CN109575202A - A kind of composite wave-suction material and preparation method thereof - Google Patents
A kind of composite wave-suction material and preparation method thereof Download PDFInfo
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- CN109575202A CN109575202A CN201710896511.XA CN201710896511A CN109575202A CN 109575202 A CN109575202 A CN 109575202A CN 201710896511 A CN201710896511 A CN 201710896511A CN 109575202 A CN109575202 A CN 109575202A
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- carbonyl iron
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- composite wave
- modified carbonyl
- coupling agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- 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
Abstract
The present invention provides a kind of composite wave-suction materials and preparation method thereof, this method comprises: carbonyl iron dust is mixed with silane coupling agent, react, and obtain the modified carbonyl iron particles in surface；The modified carbonyl iron particles in surface are ground, modified carbonyl iron powder is obtained；And modified carbonyl iron powder is added in solvent, methyl methacrylate is added, temperature T is warming up to, initiator is added, insulation reaction is carried out at temperature T, obtains composite wave-suction material.The absorbing property for effectively increasing composite wave-suction material by means of the present invention has widened effective suction wave frequency band of composite wave-suction material；And preparation process is simple, is easy design, can be applied to the numerous areas such as aerospace, ship naval vessels and radar antenna, electronic shield.
Description
Technical field
The present invention relates to absorbing material fields, more particularly, to a kind of composite wave-suction material and preparation method thereof.
Background technique
Carbonyl iron wave absorbing agent is presently the most one of common radar absorbent material, is a kind of typical magnetic loss type suction wave material
Material, magnetic loss angle use in the microwave band for being higher than superhigh frequency band up to 40 ° or so, are a kind of good electro-magnetic wave absorptions
Agent.But there is also some disadvantages simultaneously for it, and such as: corrosion resistance is poor；Dielectric constant is big and spectral characteristic is poor, low frequency absorbent properties compared with
Difference；Density is larger, and absorbent volume duty ratio is big, is difficult to disperse, and long-term place is easy to happen oxidation in air.Carbonyl iron
The diameter very little of grain, oxidation will cause the loss for effectively inhaling wave component, cause the reduction of absorbing property.Single absorbing material is very
Difficulty meets the characteristics of high-performance absorbs.
Currently, using double-coating core-shell structure in the prior art to overcome the above problem, this is needed by twice
Polymerization reaction, technique is relatively complicated, and absorbing property is not high, it is relatively narrow to inhale wave frequency band.
Summary of the invention
In view of the above problems, the present invention is by being modified carbonyl iron dust with wet process, that is, carried out to carbonyl iron dust surface
It is modified, modified carbonyl iron powder is obtained, the carbonyl iron dust of methyl methacrylate after modification is made using in-situ compound technology later
Polymerization reaction occurs for surface.
The present invention provides a kind of methods for preparing composite wave-suction material, comprising:
Carbonyl iron dust is mixed with silane coupling agent, is reacted, the modified carbonyl iron particles in surface are obtained；The surface is changed
The carbonyl iron particles of property are ground, and modified carbonyl iron powder is obtained；And the modified carbonyl iron powder is added in solvent, then
Methyl methacrylate is added, is warming up to temperature T, initiator is added, carries out insulation reaction at the temperature T, obtains compound
Absorbing material.
In the above-mentioned methods, the mass ratio of the carbonyl iron dust and the silane coupling agent is 50~80:3~15.
In the above-mentioned methods, the silane coupling agent includes A-1100 (gamma-aminopropyl-triethoxy-silane), A-187
One kind of (γ-glycidyl ether oxygen propyl trimethoxy silicane) and A-172 (vinyl-three (2- methoxy ethoxy) silane)
Or it is a variety of.
In the above-mentioned methods, further includes: before carbonyl iron dust is reacted with silane coupling agent, in 40~60 DEG C of water-bath
Carry out 30~90min of ultrasonic disperse.
In the above-mentioned methods, the time that carbonyl iron dust is reacted with silane coupling agent is 40~60min.
In the above-mentioned methods, the temperature that carbonyl iron dust is reacted with silane coupling agent is room temperature.
In the above-mentioned methods, the time of the grinding is 20~48h.
In the above-mentioned methods, the solvent includes the one or two of ethyl acetate and toluene.
In the above-mentioned methods, the mass ratio of the modified carbonyl iron powder and methyl methacrylate is 30~60:40~65.
In the above-mentioned methods, the temperature T is 60~70 DEG C.
In the above-mentioned methods, the initiator includes one kind or two of Ammonium Persulfate 98.5 aqueous solution and persulfate aqueous solution
Kind.
In the above-mentioned methods, the time of the insulation reaction is 1~3h.
The present invention also provides a kind of composite wave-suction materials prepared according to the above method.
The present invention is modified carbonyl iron dust surface, improves carbonyl by being modified to carbonyl iron dust with wet process
The oxidation resistance and dispersibility of iron powder, while methyl methacrylate (MMA) is made after modification using in-situ compound technology
Carbonyl iron dust surface carries out polymerization reaction, and inorganic magnetic absorbing material is compound with polymer polyol, effectively increases composite wood
The absorbing property of material has widened effective suction wave frequency band of composite wave-suction material, and excellent with simple process, easy design etc.
Point.
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 present invention obtains modified carbonyl iron powder by organosilan surface modified carbonyl iron powder, improves the anti-of carbonyl iron dust
Oxidability and dispersibility, that is, mix carbonyl iron dust by certain mass ratio with silane coupling agent, in 40~60 DEG C of water-bath
30~60min of ultrasonic disperse is carried out, is dispersed in carbonyl iron dust in silane coupler solution, so that carbonyl iron dust can be by
Uniformly cladding, later, 40~60min of normal-temperature reaction is filtered (with the filter paper of 80~120 micron pore sizes), obtained solid is spent
Ionized water or distilled water repeatedly wash, dry 10~12h in 80~120 DEG C of baking oven, obtain the modified carbonyl iron in surface
Grain；Later, the modified carbonyl iron particles in surface are placed in 20~48h of grinding in ball mill, obtain modified carbonyl iron powder；Wherein,
The mass ratio of carbonyl iron dust and silane coupling agent is that 50~80:3~15 cannot be preferable when the dosage of silane coupling agent is less
Ground dispersion and modified carbonyl iron powder, when the dosage of silane coupling agent is more, excessive silane coupling agent can reduce modified carbonyl
The absorbing property of iron powder, therefore, when the mass ratio of carbonyl iron dust and silane coupling agent is in 50~80:3~15 ranges, preparation
Modified carbonyl iron powder absorbing property it is best；Silane coupling agent includes A-1100 (gamma-aminopropyl-triethoxy-silane), A-
187 (γ's-glycidyl ether oxygen propyl trimethoxy silicane) and A-172 (vinyl-three (2- methoxy ethoxy) silane)
It is one or more.
Later, the present invention makes the carbonyl iron of methyl methacrylate (MMA) after modification by using in-situ compound technology
Powder surface reacts, that is, modified carbonyl iron powder is added to solvent, and (solvent includes one kind or two of ethyl acetate and toluene
Kind, the additive amount of solvent can disperse carbonyl iron dust) in, 20~30min of ultrasonic disperse simultaneously stirs 1~2h, MMA is added,
Temperature is risen to 60~70 DEG C, the Ammonium Persulfate 98.5 of a small amount of (for example, be less than modified carbonyl iron powder and MMA gross mass 5%) is added
The initiators initiation reaction such as aqueous solution, persulfate aqueous solution carries out 1~3h of insulation reaction at 60~70 DEG C, filters (with 80
The filter paper of~120 micron pore sizes), by obtained solid hydrochloric acid (mass fraction be lower than 20% dilute hydrochloric acid) and distilled water or go from
Sub- water cleaning is placed on 10~12h of drying in 80~120 DEG C of baking oven, grinds 20~48h in ball mill to get modified carbonyl is arrived
Iron powder/polymethyl methacrylate (PMMA) composite wave-suction material；Wherein, modified carbonyl iron powder and methyl methacrylate
(MMA) mass ratio is 30~60:40~65, when the mass ratio of modified carbonyl iron powder and methyl methacrylate is 30~60:
When in the range of 40~65, modified carbonyl iron powder can be effectively compounded to form with methyl methacrylate to be inhaled wave frequency bandwidth, inhales wave
The good modified carbonyl iron powder/PMMA composite wave-suction material of performance, when the mass ratio of modified carbonyl iron powder and methyl methacrylate
When except the range of 30~60:40~65, excessive carbonyl iron dust or methyl methacrylate will affect composite wave-suction material
Absorbing property, to reduce modified carbonyl iron powder/PMMA composite wave-suction material absorbing property.
Embodiment 1
50 parts of carbonyl iron dusts are mixed with 3 parts of A-1100 silane coupler solutions, carry out ultrasonic disperse in 40 DEG C of water-baths
30min is uniformly dispersed in iron powder in solution, normal-temperature reaction 40min, and filtering repeatedly washes obtained solid with deionized water
It washs, dry, the modified carbonyl iron particles in surface are made；The modified carbonyl iron particles in surface are placed in ball mill and grind 20h, are obtained
To modified carbonyl iron powder；
30 parts of modified carbonyl iron powders are added in ethyl acetate solution, ultrasonic disperse simultaneously stirs, and adds 50 parts of methyl
Methyl acrylate, temperature rise to 60 DEG C, and the initiation reaction of Ammonium Persulfate 98.5 aqueous solution, 60 DEG C of insulation reaction 1.5h, filtering, by institute is added
It obtains solid hydrochloric acid and distilled water is cleaned to be placed in 80 DEG C of baking ovens in dry, ball mill and be ground, modified carbonyl iron can be obtained
Powder/PMMA composite wave-suction material.
Embodiment 2
60 parts of carbonyl iron dusts are mixed with 8 parts of A-187 silane coupler solutions, carry out ultrasonic disperse in 50 DEG C of water-baths
60min is uniformly dispersed in iron powder in solution, normal-temperature reaction 60min, and filtering repeatedly washes obtained solid with deionized water
It washs, dry, the modified carbonyl iron particles in surface are made；The modified carbonyl iron particles in surface are placed in ball mill and grind 28h, are obtained
To modified carbonyl iron powder；
40 parts of modified carbonyl iron powders are added in ethyl acetate solution, ultrasonic disperse simultaneously stirs, and adds 60 parts of methyl
Methyl acrylate, temperature rise to 65 DEG C, and the initiation reaction of Ammonium Persulfate 98.5 aqueous solution, 65 DEG C of insulation reaction 2h, filtering, by gained is added
Solid hydrochloric acid and distilled water are cleaned to be placed in 100 DEG C of baking ovens in dry, ball mill and be ground, and modified carbonyl iron can be obtained
Powder/PMMA composite wave-suction material.
Embodiment 3
65 parts of carbonyl iron dusts are mixed with 10 parts of A-172 silane coupler solutions, carry out ultrasonic disperse in 55 DEG C of water-baths
80min is uniformly dispersed in iron powder in solution, normal-temperature reaction 50min, and filtering repeatedly washes obtained solid with deionized water
It washs, dry, the modified carbonyl iron particles in surface are made；The modified carbonyl iron particles in surface are placed in ball mill and grind 36h, are obtained
To modified carbonyl iron powder；
50 parts of modified carbonyl iron powders are added in toluene solution, ultrasonic disperse simultaneously stirs, and adds 65 parts of metering systems
Sour methyl esters, temperature rise to 63 DEG C, and persulfate aqueous solution initiation reaction, 65 DEG C of insulation reaction 2.5h is added, and gained is consolidated in filtering
Body hydrochloric acid and distilled water are cleaned to be placed in 100 DEG C of baking ovens in dry, ball mill and be ground, can be obtained modified carbonyl iron powder/
PMMA composite wave-suction material.
Embodiment 4
70 parts of carbonyl iron dusts are mixed with 15 parts of A-187 silane coupler solutions, carry out ultrasonic disperse in 55 DEG C of water-baths
90min is uniformly dispersed in iron powder in solution, normal-temperature reaction 60min, and filtering repeatedly washes obtained solid with deionized water
It washs, dry, the modified carbonyl iron particles in surface are made；The modified carbonyl iron particles in surface are placed in ball mill and grind 40h, are obtained
To modified carbonyl iron powder；
60 parts of modified carbonyl iron powders are added in ethyl acetate solution, ultrasonic disperse simultaneously stirs, and adds 40 parts of methyl
Methyl acrylate, temperature rise to 65 DEG C, and the initiation reaction of Ammonium Persulfate 98.5 aqueous solution, 65 DEG C of insulation reaction 1h, filtering, by gained is added
Solid hydrochloric acid and distilled water are cleaned to be placed in 120 DEG C of baking ovens in dry, ball mill and be ground, and modified carbonyl iron can be obtained
Powder/PMMA composite wave-suction material.
Embodiment 5
80 parts of carbonyl iron dusts are mixed with 15 parts of A-187 silane coupler solutions, carry out ultrasonic disperse in 60 DEG C of water-baths
90min is uniformly dispersed in iron powder in solution, normal-temperature reaction 60min, and filtering repeatedly washes obtained solid with deionized water
It washs, dry, the modified carbonyl iron particles in surface are made；The modified carbonyl iron particles in surface are placed in ball mill and grind 48h, are obtained
To modified carbonyl iron powder；
50 parts of modified carbonyl iron powders are added in toluene solution, ultrasonic disperse simultaneously stirs, and adds 50 parts of metering systems
Sour methyl esters, temperature rise to 65 DEG C, and Ammonium Persulfate 98.5 aqueous solution and persulfate aqueous solution initiation reaction, 65 DEG C of insulation reactions are added
Obtained solid hydrochloric acid and distilled water are cleaned to be placed in 120 DEG C of baking ovens in dry, ball mill and be ground, can obtained by 2h, filtering
To modified carbonyl iron powder/PMMA composite wave-suction material.
Embodiment 6
70 parts of carbonyl iron dusts are mixed with 7 parts of A-187 silane coupler solutions and 6 parts of A-1100 silane coupler solutions,
Ultrasonic disperse 80min is carried out in 50 DEG C of water-baths, is uniformly dispersed in iron powder in solution, and normal-temperature reaction 55min is filtered, will
Obtained solid is repeatedly washed with deionized water, is dry, and the modified carbonyl iron particles in surface are made；By the modified carbonyl iron in surface
Grain, which is placed in ball mill, grinds 28h, obtains modified carbonyl iron powder；
40 parts of modified carbonyl iron powders are added in the mixed solution of ethyl acetate and toluene, ultrasonic disperse simultaneously stirs, then
60 parts of methyl methacrylates are added, temperature rises to 70 DEG C, and persulfate aqueous solution initiation reaction, 65 DEG C of insulation reactions are added
Obtained solid hydrochloric acid and distilled water are cleaned to be placed in 80 DEG C of baking ovens in dry, ball mill and be ground, can obtained by 3h, filtering
To modified carbonyl iron powder/PMMA composite wave-suction material.
The above score is parts by weight, and the power of the above ultrasonic disperse is 600~900W；The revolving speed stirred above is
400~600r/min, the above grinding are all made of QM planetary ball mill using grinder.
By modified carbonyl iron powder/PMMA composite wave-suction material of the embodiment 1 into embodiment 6 and paraffin according to mass ratio
70:30 is uniformly mixed, and is cast, is solidified and suppresses.Using waveguide method commonly used in the art in Agilent microwave vector network point
Complex dielectric permittivity ε γ and complex permeability μ γ of the composite wave-suction material sample in 2~18GHz wave band are tested in analyzer.Utilize meter
Calculation machine auxiliary is calculated and is simulated with a thickness of the absorbing property of 1mm absorbing material, calculates and analog result see the table below 1:
Table 1
As it can be seen from table 1 the present invention is by being modified carbonyl iron dust with wet process, that is, disperse carbonyl iron dust in
In silane coupling agent, then by ultrasonic disperse in water-bath, it is dispersed in carbonyl iron dust in silane coupler solution, by having
The silane surface modified carbonyl iron dust of machine, obtains modified carbonyl iron powder, improves the oxidation resistance and dispersibility of carbonyl iron dust, then leads to
Cross keeps modified carbonyl iron powder compound with methyl methacrylate using in-situ compound technology, effectively increases composite wave-suction material
Absorbing property has widened effective suction wave frequency band of composite wave-suction material, so that frequency of the composite wave-suction material in 2~18GHz
Reflectivity in range is down to -24.08dB；And preparation process is simple, is easy design, can be applied to aerospace, ship warship
The numerous areas such as ship and radar antenna, electronic shield.
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 (13)
1. a kind of method for preparing composite wave-suction material characterized by comprising
Carbonyl iron dust is mixed with silane coupling agent, is reacted, the modified carbonyl iron particles in surface are obtained；
The modified carbonyl iron particles in the surface are ground, modified carbonyl iron powder is obtained；And
The modified carbonyl iron powder is added in solvent, methyl methacrylate is added, is warming up to temperature T, is added and causes
Agent carries out insulation reaction at the temperature T, obtains composite wave-suction material.
2. the method according to claim 1, wherein the mass ratio of the carbonyl iron dust and the silane coupling agent
For 50~80:3~15.
3. according to the method described in claim 2, it is characterized in that, the silane coupling agent includes A-1100, A-187 and A-
172 it is one or more.
4. the method according to claim 1, wherein further include: it is reacted with silane coupling agent in carbonyl iron dust
Before, 30~90min of ultrasonic disperse is carried out in 40~60 DEG C of water-bath.
5. the method according to claim 1, wherein time for being reacted with silane coupling agent of carbonyl iron dust be 40~
60min。
6. the method according to claim 1, wherein the temperature that carbonyl iron dust is reacted with silane coupling agent is normal
Temperature.
7. the method according to claim 1, wherein the time of the grinding is 20~48h.
8. the method according to claim 1, wherein the solvent includes one kind or two of ethyl acetate and toluene
Kind.
9. the method according to claim 1, wherein the matter of the modified carbonyl iron powder and methyl methacrylate
Amount is than being 30~60:40~65.
10. the method according to claim 1, wherein the temperature T is 60~70 DEG C.
11. the method according to claim 1, wherein the initiator includes Ammonium Persulfate 98.5 aqueous solution and over cure
The one or two of sour aqueous solutions of potassium.
12. the method according to claim 1, wherein the time of the insulation reaction is 1~3h.
13. a kind of composite wave-suction material of the preparation of method described in any one of -12 according to claim 1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029480A (en) * | 2020-08-24 | 2020-12-04 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN113583352A (en) * | 2021-08-19 | 2021-11-02 | 南京冠旭新材料科技有限公司 | Wave-absorbing patch and preparation method thereof |
| CN113921359A (en) * | 2021-08-16 | 2022-01-11 | 江汉大学 | Surface modification method of wave absorbing material |
| CN114316509A (en) * | 2021-12-29 | 2022-04-12 | 电子科技大学 | PEEK-based composite wave-absorbing 3D printing wire material and preparation method thereof |
| CN114314681A (en) * | 2021-12-23 | 2022-04-12 | 航天科工武汉磁电有限责任公司 | Preparation method of silicon dioxide coated carbonyl iron material |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
| CN113921359B (en) * | 2021-08-16 | 2024-04-26 | 江汉大学 | Surface modification method of wave-absorbing material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029480A (en) * | 2020-08-24 | 2020-12-04 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN112029480B (en) * | 2020-08-24 | 2021-09-24 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN113921359A (en) * | 2021-08-16 | 2022-01-11 | 江汉大学 | Surface modification method of wave absorbing material |
| CN113921359B (en) * | 2021-08-16 | 2024-04-26 | 江汉大学 | Surface modification method of wave-absorbing material |
| CN113583352A (en) * | 2021-08-19 | 2021-11-02 | 南京冠旭新材料科技有限公司 | Wave-absorbing patch and preparation method thereof |
| CN114314681A (en) * | 2021-12-23 | 2022-04-12 | 航天科工武汉磁电有限责任公司 | Preparation method of silicon dioxide coated carbonyl iron material |
| CN114316509A (en) * | 2021-12-29 | 2022-04-12 | 电子科技大学 | PEEK-based composite wave-absorbing 3D printing wire material and preparation method thereof |
| CN114316509B (en) * | 2021-12-29 | 2023-08-08 | 电子科技大学 | PEEK-based composite wave-absorbing 3D printing wire and preparation method thereof |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
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Application publication date: 20190405 |