CN114933800A - Nano ferrite/liquid silicon rubber radar wave-absorbing composite material - Google Patents
Nano ferrite/liquid silicon rubber radar wave-absorbing composite material Download PDFInfo
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- CN114933800A CN114933800A CN202210519922.8A CN202210519922A CN114933800A CN 114933800 A CN114933800 A CN 114933800A CN 202210519922 A CN202210519922 A CN 202210519922A CN 114933800 A CN114933800 A CN 114933800A
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 29
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 title claims description 7
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 10
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 7
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002114 nanocomposite Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 239000000945 filler Substances 0.000 abstract description 5
- 238000002310 reflectometry Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000012512 characterization method Methods 0.000 abstract description 2
- 239000011810 insulating material Substances 0.000 abstract description 2
- 238000004626 scanning electron microscopy Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 9
- 239000011358 absorbing material Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000006854 communication Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002356 single layer Substances 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UJGOCJFDDHOGRX-UHFFFAOYSA-M [Fe]O Chemical compound [Fe]O UJGOCJFDDHOGRX-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000005260 human cell Anatomy 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 239000012762 magnetic filler Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
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- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention belongs to the technical field of electrical insulating materials, and discloses a nano ferrite/Liquid Silicone Rubber radar wave-absorbing composite material prepared by taking high-flexibility addition type Liquid Silicone Rubber (LSR) as a dielectric medium matrix, wherein nano strontium ferrite powder (SrFe) is respectively used as 12 O 19 ) And nano Carbonyl Iron Powder (CIP) as a ferrite filler to prepare the radar wave-absorbing composite material with excellent wave-absorbing performance. Characterization of SrFe by scanning Electron microscopy 12 O 19 The nano-filler dispersibility in the/LSR and CIP/LSR composite materials and the mechanical property and direct current performance are testedTesting the conductivity and the direct current breakdown field strength; SrFe compared to pure LSR 12 O 19 The mechanical properties and DC breakdown field strength of the/LSR and CIP/LSR composite materials are reduced, the DC conductivity is increased, nonlinearity appears under high field strength, and SrFe is evaluated through the measured dielectric loss, magnetic loss and reflectivity 12 O 19 the/LSR and CIP/LSR composite material has wave-absorbing performance.
Description
Technical Field
The invention belongs to the technical field of electrical insulating materials, and relates to a nano ferrite/liquid silicone rubber radar wave-absorbing composite material and a preparation method thereof.
Background
In recent years, a communication technology, a remote sensing technology, a positioning navigation technology and the like based on electromagnetic waves provide a convenient service platform for production and life, so that communication among people is more convenient, and the world can be clearly shown in front of people; however, at the same time, the disadvantages caused by the advanced technology are more and more obvious, and some precise electronic devices need to protect a large amount of electromagnetic wave interference in order to stably and normally operate in a complex electromagnetic environment.
The communication equipment also needs reasonable and accurate line selection, inhibits other electromagnetic wave interference signals, ensures that the problems of channel crosstalk and the like do not occur in the communication process, and achieves an effective communication process; on the other hand, electromagnetic waves also have an effect on the body mechanism of a person; high intensity electromagnetic radiation, if ingested by human cells, can cause physiological changes that can damage the nervous system, reproductive system, and immune system to some extent.
The metal micro powder is a wave-absorbing material with wide application, and compared with other materials, the metal micro powder has a simpler internal structure, higher magnetic conductivity and magnetic loss, and can bear relatively higher Curie temperature.
Disclosure of Invention
Aiming at the defects of the prior art, the first purpose of the invention is to better solve the electromagnetic wave pollution and realize the radar stealth technology, prepare the nano ferrite dielectric composite material with more excellent wave-absorbing performance, and prepare the nano composite material by respectively adopting nano strontium ferrite powder and nano carbonyl iron powder to addition liquid silicone rubber.
The second purpose of the invention is to establish a double-layer wave-absorbing material structure model, compare the double-layer wave-absorbing material structure model with a single-layer wave-absorbing material structure, and explore the influence of the material types and the thicknesses of a matching layer and a loss layer on the wave-absorbing performance of the double-layer wave-absorbing structure, so as to provide the double-layer wave-absorbing material and the double-layer wave-absorbing structure with the best wave-absorbing performance.
The technical scheme of the invention is as follows:
a nano ferrite/liquid silicon rubber radar wave-absorbing composite material comprises the following steps:
adding liquid silicon rubber is selected as a base material and is respectively doped with nano SrFe 12 O 19 Powder ofAnd nano CIP powder magnetic filler to prepare SrFe with different mass fractions 12 O 19 the/LSR and CIP/LSR nanocomposites.
Evaluation of SrFe 12 O 19 The wave absorbing performance of the/LSR and CIP/LSR composite materials adopts a coaxial method and a bow method respectively to SrFe with different components 12 O 19 The electromagnetic parameters and radar reflectivity of the/LSR and CIP/LSR composites were tested.
According to experimental data of wave absorption performance of two composite materials, simulating radar wave scattering of a single-layer wave absorption structure by using CST simulation software, and discussing the thickness and incident angle of a layer for SrFe 12 O 19 Selecting the single-layer wave-absorbing material with the most excellent wave-absorbing performance under the influence of radar reflectivity of the/LSR and CIP/LSR composite materials.
The invention also comprises a characterization method of the nano ferrite/liquid silicone rubber radar wave-absorbing composite material, which comprises the following steps:
firstly, in order to observe the microscopic appearance of the sample more clearly and accurately, a sample material with the thickness of 0.75mm needs to be cut into sheets, put into liquid nitrogen and quickly taken out for quenching; then, carrying out gold spraying operation on the quenched section, namely plating a layer of metal particles, and then scanning and observing the sample by using an SU8020 device, so that the section appearance of the sample can be observed;
secondly, in order to investigate the mechanical tensile property of the blended material, a WDW-10C type universal testing machine is used as experimental equipment in the experiment, and the multi-component composite material is tested by selecting the engineering standard GB/T1040.2-2006.
Thirdly, in order to explore the influence of the nano powder doping on the electrical insulation performance of the composite material, the experiment carries out laboratory tests on the direct current conductivity and the direct current breakdown field strength of the nano liquid silicone rubber composite material, and a direct current breakdown field strength test system is shown in fig. 1, so as to explore the application value of the nano liquid silicone rubber composite material in an actual working scene.
Fourthly, when the electromagnetic parameters of the composite materials with different components are tested, the outer diameter of the sample is 7mm, the inner diameter of the sample is 3.04mm, the thickness of the sample is 2-3 mm, and the sample is shown in figure 2.
Preferably, the thickness of the sample to be measured selected in the experiment in the second step is about 0.75mm, and the sample is punched into a dumbbell shape by a dumbbell cutter.
Preferably, in the second step, the initial distance between the clamps is 50mm, the gauge length is 20mm, the width of the narrow parallel part is 6mm, the tensile rate of the testing machine is set to be 50mm/min, and the testing environment temperature is 25 ℃.
Preferably, the thickness of the sample with the direct current conductivity in the third step is about 0.2mm, and the sample is pre-placed for 24h for electrostatic treatment before the experiment is started for data accuracy.
Preferably, before the measurement in the third step is started, the actual thickness of the composite material with different components is measured by a thickness gauge and recorded; in the test, the voltage is controlled from 200V to 4000V, the reading is carried out after the voltage is kept stable for 15 minutes after each boosting, and the post-processing of the data is carried out.
Compared with the prior art, the invention has the following beneficial effects:
first, in comparison with pure LSR, SrFe 12 O 19 The tensile strength and the direct-current breakdown strength of the/LSR and CIP/LSR composite materials are slightly reduced; SrFe 12 O 19 The direct current conductivity of the/LSR and CIP/LSR nanocomposites is proportional to the concentration of the ferrite filler and significant conductance nonlinearity occurs at high electric field strengths.
Second, the SrFe obtained by the invention 12 O 19 The dielectric loss, magnetic loss and reflectivity test results of the/LSR and CIP/LSR nano composite material in a radar waveband (2-18 GHz) show that: the radar wave absorption is mainly magnetic loss; SrFe 12 O 19 The absorption peak of the/LSR composite material is positioned in a high frequency band of 10-18 GHz, when the doping concentration is 7 wt%, the minimum reflection loss is-33 dB around-11 GHz, and the effective absorption bandwidth is 10.1 GHz; the absorption peak of the CIP/LSR nano composite material is in a low frequency band of 2-8 GHz, the highest wave-absorbing performance is obtained at 3 wt% nano filling rate, the minimum reflection loss is-21 dB at-7 GHz, and the effective absorption bandwidth is 3.9 GHz; with the increase of the concentration of the ferrite nano filler, the absorption peaks of the two composite materials move to low frequencies.
Third, thisThe CST electromagnetic wave scattering simulation result of the single-layer wave-absorbing structure shows that: the SrFe can be caused by increasing the single-layer wave-absorbing thickness 12 O 19 The radar wave absorption peak of the/LSR and CIP/LSR nano composite material moves to low frequency, and the effective absorption bandwidth is narrowed; when SrFe 12 O 19 The absorption performance is best when the coating thicknesses of the/LSR and CIP/LSR composite materials are respectively 2mm and 3 mm; when the incident angle of radar waves is increased within the range of 0-75 degrees, the wave absorbing performance of the two composite materials is reduced, but the frequency of an absorption peak is basically unchanged, so that the wave absorbing performance of the radar waves with vertical incidence is highest.
Drawings
FIG. 1 is a schematic diagram of a DC breakdown field strength testing system according to the present invention.
FIG. 2 is a sample size picture of the coaxial electromagnetic parameters of the present invention.
FIG. 3 is a scanning electron microscope of doped nanocomposites with different mass fractions.
In fig. 3: 1 is 3 wt% -CIP/LSR and 2 is 3 wt% -SrFe 12 O 19 LSR, 3 is 5 wt% -CIP/LSR, 4 is 5 wt% -SrFe 12 O 19 LSR, 5 is 7 wt% -CIP/LSR, 6 is 7 wt% -SrFe 12 O 19 /LSR。
Detailed Description
The nano ferrite/silicon rubber composite material takes liquid silicon rubber as a matrix material, and is doped with nano strontium ferrite and carbonyl iron; the obtained nano ferrite/silicon rubber composite material has high resistivity, and the dielectric property and the magnetic property are also very excellent, so that the loss attenuation in the wave-absorbing material has a very positive promotion effect.
The preparation method of the nano ferrite/liquid silicone rubber radar wave-absorbing composite material mainly comprises the following two steps:
firstly, liquid silicon rubber is placed in a wiped iron beaker, the iron beaker is placed in a multifunctional dispersion stirrer for full mixing and stirring, and nano strontium ferrite powder or carbonyl iron powder is added for stirring until the mixture is uniformly stirred.
Secondly, the mixed material is put into a vacuum drying oven for vacuum treatment, after bubbles are removed, the mixed material is put into a flat vulcanizing machine with the temperature of 120 ℃ and the pressure of 15MPa for vulcanization for 30 minutes, and then the mixed material is put into a drying oven with the temperature of 200 ℃ for secondary crosslinking.
The preparation method of the liquid silicone rubber nanocomposite and the related performance test method select the two-component addition type liquid silicone rubber as a matrix, and the nano strontium ferrite and the hydroxyl iron powder as the magnetic nano-fillers to respectively prepare SrFe with the mass fractions of 3 wt%, 5 wt% and 7 wt% 12 O 19 the/LSR and CIP/LSR nano composite material samples are characterized by the dispersibility of nano particles by a scanning electron microscope, and mechanical tensile property, direct current conductivity, direct current breakdown field strength, electromagnetic parameters and radar reflectivity are tested.
The scanning electron microscopy results for nanocomposites doped with different mass fractions are shown in figure 3. According to the results of a scanning electron microscope, the nano strontium ferrite powder and the nano carbonyl iron powder are both granular, and the two kinds of nano powders have better dispersibility in liquid silicone rubber, but with the increase of the doping concentration of the nano powders, the agglomeration of the composite material can be seen, particularly the small agglomeration of the nano particles can be seen in the 7 wt% -CIP/LSR composite material, and compared with the 7 wt% -SrFe composite material, the small agglomeration of the nano particles can be seen more obviously 12 O 19 The agglomeration of/LSR is not so pronounced.
Claims (2)
1. The nano ferrite/liquid silicon rubber radar wave-absorbing composite material is characterized by comprising the following preparation raw materials: the model is
737 addition type liquid silicone rubber, 40nm nanometer carbonyl iron powder, and 100nm nanometer strontium ferrite powder.
2. A nanocomposite as claimed in claim 1, which is placed in a mold, vulcanized at 15MPa for 30 minutes with a press vulcanizer temperature set at 120 ℃ to subject the mixture to primary crosslinking, and then the sample is taken out and placed in an electrothermal forced air drying oven at 200 ℃ for 4 hours.
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| CN202210519922.8A CN114933800A (en) | 2022-05-13 | 2022-05-13 | Nano ferrite/liquid silicon rubber radar wave-absorbing composite material |
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| CN202210519922.8A CN114933800A (en) | 2022-05-13 | 2022-05-13 | Nano ferrite/liquid silicon rubber radar wave-absorbing composite material |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030044623A1 (en) * | 2001-05-07 | 2003-03-06 | Ikuo Sakurai | Electromagnetic wave absorber |
| CN101650977A (en) * | 2009-09-09 | 2010-02-17 | 湖南大学 | Nano iron oxide /graphite composite electromagnetic absorption material and preparation method thereof |
| CN102807840A (en) * | 2012-08-17 | 2012-12-05 | 中北大学 | Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material |
| WO2013084920A1 (en) * | 2011-12-05 | 2013-06-13 | デクセリアルズ株式会社 | Electromagnetic wave-absorbing thermal-conductive sheet and method for manufacturing electromagnetic wave-absorbing thermal-conductive sheet |
| CN105348660A (en) * | 2015-11-02 | 2016-02-24 | 浙江欧仁新材料有限公司 | Composite wave absorbing material and preparation method thereof |
| CN108384243A (en) * | 2018-03-02 | 2018-08-10 | 龙岩紫荆创新研究院 | A kind of magnetic composite and preparation method thereof |
| CN108394938A (en) * | 2018-04-17 | 2018-08-14 | 哈尔滨工业大学 | A kind of pros' bodily form strontium ferrite wave absorbing agent and preparation method thereof |
| CN109207123A (en) * | 2018-09-10 | 2019-01-15 | 中南大学 | A kind of double shell structurre carbonyl iron composite absorbers and preparation method |
-
2022
- 2022-05-13 CN CN202210519922.8A patent/CN114933800A/en active Pending
Patent Citations (8)
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| WO2013084920A1 (en) * | 2011-12-05 | 2013-06-13 | デクセリアルズ株式会社 | Electromagnetic wave-absorbing thermal-conductive sheet and method for manufacturing electromagnetic wave-absorbing thermal-conductive sheet |
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| CN109207123A (en) * | 2018-09-10 | 2019-01-15 | 中南大学 | A kind of double shell structurre carbonyl iron composite absorbers and preparation method |
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Application publication date: 20220823 |