claims abstract description 44
- 230000002745 absorbent Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 50
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000498 ball milling Methods 0.000 claims abstract description 39
- 238000001914 filtration Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000011324 bead Substances 0.000 claims description 12
- 239000000428 dust Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- UMYVESYOFCWRIW-UHFFFAOYSA-N cobalt;methanone Chemical compound O=C=[Co] UMYVESYOFCWRIW-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 5
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 description 11
- 238000006116 polymerization reaction Methods 0.000 description 11
- 239000004793 Polystyrene Substances 0.000 description 10
- 229920002223 polystyrene Polymers 0.000 description 10
- 238000001035 drying Methods 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 8
- 238000003701 mechanical milling Methods 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 4
- 229920006389 polyphenyl polymer Polymers 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000000640 hydroxylating effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The present invention provides a kind of absorbent and preparation method thereof, this method, which is included in ball grinder, is added abrading-ball and Magnaglo, sequentially adds ball-milling medium, styrene, ball milling；And filtering, be absorbed agent.The present invention is combined into one by the way that the flaking process of absorbent is coated process with surface, to avoid the cumbersome technique of first ball milling rear surface processing, and pieces of absorbent agent prepared by the method for the present invention improves the impedance matching of absorbent, it is more excellent in the absorbing property of low frequency (being less than or equal to 5GHz) to make it, and the suction wavestrip widened less than -10dB is wide.
Description
Technical field
The present invention relates to absorbing materials, more particularly, to a kind of absorbent and preparation method thereof.
Background technique
Microwave absorption presses loss mechanism, can be divided into resistor-type, dielectric type and magnetic medium type three categories, wherein with iron oxygen
Body, ultrafine metallic micropowder, carbonyl iron dust etc. are the magnetic medium type absorbing material of representative, have temperature stability can good, microwave magnetic
The advantages that conductance is higher, Curie temperature is higher, it has also become the main direction of development of absorbing material.Both guarantee absorbent to reach
Magnetic conductivity and imaginary part of dielectric constant with higher, and real part of permittivity can be reduced to the greatest extent to obtain the excellent of impedance matching
Change, it usually needs absorbent is surface-treated.Currently, the method being surface-treated to absorbent is mainly: first to carbonyl
Base iron powder implements ball milling, cleans the flaky carbonyl iron powder that ball milling obtains with highly basic and carries out hydroxylating processing, positive four fourth of metatitanic acid is added
Carbonyl iron-TiO is obtained by filtration after ester ultrasonic agitation2Core-shell structure particle, treatment process is cumbersome, needs first ball milling, iron after drying
Powder is added in configured solution and is surface-treated, and is unfavorable for producing in enormous quantities.
Summary of the invention
The present invention while by spherical absorbent flattening, passes through what is generated in mechanical milling process using mechanochemical method
High-energy forms polystyrene layer in absorbent surface in-situ polymerization, its dielectric constant is reduced under the premise of not influencing magnetic conductivity
To improve impedance matching, while the interface that the polymeric membrane of absorbent surface can also improve between polymeric matrix is compatible
Property, its absorbing property is improved, is combined into one by the way that the flaking process of absorbent is coated process with surface, to avoid first ball
Grind the cumbersome technique of rear surface processing.
The present invention provides a kind of methods for preparing absorbent, which comprises
Abrading-ball and Magnaglo are added in ball grinder, sequentially adds ball-milling medium, styrene, ball milling；And filtering,
Be absorbed agent.
In above method, the Magnaglo include carbonyl iron dust, carbonyl cobalt powder, carbonyl nickel powder, in ferrimag powder
It is one or more.
In above method, the abrading-ball includes one of agate bead, stainless shot, zirconium oxide bead or a variety of.
In above method, the abrading-ball and the magnetism are added in the ball grinder by the ratio of grinding media to material of 5:1~40:1
Powder.
In above method, the ball-milling medium includes one of dehydrated alcohol, acetone, hexamethylene or a variety of.
In above method, the quality of the styrene is the 1~5% of the quality of the Magnaglo.
In above method, be added the ball-milling medium to the ball grinder capacity one third to 2/3rds.
In above method, the revolving speed of the ball milling is 250~550rpm.
In above method, the time of the ball milling is 8~48h.
The present invention also provides a kind of absorbents prepared according to above method.
The present invention is combined into one by the way that the flaking process of absorbent is coated process with surface, thus after avoiding first ball milling
The cumbersome technique of surface treatment, and pieces of absorbent agent prepared by the method for the present invention improves the impedance of absorbent
Match, it is more excellent in the absorbing property of low frequency (being less than or equal to 5GHz) to make it, and widened the suction wavestrip less than -10dB
It is wide.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
The styrene that the present invention uses have the advantages that at normal temperature can slow autohemagglutination, pass through absorbent flaking process
Combination with surface cladding process, which is realized, carries out styrene in-situ polymerization in absorbent surface, prepares polystyrene-piece
The absorbent of shape Magnaglo core-shell structure.
The present invention has passed through a kind of method for preparing absorbent, method includes the following steps:
Corrresponding quality abrading-ball and Magnaglo are packed into ball grinder by ratio of grinding media to material 5:1~40:1, ball-milling medium is added to ball
The styrene of Magnaglo quality 1~5%, 250~550rpm ball milling 8 is added to 2/3rds in the one third of grinding jar capacity
~48h is washed three to five times after taking out powder by filtering with dehydrated alcohol, be placed in electric drying oven with forced convection in 70~
100 DEG C are dried to alcohol and volatilize completely, obtain the sheet-like magnetic powdery absorbent of polystyrene cladding；Wherein, the Magnaglo
Including but not limited to one of carbonyl iron dust, carbonyl cobalt powder, carbonyl nickel powder, ferrimag powder (such as FeSiAl powder) or a variety of；
Abrading-ball includes but is not limited to one of agate bead, stainless shot, zirconium oxide bead or a variety of；Ball-milling medium includes but is not limited to nothing
One of water-ethanol, acetone, hexamethylene are a variety of.
In above method, using one of the ratio of grinding media to material and dehydrated alcohol of 5:1~40:1, acetone, hexamethylene or
The wet ball grinding technique of a variety of ball-milling mediums, the wet ball grinding technique that the present invention uses effectively reduce Magnaglo slimeball
Probability improves ball milling speed, and shortens Ball-milling Time.
In above method, the quality of styrene is the 1~5% of the quality of Magnaglo, so that by magnetic absorbent
The polymerization for causing styrene monomer while flaking using the huge energy generated in mechanical milling process, makes it in Magnaglo
In situ Polymerization generates polystyrene clad, so that the absorbent of preparation is become hydrophobic, is conducive to improve it in polymer matrix
Compatibility and dispersing uniformity in body improve its absorbing property to increase the loading of the absorbent；If styrene
Additive amount is excessive, then the clad formed in mechanical milling process on Magnaglo surface is blocked up, influences the final suction wave frequency of absorbent
Point and bandwidth, if styrene additive amount is very few, the styrene of in-situ polymerization may not coated magnetic powder surface, from
And the absorbing property of absorbent cannot be effectively improved.
In above method, 8~48h of ball milling under the revolving speed of 250~550rpm, if rotational speed of ball-mill is too big, such as larger than
550rpm is then difficult to control the ball milling to Magnaglo；Rotational speed of ball-mill is too small, such as less than 250rpm, then cannot be preferably to magnetic
Property powder carry out ball milling；If Ball-milling Time is too short, such as less than 8h, then Magnaglo flattening limitation, and styrene
The in-situ polymerization of monomer is insufficient, so that polystyrene clad cannot be generated in Magnaglo in situ Polymerization；If ball
Consume time too long, such as larger than 48h, then can destroy the sheet-like magnetic powder of the polystyrene cladding of generation, therefore, when 250~
Under the revolving speed of 550rpm when 8~48h of ball milling, it can guarantee to produce while by magnetic absorbent flaking using in mechanical milling process
Raw huge energy causes the polymerization of styrene monomer, so that it is generated polystyrene cladding in Magnaglo in situ Polymerization
Layer.
Embodiment 1
The zirconium oxide bead of corrresponding quality and carbonyl iron dust are packed into ball grinder by ratio of grinding media to material 5:1, dehydrated alcohol is added to ball
2/3rds of grinding jar capacity, are added the styrene of carbonyl iron dust quality 1%, and 250rpm ball milling 8h takes out powder by filtering
Later, it is washed three times with dehydrated alcohol, is placed in electric drying oven with forced convection and is dried to alcohol in 70 DEG C and volatilizees completely, obtain polyphenyl
The flaky carbonyl iron powder absorbent of ethylene cladding.
Embodiment 2
The zirconium oxide bead of corrresponding quality and carbonyl iron dust are packed into ball grinder by ratio of grinding media to material 20:1, dehydrated alcohol is added to ball
2/3rds of grinding jar capacity, are added the styrene of carbonyl iron dust quality 3%, and 400rpm ball milling takes out powder for 24 hours, by filtering
Later, it is washed three times with dehydrated alcohol, is placed in electric drying oven with forced convection and is dried to alcohol in 70 DEG C and volatilizees completely, obtain polyphenyl
The flaky carbonyl iron powder absorbent of ethylene cladding.
Embodiment 3
The zirconium oxide bead of corrresponding quality and carbonyl iron dust are packed into ball grinder by ratio of grinding media to material 40:1, dehydrated alcohol is added to ball
2/3rds of grinding jar capacity, are added the styrene of carbonyl iron dust quality 5%, and 550rpm ball milling 48h takes out powder by filtering
Later, it is washed three times with dehydrated alcohol, is placed in electric drying oven with forced convection and is dried to alcohol in 70 DEG C and volatilizees completely, obtain polyphenyl
The flaky carbonyl iron powder absorbent of ethylene cladding.
Embodiment 4
The zirconium oxide bead of corrresponding quality and agate bead (mass ratio 1:1) and carbonyl nickel powder are packed into ball by ratio of grinding media to material 5:1
Grinding jar is added dehydrated alcohol and acetone (mass ratio 1:1) to 2/3rds of ball milling tankage size, carbonyl nickel powder quality is added
1% styrene, 350rpm ball milling 8h are washed three times with dehydrated alcohol after taking out powder by filtering, are placed in electric heating air blast
Alcohol is dried in 80 DEG C in drying box to volatilize completely, obtains the sheet carbonyl nickel powder absorbent of polystyrene cladding.
Embodiment 5
The stainless shot of corrresponding quality and FeSiAl powder are packed into ball grinder by ratio of grinding media to material 10:1, hexamethylene is added to ball milling
The one third of tankage size, be added FeSiAl silty amount 4% styrene, 450rpm ball milling 23h, by filtering take out powder it
Afterwards, it is washed five times with dehydrated alcohol, is placed in electric drying oven with forced convection and is dried to alcohol in 90 DEG C and volatilizees completely, obtain polyphenyl second
The sheet FeSiAl powder absorbent of alkene cladding.
Embodiment 6
The agate bead of corrresponding quality and carbonyl cobalt powder are packed into ball grinder by ratio of grinding media to material 30:1, acetone to ball grinder is added and holds
The half of amount, the styrene of addition carbonyl cobalt silty amount 5%, 550rpm ball milling 48h, after taking out powder by filtering,
It is washed four times with dehydrated alcohol, is placed in electric drying oven with forced convection and is dried to alcohol in 100 DEG C and volatilizees completely, obtain polystyrene
The sheet carbonyl cobalt powder absorbent of cladding.
Absorbent obtained in embodiment 1 to embodiment 6 and paraffin 8.5:1.5 in mass ratio are heated after mixing,
Internal diameter is pressed into grinding tool to be 3.04mm, carry out electromagnetic performance within the scope of 1~18GHz with a thickness of the coaxial rings sample of 2~4mm
Test, and the reflection loss RL curve with a thickness of 1.5mm sample is simulated using resulting electromagnetic parameter, test result is seen below
Table 1:
Table 1
| Embodiment | Frequency at peak value | Reflection loss at peak value | The suction wavestrip of < -10dB is wide |
| 1 | 4.3GHz | -20.4dB | 1.86GHz |
| 2 | 2.8GHz | -22.6dB | 1.51GHz |
| 3 | 2.1GHz | -28.2dB | 1.26GHz |
| 4 | 2.5GHz | -32.6dB | 0.98GHz |
| 5 | 2.2GHz | -31.2dB | 1.72GHz |
| 6 | 2.6GHz | -28.6dB | 0.99GHz |
By upper table 1 it is found that absorbent prepared by the method for the present invention is realized (is less than or equal in low frequency
5GHz) the high-selenium corn in range so that the reflection loss at its peak value is below -20dB, and has widened the suction less than -10dB
Wavestrip is wide, so that it inhales the wide up to 1.86GHz of wavestrip, this is because method of the invention is by magnetic absorbent flaking
The polymerization for causing styrene monomer using the huge energy generated in mechanical milling process simultaneously, makes it in Magnaglo surface in situ
Polymerization generates polystyrene clad, and the polystyrene clad of formation reduces the dielectric constant of absorbent, improves impedance
Matching, and absorbent is made to become hydrophobic, be conducive to improve its compatibility and dispersing uniformity in a polymer matrix, increase
Loading is realized in low frequency (be less than or equal to 5GHz) with, to the good absorption of microwave, and having widened suction wavestrip in range
It is wide.
In addition, method of the invention, ball milling and cladding are combined, the complexity of process is reduced.
It can be applied to such as rubber wave absorbing patch, antiradar coatings microwave absorbing material field.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit of the invention
In the case where range, a variety of variations can be carried out, replaced and changed.
Claims (10)
1. a kind of method for preparing absorbent, which is characterized in that the described method includes:
Abrading-ball and Magnaglo are added in ball grinder, sequentially adds ball-milling medium, styrene, ball milling；And filtering, it obtains
Absorbent.
2. the method according to claim 1, wherein the Magnaglo includes carbonyl iron dust, carbonyl cobalt powder, carbonyl
One of base nickel powder, ferrimag powder are a variety of.
3. the method according to claim 1, wherein the abrading-ball includes agate bead, stainless shot, zirconium oxide bead
One of or it is a variety of.
4. the method according to claim 1, wherein adding in the ball grinder by the ratio of grinding media to material of 5:1~40:1
Enter the abrading-ball and the Magnaglo.
5. the method according to claim 1, wherein the ball-milling medium includes dehydrated alcohol, acetone, hexamethylene
One of or it is a variety of.
6. the method according to claim 1, wherein the quality of the styrene is the quality of the Magnaglo
1~5%.
7. the method according to claim 1, wherein be added the ball-milling medium to the ball grinder capacity
One third is to 2/3rds.
8. the method according to claim 1, wherein the revolving speed of the ball milling is 250~550rpm.
9. the method according to claim 1, wherein the time of the ball milling is 8~48h.
10. a kind of absorbent of method according to claim 1 to 9 preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711408086.1A CN109957274A (en) | 2017-12-22 | 2017-12-22 | A kind of absorbent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711408086.1A CN109957274A (en) | 2017-12-22 | 2017-12-22 | A kind of absorbent and preparation method thereof |
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Family
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Cited By (5)
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| CN110982421A (en) * | 2019-11-08 | 2020-04-10 | 航天科工武汉磁电有限责任公司 | High-temperature-resistant wave-absorbing coating and preparation method thereof |
| CN111001549A (en) * | 2019-12-11 | 2020-04-14 | 中国航空制造技术研究院 | Preparation method of corrosion-resistant wave-absorbing coating containing core-shell structure type magnetic absorbent |
| CN112071618A (en) * | 2020-08-28 | 2020-12-11 | 南京大学 | Preparation method of iron-silicon-aluminum sheet magnetic powder with surface insulated and coated with titanium dioxide |
| CN112191852A (en) * | 2020-09-14 | 2021-01-08 | 南京航空航天大学 | Preparation method of weather-resistant electromagnetic wave absorption layer/plate |
| CN114101685A (en) * | 2021-09-29 | 2022-03-01 | 北京环境特性研究所 | Low-frequency radar wave absorbent and preparation method thereof |
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| CN111001549B (en) * | 2019-12-11 | 2022-03-04 | 中国航空制造技术研究院 | Preparation method of corrosion-resistant wave-absorbing coating containing core-shell structure type magnetic absorbent |
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| CN112191852A (en) * | 2020-09-14 | 2021-01-08 | 南京航空航天大学 | Preparation method of weather-resistant electromagnetic wave absorption layer/plate |
| CN112191852B (en) * | 2020-09-14 | 2021-07-13 | 南京航空航天大学 | Preparation method of weather-resistant electromagnetic wave absorption layer/plate |
| CN114101685A (en) * | 2021-09-29 | 2022-03-01 | 北京环境特性研究所 | Low-frequency radar wave absorbent and preparation method thereof |
| CN114101685B (en) * | 2021-09-29 | 2023-06-09 | 北京环境特性研究所 | Low-frequency radar wave absorbent and preparation method thereof |
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