CN110591164B - Solid nano dispersion wave-absorbing material - Google Patents
Solid nano dispersion wave-absorbing material Download PDFInfo
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- CN110591164B CN110591164B CN201910949343.5A CN201910949343A CN110591164B CN 110591164 B CN110591164 B CN 110591164B CN 201910949343 A CN201910949343 A CN 201910949343A CN 110591164 B CN110591164 B CN 110591164B
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- 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
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
Abstract
The invention discloses a solid nano-dispersion wave-absorbing material, which is single magnetic domain Fe obtained by microbial fermentation3O4The nano crystal-magnetosome is used as absorbent, and is compounded with carbon material, and then the biological nano wave-absorbing material is prepared by spray drying technology. The wave-absorbing material has the advantages of simple preparation method, small magnetic body filling amount, large powder production amount, lower production cost, easy large-scale industrial production, uniform and uniform particles of the obtained wave-absorbing material, strong stability, excellent wave-absorbing performance, wide wave-absorbing frequency, better effect compared with the current wave-absorbing material and high practical application value.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a solid nano-dispersion wave-absorbing material.
Background
With the development requirement of the electromagnetic stealth technology in the military field and the increasing severity of the problems of electromagnetic pollution and electromagnetic interference, the wave-absorbing material gradually becomes a research hotspot in the field of functional materials. A wave-absorbing material is a material that absorbs or substantially attenuates the energy of electromagnetic waves incident on its surface, thereby reducing the interference of electromagnetic waves and converting the electromagnetic energy into other forms of energy for consumption. In modern war, the demand for improving stealth performance and anti-electromagnetic interference capability of weapons is more and more strong in the face of radar detection technology of radar and strong electromagnetic interference technology of electronic warfare. The main approach for solving the problems is to design a material which can better absorb and shield electromagnetic waves, install the material on the surface of the weapon, and utilize a wave-absorbing material to absorb the electromagnetic waves or reduce the reflection of the electromagnetic waves, thereby realizing the invisible and anti-electromagnetic interference of the weapon. The traditional wave-absorbing materials, such as ferrite, metal micropowder, silicon carbide and the like, generally have the defects of narrow absorption band, high density, large filling ratio and the like, so that the application of the materials in practice is limited. The ideal wave-absorbing material generally needs to meet the requirements of thin thickness, light weight, wide absorption frequency, strong absorption performance (thin, light, wide and strong), and the like. Therefore, the development of the novel wave-absorbing material with novel structure and excellent comprehensive performance has important scientific value and application prospect.
Patent CN103347377A reports that RGO/Co is synthesized in two steps by a hydrothermal method3O4When the thickness of a sample is 3.3mm, the nano composite material has the best wave-absorbing performance at 13.8GHz, and the reflection loss reaches-43.7 dB. The method combines RGO and Co3O4Recombination to obtain RGO/Co3O4Nanocomposite, compared to single RGO and Co3O4The wave-absorbing performance is improved, but the method has complex raw material preparation process, so that the method is not suitable for large-scale production and limits practical application. According to "nanotechnology" 2015 (2): 46-50 reports that tubular Fe @ C composite materials with the outer diameter of 50-60 nm and the inner diameter of 30-40 nm are obtained by using ferrocene as a raw material through pyrolysis under the action of an external magnetic field by utilizing a Chemical Vapor Deposition (CVD) technology, and the maximum reflection loss is-18 dB when the thickness of the Fe @ C is 5mm and the frequency is 2.5 GHz. The Fe @ C complex prepared by the methodThe composite material has small size, good appearance and low preparation cost, but the wave-absorbing frequency band is narrow.
Disclosure of Invention
The invention aims to overcome the problems of narrow absorption band, high density, large filling ratio and the like of the existing wave-absorbing material, and provides a method for preparing a solid nano-dispersion wave-absorbing material which is prepared by a spray drying method and has the excellent characteristics of wide absorption band, low density, small filling ratio and the like.
Aiming at the purposes, the technical scheme adopted by the invention is as follows: the wave-absorbing material is prepared by uniformly mixing a magnetosome, a binder, a carbon material and a solvent according to the mass ratio of 1: 3-8: 0.5-3: 20-100, and then carrying out spray drying.
The carbon material is carbon fiber or graphene.
The binder is one or more of acacia, maltodextrin, polystyrene, polyurethane, polyaniline and polyacrylic acid.
The solvent is any one of water, acetone and ethyl acetate.
The mass ratio of the magnetosome to the binder, the carbon material and the solvent is preferably 1: 4-5: 1-2: 30-50.
The above-mentioned mode of uniformly mixing is firstly high-speed shearing, then high-pressure homogenizing.
The high-speed shearing power is 1000-1500W, and the pressure is 0.6-1.2 MPa.
The pressure for high-pressure homogenization is 500-1200 bar.
The air inlet temperature of the spray drying is 160-200 ℃, and the feeding rate is 50-200 kg/h.
The magnetosome is fermented and cultured according to the method disclosed in the publication No. CN101434921A entitled "a method for producing magnetosome by culturing magnetosome", fermentation liquor is centrifuged by a high-speed centrifuge, supernatant is removed, somatic cells are collected, water is added to reach a suspension state by a high-speed shearing machine, the obtained suspension is subjected to cell disruption by a high-pressure homogenizer, magnetosome is collected by a magnetic attraction method, impurities such as protein and the like are washed by PBS buffer solution, salt solution is removed by washing, and the magnetosome with high purity is obtained by freeze drying.
The invention has the following beneficial effects:
1. the invention utilizes single magnetic domain Fe obtained by microbial fermentation3O4The nano crystal-magnetosome is used as absorbent, and is compounded with carbon material, and then the biological nano wave-absorbing material is prepared by spray drying technology. The prepared wave-absorbing material has uniform and uniform particles, strong stability and high practical application value.
2. The wave-absorbing material has excellent wave-absorbing performance, wide wave-absorbing frequency, better effect than the current wave-absorbing material and wider application range.
3. The wave-absorbing material has the advantages of simple preparation method, small magnetic body filling amount, large powder generation amount, lower production cost and easy large-scale industrial production.
Drawings
Figure 1 is a reflection loss chart of the wave-absorbing material/paraffin wax prepared in example 1 at different thicknesses.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
20g of gum arabic was added to 200g of water, and stirred to dissolve it, and then 5g of magnetosome and 5g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) Is-55.2 dB at the thickness of 3mm, and is electromagnetic wave at 2-18 GHz at the thickness of 3mmThe bandwidth with reflection loss less than-10 dB in the band is 8.5GHz (see fig. 1).
Example 2
20g of gum arabic was added to 250g of water, and stirred to dissolve it, and then 4g of magnetosome and 4g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 6.8GHz, the reflection loss of the bandwidth is less than-10 dB in the electromagnetic wave frequency band of 2-18 GHz when the bandwidth is 3mm and-35.2 dB when the thickness is 3 mm.
Example 3
20g of gum arabic was added to 200g of water, and stirred to dissolve it, and then 4g of magnetosome and 4g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 7.8GHz, the reflection loss of the bandwidth is less than-10 dB in the electromagnetic wave frequency band of 2-18 GHz when the bandwidth is 3mm and-39.5 dB when the thickness is 3 mm.
Example 4
20g of gum arabic was added to 150g of water, and stirred to dissolve it, and then 4g of magnetosome and 4g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 6.7GHz when the thickness is 3mm and the reflection loss is less than-10 dB in the electromagnetic wave frequency band of 2-18 GHz when the thickness is 3 mm.
Example 5
20g of gum arabic was added to 200g of water, and stirred to dissolve it, and then 5g of magnetosome and 4g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 8.1GHz, the reflection loss of the bandwidth is less than-47.3 dB when the bandwidth is 3mm, and the reflection loss of the bandwidth is less than-10 dB when the bandwidth is 3 mm.
Example 6
20g of gum arabic was added to 200g of water, and stirred to dissolve it, and then 6g of magnetosome and 4g of carbon fiber were added thereto, and suspended using a high-speed shearing machine at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is-44.8 dB when the thickness is 3mm, and the bandwidth is 7.8GHz when the reflection loss is less than-10 dB in an electromagnetic wave frequency band of 2-18 GHz when the thickness is 3 mm.
Example 7
20g of polyurethane was added to 200g of ethyl acetate, stirred to dissolve it, and then 5g of magnetosome and 5g of carbon fiber were added thereto, and they were brought into a suspended state using a high-speed shearer at a power of 1200W and a pressure of 0.8 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1000bar, and then spray-drying, wherein the air inlet temperature of the spray-drying is 180 ℃, and the feeding speed is 60kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 6.5GHz when the thickness is 3mm and the reflection loss is less than-10 dB in the electromagnetic wave frequency band of 2-18 GHz when the thickness is 3mm, and-45.2 dB.
Example 8
20g of polystyrene was added to 200g of ethyl acetate, and stirred to be dissolved, then 5g of magnetosome and 5g of graphene were added thereto, and they were brought into a suspended state using a high-speed shearer at a power of 1000W and a pressure of 1.0 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 800bar, and then spray-drying, wherein the inlet air temperature of the spray-drying is 200 ℃, and the feeding rate is 100kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
Dispersing the wave-absorbing material in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and mixing the wave-absorbing material/paraffinPressing into a ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 6.7GHz when the thickness is 3mm and the reflection loss is less than-10 dB in the electromagnetic wave frequency band of 2-18 GHz when the thickness is 3 mm.
Example 9
20g of polyacrylic acid was added to 200g of ethyl acetate, and stirred to dissolve the polyacrylic acid, and then 5g of magnetosome and 10g of graphene were added thereto, and suspended by using a high-speed shearing machine at a power of 1500W and a pressure of 0.6 MPa. Homogenizing the obtained suspension by a high-pressure homogenizer under the pressure of 1200bar, and then spray-drying, wherein the inlet air temperature of the spray-drying is 160 ℃, and the feeding rate is 80kg/h, so as to obtain the solid nano-dispersion wave-absorbing material.
The wave-absorbing material is dispersed in paraffin, wherein the mass fraction of the wave-absorbing material is 30%, and the wave-absorbing material/paraffin mixture is pressed into a circular ring with the outer diameter of 7mm, the inner diameter of 3mm and the thickness of 3 mm. The lowest reflection loss value (RL) is obtained by testing the dielectric constant and the magnetic conductivity of the wave-absorbing material by using a vector network analyzermin) The bandwidth is 7.6GHz, the reflection loss of the bandwidth is less than-38.1 dB at the thickness of 3mm in the electromagnetic wave frequency band of 2-18 GHz, and the bandwidth is 7.6 GHz.
Claims (3)
1. A solid nano dispersion wave-absorbing material is characterized in that: the wave-absorbing material is prepared by uniformly mixing a magnetosome, a binder, a carbon material and a solvent according to the mass ratio of 1: 3-8: 0.5-3: 20-100, and then carrying out spray drying; wherein, the binder is firstly added into the solvent, stirred and dissolved, and then added with the magnetosome and the carbon material; the uniform mixing mode comprises high-speed shearing and then high-pressure homogenizing, wherein the high-speed shearing power is 1000-1500W, the pressure is 0.6-1.2 MPa, and the high-pressure homogenizing pressure is 500-1200 bar;
the carbon material is carbon fiber or graphene;
the binder is any one or a mixture of more of Arabic gum, maltodextrin, polystyrene, polyurethane, polyaniline and polyacrylic acid;
the solvent is any one of water, ethyl acetate and acetone.
2. The solid nano-dispersion wave-absorbing material according to claim 1, wherein: the mass ratio of the magnetosome to the binder, the carbon material and the solvent is 1: 4-5: 1-2: 30-50.
3. The solid nano-dispersion wave-absorbing material according to claim 1, wherein: the air inlet temperature of the spray drying is 160-200 ℃, and the feeding rate is 50-200 kg/h.
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