CN114481364A - Janus type electromagnetic coupling microwave absorbent and preparation method thereof - Google Patents
Janus type electromagnetic coupling microwave absorbent and preparation method thereof Download PDFInfo
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- 239000002250 absorbent Substances 0.000 title claims abstract description 19
- 230000002745 absorbent Effects 0.000 title claims abstract description 19
- 230000008878 coupling Effects 0.000 title claims abstract description 19
- 238000010168 coupling process Methods 0.000 title claims abstract description 19
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000835 fiber Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 238000009987 spinning Methods 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001523 electrospinning Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 11
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 4
- 238000002310 reflectometry Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000011358 absorbing material Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 230000001808 coupling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Textile Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a Janus type electromagnetic coupling microwave absorbent and a preparation method thereof, wherein the preparation method comprises the following specific steps: dissolving an electric loss type raw material in an alcohol solution, dissolving a magnetic loss type raw material in an alcohol-water solution, and magnetically stirring to obtain a uniform solution; dissolving a certain amount of binder in an organic solvent, and stirring until a uniform and transparent solution is formed; and mixing the solutions to prepare spinning solutions. And (2) adopting a double-sided electrostatic spinning technology, connecting the injector with a double-sided needle by using a hose, preparing a Janus type electromagnetic coupling microwave absorbent precursor fiber by electrospinning, and calcining at high temperature for 2-5 hours to obtain the electromagnetic composite fiber. The prepared composite fiber has the advantages of large specific surface area, high coupling degree, wide raw material source and low cost, and the preparation technology is simple, easy to control and easy to realize industrial production.
Description
Technical Field
The invention belongs to the field of inorganic nano material preparation, and particularly relates to a Janus type electromagnetic coupling microwave absorbent and a preparation method thereof.
Background
The rapid development of wireless communication and electronic technologies has prompted the widespread use of electronic devices in military and civilian applications, and the hazards of electromagnetic radiation and electromagnetic interference have received increasing social attention. In order to solve this problem, the realization of attenuation and absorption of electromagnetic waves by microwave absorbing materials is the most ideal method and has received much attention. Microwave absorption is the absorption and attenuation of incident energy by energy conversion and multiple scattering. In order to improve the electromagnetic wave absorption performance of the absorbent, two key factors must be considered. One is the damping performance and the other is the impedance matching of the absorbing material to air. Traditional absorbents such as ferrite and the like have the advantages of wide absorption frequency band and strong absorption and are widely applied to wave-absorbing materials, but the defects of poor matching property with air and large specific gravity limit the application range of the traditional absorbents. In recent years, composite materials consisting of magnetic and dielectric absorbers have proven to be an effective strategy to achieve good impedance matching and electromagnetic losses by means of a synergistic coupling effect between the electrical losses of the dielectric material and the magnetic losses of the magnetic material. The electromagnetic coupling fiber composite material researched at present achieves a good effect, but the research at present still mainly focuses on random compounding, so that the contact area between the electric loss material and the magnetic loss material is small, and the coupling effect is poor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a Janus type electromagnetic coupling microwave absorbent and a preparation method thereof.
A Janus type electromagnetic coupling microwave absorbent and a preparation method thereof comprise the following steps:
dissolving an electric loss type raw material in an alcohol solution, dissolving a magnetic loss type raw material in an alcohol-water solution, and magnetically stirring to obtain uniform solutions A and B; dissolving a certain amount of binder in an organic solvent, and stirring until a uniform and transparent solution C is formed; and dividing the solution C into 2 parts, mixing the solution C with the solution A and the solution B respectively, and stirring for 3-5 hours to prepare spinning solutions D and E. And respectively filling the solution D and the solution E into a syringe, and connecting a hose with a double-sided syringe needle. Adjusting electrostatic spinning parameters, wherein the voltage is 10-20kV, the receiving distance is 10-20cm, the needle diameter is 0.4-0.9mm, the liquid outlet speed is 1mL/h, obtaining precursor fiber by electrostatic spinning, and calcining for 2-5 hours at high temperature to obtain the electromagnetic composite fiber.
The electrical loss type raw material is one or two of nitrate or acetate of strontium and barium, and tetrabutyl titanate.
The magnetic loss type raw material is one or more of nitrates or acetates of cobalt, iron, zinc and nickel.
The binder is one or two of polyvinylpyrrolidone or polyvinyl alcohol.
The solvent is one or two of dimethylformamide or ethanol.
The certain amount of the binder is 8-12% of the total mass of the solution.
The double-sided syringe needle refers to the fact that the solutions D and E are only contacted at the needle point and are sprayed out together.
The high temperature is 750-1050 ℃.
The invention has the beneficial effects that:
(1) the composite fiber has a Janus type structure, so that the contact area of the electric loss type material and the magnetic loss type material is effectively increased, the coupling performance of the electric loss type material and the magnetic loss type material is enhanced, and the microwave absorption performance of the fiber is improved.
(2) The Janus type electromagnetic loss composite fiber material prepared by the invention has the advantages of wide raw material source, simple process, controllable technology and low cost, and is expected to realize large-scale production.
Drawings
FIG. 1 is a schematic view of a Janus type electromagnetic coupling microwave absorbent prepared according to the present invention;
FIG. 2 is an XRD diagram of the cobalt ferrite/barium titanate fiber composite material prepared by the invention.
FIG. 3 is a RL graph of the cobalt ferrite/barium titanate fiber composite material prepared by the invention.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
Adding 2.61g of barium nitrate and 3.40g of tetrabutyl titanate serving as power-loss raw materials into 20mL of ethanol, adding 2.91g of cobalt nitrate and 8.08g of ferric nitrate serving as magnetic-loss raw materials into 50mL of alcohol-water solution, and uniformly stirring to obtain uniform solutions A and B; weighing 2g of polyvinylpyrrolidone, adding polyvinylpyrrolidone into 20mL of dimethylformamide, and stirring for 3 hours to obtain a uniform solution C; and dividing the solution C into 2 parts, mixing the solution C with the solution A and the solution B respectively, and stirring for 5 hours to obtain spinning solutions D and E. 10mL of D and E are filled into an injector, a hose is connected with a double-sided needle, spinning is carried out under the conditions of 15kV voltage, 15cm receiving distance and 1mL/h liquid flow rate to obtain Janus precursor fiber, and the Janus precursor fiber is calcined at 1050 ℃ for 2h to obtain Janus type composite fiber, wherein the XRD pattern of the Janus type composite fiber is shown in figure 2. The lowest reflectivity of the obtained sample in the range of 2-18GH reaches-89 dB, and the effective absorption bandwidth reaches 9.4GHz, as shown in figure 3.
Example 2
Adding 2.61g of barium nitrate and 3.40g of tetrabutyl titanate serving as power-loss raw materials into 20mL of ethanol, adding 2.91g of cobalt nitrate and 8.08g of ferric nitrate serving as magnetic-loss raw materials into 50mL of alcohol-water solution, and uniformly stirring to obtain uniform solutions A and B; weighing 2.5g of polyvinylpyrrolidone, adding polyvinylpyrrolidone into 20mL of dimethylformamide, and stirring for 3 hours to obtain a uniform solution C; and dividing the solution C into 2 parts, mixing the solution C with the solution A and the solution B respectively, and stirring for 5 hours to obtain spinning solutions D and E. And (3) filling 10mL of D and E into an injector, connecting a hose with a double-sided needle, spinning under the conditions of 15kV voltage, 15cm receiving distance and 1mL/h liquid flow rate to obtain the Janus precursor fiber, and calcining at 850 ℃ for 2h to obtain the Janus type composite fiber. The lowest reflectivity of the obtained sample in the range of 2-18GH reaches-64 dB, and the effective absorption bandwidth reaches 5.2 GHz.
Example 3
Adding 2.61g of barium nitrate and 3.40g of tetrabutyl titanate serving as power-loss raw materials into 20mL of ethanol, adding 2.91g of cobalt nitrate and 8.08g of ferric nitrate serving as magnetic-loss raw materials into 50mL of alcohol-water solution, and uniformly stirring to obtain uniform solutions A and B; weighing 2.5g of polyvinylpyrrolidone, adding polyvinylpyrrolidone into 20mL of dimethylformamide, and stirring for 3 hours to obtain a uniform solution C; and dividing the solution C into 2 parts, mixing the solution C with the solution A and the solution B respectively, and stirring for 5 hours to obtain spinning solutions D and E. And (3) filling 10mL of D and E into an injector, connecting a hose with a double-sided needle, spinning under the conditions of 15kV voltage, 15cm receiving distance and 1mL/h liquid flow rate to obtain the Janus precursor fiber, and calcining at 750 ℃ for 2h to obtain the Janus type composite fiber. The lowest reflectivity of the obtained sample in the range of 2-18GH reaches-42 dB, and the effective absorption bandwidth reaches 3.0 GHz.
Example 4
Taking electricity loss type raw materials, namely 2.61g of barium nitrate and 3.40g of tetrabutyl titanate, adding the electricity loss type raw materials into 20mL of ethanol, taking magnetic loss type raw materials, namely 2.91g of cobalt nitrate and 8.08g of ferric nitrate, adding the magnetic loss type raw materials into 50mL of alcohol-water solution, and uniformly stirring to obtain uniform solutions A and B; weighing 1.8g of polyvinylpyrrolidone, adding polyvinylpyrrolidone into 20mL of dimethylformamide, and stirring for 3 hours to obtain a uniform solution C; and dividing the solution C into 2 parts, mixing the solution C with the solution A and the solution B respectively, and stirring for 5 hours to obtain spinning solutions D and E. And (3) filling 10mL of D and E into an injector, connecting a hose with a double-sided needle, spinning under the conditions of 15kV voltage, 15cm receiving distance and 1mL/h liquid flow rate to obtain the Janus precursor fiber, and calcining at 950 ℃ for 2h to obtain the Janus type composite fiber. The lowest reflectivity of the obtained sample in the range of 2-18GH reaches-35 dB, and the effective absorption bandwidth reaches 2.2 GHz.
Claims (8)
1. A Janus type electromagnetic coupling microwave absorbent and a preparation method thereof are characterized in that:
dissolving an electric loss type raw material in an alcohol solution, dissolving a magnetic loss type raw material in an alcohol-water solution, and magnetically stirring to obtain uniform solutions A and B; dissolving a certain amount of binder in an organic solvent, and stirring until a uniform and transparent solution C is formed; dividing the solution C into 2 parts, respectively mixing with the solution A and the solution B, and stirring for 3-5 hours to prepare spinning solutions D and E;
and respectively filling the solution D and the solution E into an injector, connecting a hose with a double-sided injector needle, adjusting electrostatic spinning parameters, controlling the voltage to be 10-20kV, the receiving distance to be 10-20cm and the diameter of the needle to be 0.4-0.9mm, carrying out electrostatic spinning to obtain precursor fibers, and calcining at high temperature for 2-5 hours to obtain the electromagnetic composite fibers.
2. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1, characterized in that: the electrical loss type raw material is one or two of nitrate or acetate of strontium and barium, and tetrabutyl titanate.
3. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the magnetic loss type raw material is one or more of nitrates or acetates of cobalt, iron, zinc and nickel.
4. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the binder is one or two of polyvinylpyrrolidone or polyvinyl alcohol.
5. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the solvent is one or two of dimethylformamide or ethanol.
6. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the certain amount of the binder is 8-12% of the total mass of the solution.
7. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the double-sided syringe needle refers to the fact that the solutions D and E are only contacted at the needle point and are sprayed out together.
8. The Janus type electromagnetic coupling microwave absorbent and the preparation method thereof according to claim 1 are characterized in that: the high temperature is 750-1050 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116641160A (en) * | 2023-06-27 | 2023-08-25 | 东华大学 | Light elastic iron-cobalt-nickel/carbon-based wave-absorbing material, and preparation method and application thereof |
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