CN109207121A - 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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- CN109207121A CN109207121A CN201710516161.XA CN201710516161A CN109207121A CN 109207121 A CN109207121 A CN 109207121A CN 201710516161 A CN201710516161 A CN 201710516161A CN 109207121 A CN109207121 A CN 109207121A
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- graphene oxide
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- iron powder
- composite wave
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 46
- 239000006185 dispersion Substances 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000077 silane Inorganic materials 0.000 claims abstract description 17
- 239000000428 dust Substances 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000011358 absorbing material Substances 0.000 abstract description 10
- 239000012265 solid product Substances 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 26
- 230000005291 magnetic effect Effects 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 235000019441 ethanol Nutrition 0.000 description 13
- 238000007254 oxidation reaction Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 240000008042 Zea mays Species 0.000 description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 235000005822 corn Nutrition 0.000 description 3
- -1 deionized water modified carbonyl iron powder Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Substances [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- MRLBXVQKUIIMQT-UHFFFAOYSA-N N-[[dimethoxy(propyl)silyl]oxymethyl]ethanamine Chemical compound C(C)NCO[Si](OC)(OC)CCC MRLBXVQKUIIMQT-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
Abstract
The present invention provides a kind of composite wave-suction materials and preparation method thereof, comprising: carbonyl iron dust is added in silane coupler solution, adds ammonium hydroxide and deionized water, dispersion, separation clean solid product, obtain modified carbonyl iron powder；And mix graphene oxide dispersion with the modified carbonyl iron powder, it separates, obtains the composite wave-suction material.The composite wave-suction material can satisfy thin, light, wide, the strong requirement of absorbing material, can be applied to the numerous areas such as aerospace, ship naval vessels, radar antenna and electronic shield.
Description
Technical field
The present invention relates to Material Fields, more particularly, to a kind of composite wave-suction material and preparation method thereof.
Background technique
Carbonyl iron dust is widely used in absorbing material field, is a kind of typical magnetic loss type absorbing material, but respectively to same
Property spherical carbonyl iron powder absorbent density it is big, acid and alkali-resistance, oxidation resistance is poor, dielectric constant is big and spectral characteristic is poor, magnetic conductance
Rate is low, disadvantage poor with the impedance matching property of air and relatively narrow absorption band, it is difficult to realize absorbing material in wider frequency
High-selenium corn under rate is unable to reach the excellent requirement of absorbing material performance, limits its application to a certain extent.
Therefore, it is high and inhale the Wave suction composite material of wave frequency bandwidth to be badly in need of studying a kind of reflection loss, inhales wave material to meet
Thin, light, wide, the strong requirement of material.
Summary of the invention
The present invention is by being modified carbonyl iron dust in silane coupler solution, by the way that ammonium hydroxide, deionized water is added
Etc. obtaining modified carbonyl iron powder, and graphene oxide is obtained by Hummers method, in Hummers method, using dense H2SO4、
NaNO2And KMnO4For oxidant, the oxygen-containing groups such as hydroxyl, epoxy group, carboxyl are introduced between graphite laminate structure using oxidation reaction
Group, becomes graphene oxide for graphene, graphene oxide dispersion is obtained after ultrasonic disperse, so that graphene oxide is uniform
Dispersion；Later by combining modified carbonyl iron powder and graphene dispersing solution in concentrated hydrochloric acid solution, obtain inhaling wave frequency bandwidth
Composite wave-suction material.
The present invention provides a kind of methods for preparing composite wave-suction material, comprising the following steps:
Carbonyl iron dust is added in silane coupler solution, adds ammonium hydroxide and deionized water, dispersion, separation, cleaning is admittedly
Body product obtains modified carbonyl iron powder；And mix graphene oxide dispersion with the modified carbonyl iron powder, it separates, obtains
To the composite wave-suction material.
In the above-mentioned methods, the graphene oxide dispersion is prepared by the following method:
Graphene oxide is prepared using Hummers method, then is added graphene oxide into deionized water, disperses, obtains
The graphene oxide dispersion.
In the above-mentioned methods, the solvent of the silane coupler solution includes one kind or more of propyl alcohol, methanol and isopropanol
Kind.
In the above-mentioned methods, silane coupling agent includes KH550 (gamma-aminopropyl-triethoxy-silane), A-1120 (γ-ammonia
Ethylaminopropyl trimethoxy silane) and A-1130's (triamido silane) is one or more, the silane coupling agent is described
Mass fraction in silane coupler solution is 3%~10%.
In the above-mentioned methods, the carbonyl iron dust of 4~9g is added in the silane coupler solution of every 100mL.
In the above-mentioned methods, the volume ratio of the silane coupler solution, the ammonium hydroxide and the deionized water be 80~
120:1.2~2:5~8.
In the above-mentioned methods, by the graphene oxide dispersion in concentrated hydrochloric acid solution of the mass fraction greater than 37.5%
It is mixed with the modified carbonyl iron powder.
In the above-mentioned methods, the graphene oxide dispersion and the volume ratio of the concentrated hydrochloric acid solution are 0.9~1.1:
2.2~2.6.
In the above-mentioned methods, the graphene oxide of 0.9~1.1g is added in the deionized water of every 100mL.
In the above-mentioned methods, the mass ratio of the graphene oxide and the modified carbonyl iron powder be 0.9~1.1:5~
30。
The present invention also provides a kind of composite wave-suction materials prepared according to the above method.
Composite wave-suction material prepared by the method for the present invention realizes the broadband high-selenium corn of absorbing material.Pass through
Silane coupler solution, ammonium hydroxide and deionized water modified carbonyl iron powder, so that modified carbonyl iron dust has the ferromagnetic of raising
Property, and dielectric loss and magnetic loss are had both, it is advantageously implemented impedance matching and the high reflection damage in lower frequency ranges
Consumption；In addition, the graphene oxide in the composite material has high electrical conductance and thermal conductivity, and large specific surface area, be conducive to
The decaying of electromagnetic wave is absorbed；Both Material claddings are advantageously implemented widening for absorption band, with reach absorbing material it is thin,
Gently, wide, strong requirement.
Meanwhile in the case where being conducive to concentrated hydrochloric acid solution environment of the modified carbonyl iron powder in conjunction with graphene oxide, by oxygen
The control of graphite alkene dispersion liquid concentration and control to graphene oxide and the mass ratio of modified carbonyl iron powder, so that oxidation
It while graphene can disperse well, can also be effectively combined with modified carbonyl iron powder, so that preparation is compound
The suction wave frequency band of absorbing material is wider, absorbing property is stronger.
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 uses Hummers method, that is, uses dense H2SO4、NaNO2And KMnO4For oxidant, existed using oxidation reaction
The oxygen-containing groups such as hydroxyl, epoxy group, carboxyl are introduced between graphite laminate structure, graphene are become into graphene oxide, then will oxidation
Graphene is add to deionized water, and 40~60min of ultrasonic disperse obtains graphene oxide dispersion, wherein in every 100mL
0.9~1.1g graphene oxide is added in deionized water, that is, the concentration of graphene oxide dispersion is 0.009~0.011/mL.
4~9g carbonyl iron dust, ultrasound is added in every 100mL silane coupler solution (mass fraction is 3%~10%)
Disperse 20~40min, adds ammonium hydroxide and deionized water, 50~70min of ultrasonic disperse, separated using magnetic method, it is clear with ethyl alcohol
Solid product is washed, 30~50 DEG C of dry 20~28h obtain modified carbonyl iron powder；Wherein, the solvent of silane coupler solution includes
Propyl alcohol, methanol and isopropanol it is one or more；Silane coupling agent includes the one or more of KH550, A-1120 and A-1130；
The volume ratio of silane coupler solution, ammonium hydroxide and deionized water is 80~120:1.2~2:5~8.
Graphene oxide dispersion and modified carbonyl iron powder are added in concentrated hydrochloric acid solution of the mass fraction greater than 37.5%,
1~1.5h is stirred with 600~800rpm under room temperature, is separated using magnetic method, 30~50 DEG C of dry 3~8h obtain composite wave-absorbing
Material；Wherein, the graphene oxide dispersion and the volume ratio of the concentrated hydrochloric acid solution are 0.9~1.1:2.2~2.6, oxygen
The mass ratio of graphite alkene and modified carbonyl iron powder is 0.9~1.1:5~30.
Embodiment 1
50mL mass fraction be 3% KH550 propanol solution in be added 2g carbonyl iron dust, ultrasonic disperse 30min, then
It is added 0.6mL ammonium hydroxide and 3.5mL deionized water, after ultrasonic disperse 60min, is separated using magnetic method, the solid after separation is produced
Object ethyl alcohol cleaning treatment is placed in drying in 40 DEG C of baking oven and for 24 hours, obtains modified carbonyl iron powder；
It is dense that 100mL graphene oxide dispersion (concentration 0.009g/mL) with 5g modified carbonyl iron powder is added to 220mL
In hydrochloric acid solution, 1.2h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is set
Dry 5h, obtains composite wave-suction material in 40 DEG C of baking oven.
Embodiment 2
It is addition 4g carbonyl iron dust in the methanol solution of 10% A-1120, ultrasonic disperse in 100mL mass fraction
20min, adds 1.5mL ammonium hydroxide and 6mL deionized water, after ultrasonic disperse 50min, is separated using magnetic method, after separation
Solid product ethyl alcohol cleaning treatment is placed in 30 DEG C of baking oven dry 28h, obtains modified carbonyl iron powder；
It is dense that 100mL graphene oxide dispersion (concentration 0.01g/mL) with 10g modified carbonyl iron powder is added to 260mL
In hydrochloric acid solution, 1.5h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is set
Dry 3h, obtains composite wave-suction material in 50 DEG C of baking oven.
Embodiment 3
It is addition 4.8g carbonyl iron dust in the aqueous isopropanol of 8% A-1130, ultrasonic disperse in 80mL mass fraction
40min, adds 2mL ammonium hydroxide and 6.5mL deionized water, after ultrasonic disperse 60min, is separated using magnetic method, after separation
Solid product ethyl alcohol cleaning treatment is placed in 50 DEG C of baking oven dry 20h, obtains modified carbonyl iron powder；
It is dense that 100mL graphene oxide dispersion (concentration 0.011/mL) with 20g modified carbonyl iron powder is added to 260mL
In hydrochloric acid solution, 1.3h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is set
Dry 8h, obtains composite wave-suction material in 30 DEG C of baking oven.
Embodiment 4
It is addition 9.6g carbonyl iron dust in the methanol solution of 5% A-1120, ultrasonic disperse in 120mL mass fraction
35min, adds 1mL ammonium hydroxide and 8mL deionized water, after ultrasonic disperse 70min, is separated using magnetic method, by consolidating after separation
Body product ethyl alcohol cleaning treatment is placed in 35 DEG C of baking oven dry 25h, obtains modified carbonyl iron powder；
It is dense that 80mL graphene oxide dispersion (concentration 0.01g/mL) with 25g modified carbonyl iron powder is added to 260mL
In hydrochloric acid solution, 1.5h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is set
Dry 5h, obtains composite wave-suction material in 40 DEG C of baking oven.
Embodiment 5
It is addition 9g carbonyl iron dust in the aqueous isopropanol of 8% KH550, ultrasonic disperse in 100mL mass fraction
30min, adds 1mL ammonium hydroxide and 7mL deionized water, after ultrasonic disperse 60min, is separated using magnetic method, by consolidating after separation
Body product ethyl alcohol cleaning treatment is placed in 40 DEG C of baking oven dry 20h, obtains modified carbonyl iron powder；
It is dense that 100mL graphene oxide dispersion (concentration 0.011/mL) with 30g modified carbonyl iron powder is added to 260mL
In hydrochloric acid solution, 2h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is placed in
Dry 6h, obtains composite wave-suction material in 40 DEG C of baking oven.
Embodiment 6
100mL mass fraction be 7% A-1120 methanol solution in be added 4g carbonyl iron dust, ultrasonic disperse 40min,
It adds 1.5mL ammonium hydroxide and 6mL deionized water, after ultrasonic disperse 60min, is separated using magnetic method, the solid after separation is produced
Object ethyl alcohol cleaning treatment is placed in drying in 40 DEG C of baking oven and for 24 hours, obtains modified carbonyl iron powder；
It is dense that 120mL graphene oxide dispersion (concentration 0.01g/mL) with 10g modified carbonyl iron powder is added to 260mL
In hydrochloric acid solution, 1.5h is stirred under room temperature, is separated using magnetic method, the ethyl alcohol cleaning treatment of the solid product after separation is set
Dry 5h, obtains composite wave-suction material in 40 DEG C of baking oven.
Using paraffin as binder, the composite wave-suction material of finally obtained different proportion is mixed by a certain percentage with paraffin
It closes uniformly, is put into homemade coaxial sample toroidal mold, is pressed into the coaxial sample annulus of certain size, annulus outer diameter
7.0mm internal diameter 3.04mm, thickness 2mm.Using vector network analyzer, the electromagnetic parameter of 2~18GHz frequency range sample is tested, and
The absorbing property of sunykatuib analysis material.The test result of absorbing property see the table below 1:
Table 1
Seen from table 1, the present invention passes through the combination of graphene oxide and modified carbonyl iron powder, so that the composite wave-absorbing of preparation
Material has good absorbing property, has stronger absorption in the wide frequency ranges of 2~18GHz, most down to -30.2dB,
And frequency bandwidth is 2.17, is modified to carbonyl iron dust, the iron of composite material can be improved in the modified carbonyl iron powder of preparation
Magnetism, reflection loss in lower frequency range is high, and graphene oxide in higher frequency range with high anti-
Loss is penetrated, modified carbonyl iron powder is used in combination with graphene oxide, and modified carbonyl iron powder and oxidation stone are made by dispersion
Black alkene comes into full contact with so that preparation composite wave-suction material realize broadband high-selenium corn, meet absorbing material it is thin, light, wide,
Strong requirement.It can be applied to the numerous areas such as aerospace, ship naval vessels, radar antenna and 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 (11)
1. a kind of method for preparing composite wave-suction material, which comprises the following steps:
Carbonyl iron dust is added in silane coupler solution, adds ammonium hydroxide and deionized water, dispersion, separation, cleaning solid produces
Object obtains modified carbonyl iron powder；And
Graphene oxide dispersion is mixed with the modified carbonyl iron powder, separates, obtains the composite wave-suction material.
2. the method according to claim 1, wherein the graphene oxide dispersion is made by the following method
It is standby:
Graphene oxide is prepared using Hummers method, then is added graphene oxide into deionized water, is dispersed, is obtained described
Graphene oxide dispersion.
3. the method according to claim 1, wherein the solvent of the silane coupler solution includes propyl alcohol, first
Pure and mild isopropanol it is one or more.
4. according to the method described in claim 3, it is characterized in that, silane coupling agent includes KH550, A-1120 and A-1130's
One or more, mass fraction of the silane coupling agent in the silane coupler solution is 3%~10%.
5. the method according to claim 1, wherein being added 4 in the silane coupler solution of every 100mL
The carbonyl iron dust of~9g.
6. the method according to claim 1, wherein the silane coupler solution, the ammonium hydroxide and described going
The volume ratio of ionized water is 80~120:1.2~2:5~8.
7. the method according to claim 1, wherein will in concentrated hydrochloric acid solution of the mass fraction greater than 37.5%
The graphene oxide dispersion is mixed with the modified carbonyl iron powder.
8. the method according to the description of claim 7 is characterized in that the graphene oxide dispersion and the concentrated hydrochloric acid solution
Volume ratio be 0.9~1.1:2.2~2.6.
9. according to the method described in claim 2, it is characterized in that, being added 0.9~1.1g's in the deionized water of every 100mL
Graphene oxide.
10. according to the method described in claim 9, it is characterized in that, the graphene oxide and the modified carbonyl iron powder
Mass ratio is 0.9~1.1:5~30.
11. a kind of composite wave-suction material of method preparation according to claim 1 to 10.
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| CN115121793A (en) * | 2022-06-15 | 2022-09-30 | 中国航空制造技术研究院 | High-temperature-resistant modification method for zirconium dioxide coated micron-sized carbonyl iron absorbent |
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