CN110041884B - Leaf-shaped nano Fe3O4Preparation method of filled wave-absorbing composite material with honeycomb sandwich structure - Google Patents
Leaf-shaped nano Fe3O4Preparation method of filled wave-absorbing composite material with honeycomb sandwich structure Download PDFInfo
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- CN110041884B CN110041884B CN201810034210.0A CN201810034210A CN110041884B CN 110041884 B CN110041884 B CN 110041884B CN 201810034210 A CN201810034210 A CN 201810034210A CN 110041884 B CN110041884 B CN 110041884B
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Abstract
The invention discloses leaf-shaped nano Fe3O4A preparation method of a filled wave-absorbing composite material with a honeycomb sandwich structure relates to the technical field of electromagnetic stealth composite materials, and alpha-Fe with a leaf shape is synthesized by taking potassium ferricyanide as a raw material through a hydrothermal method2O3(ii) a Reducing into nanometer Fe with leaf shape by high temperature heat treatment3O4Filling the mixture into honeycomb holes of a periodic aramid fiber honeycomb plate, and respectively covering glass fiber reinforced resin matrix composite material skins and carbon fiber reinforced resin matrix composite material skins on the upper side and the lower side of the honeycomb plate to obtain leaf-shaped nano Fe3O4The filled wave-absorbing composite material with the honeycomb sandwich structure. The effective absorption frequency bandwidth is 2.6GHz (12.8GHz-15.4GHz) under the thickness of 4mm, and the maximum absorption intensity at the position of 14.2GHz reaches-36 dB. The technical problems of poor electromagnetic wave absorption strength and poor mechanical bearing capacity of the traditional wave-absorbing material are solved.
Description
Technical Field
The invention relates to the technical field of electromagnetic stealth composite materials, in particular to leaf-shaped nano Fe3O4A method for preparing a filled wave-absorbing composite material with a honeycomb sandwich structure.
Background
With the development of modern radar detection technology in the military field, weaponry represented by military fighters is tracked and detected more and more frequently; meanwhile, in the civil field, the development of the radio communication technology brings about the problem of serious electromagnetic radiation pollution while bringing convenience to life of people. Therefore, the energy of the electromagnetic wave can be converted into heat energy to be lost, thereby remarkably reducing the electromagnetic wave reflectionElectromagnetic wave absorbing materials have received increasing attention as the most effective solution to the above problems. Due to the limitation of practical use environment, the ideal performance characteristics of the electromagnetic wave absorbing material include: wide effective absorption frequency band, light material density, thin material thickness and high mechanical strength. The ferrite wave-absorbing material consists of iron element, oxygen element and a series of metal elements with different valence states. As one of the most widely studied wave absorbers at present, the domain wall resonance and the natural resonance are the most dominant absorption mechanisms, and the resistivity is 102-108And has both magnetic loss capability and dielectric loss capability. Wherein Fe3O4As a traditional magnetic wave-absorbing material, the material is the most widely applied material in ferrite, has the advantages of high magnetic conductivity, high wave-absorbing strength, simple preparation and the like, and is Fe as a double-loss medium3O4Magnetic absorbing materials have both magnetic and dielectric losses to electromagnetic waves, but traditionally, Fe is used3O4The magnetic wave-absorbing material is easy to wear and damage in the process of using a coating type coating as a main part, and the requirement of the modern aircraft on the integration of the structure bearing and the wave-absorbing function of the wave-absorbing material is difficult to realize due to the state of the coating.
Disclosure of Invention
To overcome the above Fe3O4The magnetic wave-absorbing material is easy to wear and damage in the process of using a coating type coating as a main part, and the defects of the prior art that the requirement of the modern aircraft on the integration of the structure bearing and wave-absorbing function of the wave-absorbing material is difficult to realize due to the state of the coating are overcome, and the invention provides the leaf-shaped nano Fe3O4A method for preparing a filled wave-absorbing composite material with a honeycomb sandwich structure.
The technical scheme adopted by the invention is as follows: alpha-Fe with leaf shape is synthesized by hydrothermal method by taking potassium ferricyanide as raw material2O3(ii) a Adopting a high-temperature heat treatment method to remove alpha-Fe in the shape of leaves2O3Reducing into nanometer Fe with leaf shape3O4. The prepared leaf-shaped nano Fe3O4Filling into honeycomb holes of a periodic aramid fiber honeycomb plate, and respectively covering glass on the upper side and the lower side of the honeycomb plateThe leaf-shaped nano Fe is finally obtained by using the fiber reinforced resin matrix composite skin and the carbon fiber reinforced resin matrix composite skin3O4The filled wave-absorbing composite material with the honeycomb sandwich structure.
The method comprises the following steps:
(1) dissolving potassium ferricyanide in deionized water; obtaining potassium ferricyanide solution, pouring the potassium ferricyanide solution into a 100mL inner container of a polytetrafluoroethene reaction kettle, sealing, carrying out high-temperature hydrothermal reaction to obtain leaf-shaped nano alpha-Fe2O3Centrifuging to collect precipitate, washing with deionized water and alcohol in sequence, and drying to obtain leaf-shaped nano alpha-Fe2O3And (3) sampling.
(2) The dried leaf-shaped nano alpha-Fe obtained in the step (1)2O3Placing the sample in a tube furnace, and carrying out high-temperature heat treatment in a mixed gas environment of hydrogen and argon to obtain leaf-shaped nano Fe3O4And (3) a wave-absorbing material.
(3) Leaf-shaped nano Fe prepared in the step (2)3O4Filling wave-absorbing materials into the periodic aramid fiber honeycomb plate, respectively covering glass fiber reinforced resin matrix composite wave-transmitting skins and carbon fiber reinforced resin matrix composite skins with the thickness of 0.5mm on the upper and lower sides of the honeycomb plate by adopting a glue film bonding method, and finally obtaining leaf-shaped nano Fe3O4A wave-absorbing composite material with a honeycomb sandwich structure filled with wave-absorbing materials.
Dissolving the potassium ferricyanide in the step (1) in deionized water, wherein the concentration of the potassium ferricyanide is 0.1 mol/L;
performing high-temperature hydrothermal reaction in the step (1), wherein the reaction temperature is 100-150 ℃, and the reaction time is 12-48 h;
the centrifugation condition of the step (1) is 7000-9000rpm centrifugation for 5-15 min; the drying temperature is not higher than 80 ℃.
And (3) mixing the hydrogen and the argon in the step (2), wherein the flow rates of the hydrogen and the argon are respectively 10mL/min and 120 mL/min. The heat treatment temperature in the step (2) is 300-500 ℃, and the time is 1-2 h.
The specification of the periodic aramid fiber honeycomb plate in the step (2) is 300mm multiplied by 2mm, 300mm multiplied by 3mm or 300mm multiplied by 4mm, and the aperture is 2mm-10 mm; the resin matrix of the glass fiber reinforced resin matrix composite wave-transmitting skin covered on the upper surface of the filled honeycomb plate is epoxy resin or cyanate resin.
Compared with the prior art, the invention has the beneficial effects that
(1) Adopts a hydrothermal method to synthesize the nano alpha-Fe with the shape of leaves2O3Precursor is subjected to heat treatment in reducing gas environment to obtain leaf-shaped nano Fe3O4The wave-absorbing material can realize the leaf-shaped nano Fe product by controlling the hydrothermal reaction time and temperature3O4And effectively regulating and controlling the size of the appearance.
(2) Adopting leaf-shaped nano Fe3O4The method for compounding the wave-absorbing material and the honeycomb sandwich structure prepares the broadband wave-absorbing composite material with mechanical bearing capacity, can effectively control the mechanical strength of the composite material by adjusting the layer laying scheme of fibers in the fiber reinforced resin matrix composite material skin, and realizes the integrated design of the bearing and wave-absorbing functions of the wave-absorbing composite material structure.
(3) The composite material is compounded with other materials, so that the structural bearing and wave absorbing performance is improved. Through the combination of the loss type wave-absorbing material and the special structure, the strong electromagnetic wave absorption effect is realized, and the overall mechanical strength of the material is improved.
Drawings
FIG. 1 shows leaf-shaped nano Fe prepared in example 13O4Scanning electron microscope photographs;
FIG. 2 shows leaf-shaped nano Fe particles obtained in example 13O4Schematic drawing of a filled honeycomb sandwich structure composite material flat plate;
FIG. 3 shows leaf-shaped nano Fe prepared in example 13O4The filled honeycomb sandwich structure composite material plate has the electromagnetic wave reflectivity of 2-18 GHz.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
(1) Dissolving 2.63g of potassium ferricyanide in 80mL of deionized water, and stirring at a medium speed for 1h by magnetic force; obtaining potassium ferricyanide solution to obtainPouring the red solution into a 100mL inner container of a polytetravinyl reactor, sealing and putting the inner container into a stainless steel shell, and carrying out hydrothermal reaction for 48 hours at 140 ℃ to obtain the leaf-shaped nano alpha-Fe2O3The precipitate was collected by centrifugation at 8000rpm for 10min and washed several times with deionized water and alcohol. And drying for 24 hours in an air drying oven at 60 ℃ for later use.
(2) Leaf-shaped nano alpha-Fe obtained in the step (1)2O3Placing the sample in a tube furnace, and carrying out heat treatment at 350 ℃ for 1h in the mixed gas environment of reducing hydrogen and argon to obtain leaf-shaped nano Fe3O4And (3) a wave-absorbing material. Scanning electron micrographs showed the product to be in the shape of a special nano-leaf, as shown in FIG. 1. Heat treatment process for reducing alpha-Fe2O3The flow rates of hydrogen and argon in the mixed gas of hydrogen and argon are respectively 10ml/min and 120 ml/min.
(3) 50g of leaf-shaped nano Fe prepared in the step (2)3O4The wave absorbing material is filled into a periodic aramid honeycomb plate with three thicknesses of 300mm multiplied by 2mm, 300mm multiplied by 3mm and 300mm multiplied by 4mm, the periodic aramid honeycomb plate with the aperture of 4mm is covered with a glass fiber reinforced resin matrix composite wave transmitting skin and a carbon fiber reinforced resin matrix composite skin with the thickness of 0.5mm by a glue film bonding method, the resin matrix of the glass fiber reinforced resin matrix composite wave transmitting skin covered on the upper surface of the filled honeycomb plate is epoxy resin, and finally, the leaf-shaped nano Fe is obtained3O4The wave-absorbing composite material with the honeycomb sandwich structure filled with the wave-absorbing material is shown in an attached figure 2.
National military standard GJB 2038A-2011 bow-shaped frame method for three thicknesses of leaf-shaped nano Fe3O4The reflectivity of 2-18GHz electromagnetic waves of the wave-absorbing composite material plate with the honeycomb sandwich structure filled with the wave-absorbing material is tested, and the result is shown as a reflection loss test curve in the attached figure 3, wherein the reflection loss under the thickness of 4mm is lower than-10 dB, the effective absorption frequency bandwidth is 2.6GHz (12.8GHz-15.4GHz), and the maximum absorption intensity at the position of 14.2GHz reaches-36 dB.
Example 2
(1) Dissolving 2.63g of potassium ferricyanide in 80mL of deionized water, and stirring at a medium speed for 1h by magnetic force; obtaining potassium ferricyanide solutionPouring the obtained red solution into a 100mL inner container of a polytetravinyl reactor, sealing and placing the red solution into a stainless steel shell, and carrying out hydrothermal reaction for 12 hours at 100 ℃ to obtain leaf-shaped nano alpha-Fe2O3The precipitate was collected by centrifugation at 7000rpm for 5min and washed several times with deionized water and alcohol. And drying for 24 hours at 50 ℃ in an air drying oven for later use.
(2) Leaf-shaped nano alpha-Fe obtained in the step (1)2O3Placing the sample in a tube furnace, and carrying out heat treatment at 300 ℃ for 1h in the mixed gas environment of reducing hydrogen and argon to obtain leaf-shaped nano Fe3O4And (3) wave-absorbing materials. Heat treatment process for reducing alpha-Fe2O3The flow rates of hydrogen and argon in the mixed gas of hydrogen and argon are respectively 10ml/min and 120 ml/min.
(3) 50g of leaf-shaped nano Fe prepared in the step (2)3O4Filling the wave-absorbing material into a periodic aramid honeycomb plate with the aperture of 2mm and three thicknesses of 300mm multiplied by 2mm, 300mm multiplied by 3mm and 300mm multiplied by 4mm, respectively capping a glass fiber reinforced resin matrix composite wave-transmitting skin and a carbon fiber reinforced resin matrix composite skin with the thickness of 0.5mm on the upper and the lower sides of the honeycomb plate by adopting a glue film bonding method, wherein the resin matrix of the glass fiber reinforced resin matrix composite wave-transmitting skin covered on the upper surface of the filled honeycomb plate is cyanate resin, and finally obtaining the leaf-shaped nano Fe3O4A wave-absorbing composite material with a honeycomb sandwich structure filled with wave-absorbing materials.
National military standard GJB 2038A-2011 bow-shaped frame method for three thicknesses of leaf-shaped nano Fe3O4The reflectivity of 2-18GHz electromagnetic waves of the wave-absorbing composite material plate with the honeycomb sandwich structure filled with the wave-absorbing material is tested, and as a result, the effective absorption frequency bandwidth of 1.5GHz (13.4GHz-14.9GHz) with the reflection loss lower than-10 dB under the thickness of 2mm, and the maximum absorption intensity at the 14GHz position reaches-21 dB.
Example 3
(1) Dissolving 2.63g of potassium ferricyanide in 80mL of deionized water, and stirring at a medium speed for 1h by magnetic force; obtaining potassium ferricyanide solution, pouring the obtained red solution into a 100mL poly-tetra-volt ethylene reaction kettle inner container, sealing and placing the red solution into a stainless steel shell, and carrying out hydrothermal reaction for 48 hours at 150 ℃ to obtain the leaf-shaped nano-particlesalpha-Fe of rice2O3The precipitate was collected by centrifugation at 9000rpm for 15min and washed several times with deionized water and ethanol. And drying for 24 hours at 80 ℃ in an air drying oven for later use.
(2) Leaf-shaped nano alpha-Fe obtained in the step (1)2O3Placing the sample in a tube furnace, and carrying out heat treatment at 500 ℃ for 2h in a reducing hydrogen and argon mixed gas environment to obtain leaf-shaped nano Fe3O4And (3) a wave-absorbing material. Heat treatment process for reducing alpha-Fe2O3The flow rates of hydrogen and argon in the mixed gas of hydrogen and argon are respectively 10ml/min and 120 ml/min.
(3) 50g of leaf-shaped nano Fe prepared in the step (2)3O4Filling the wave-absorbing material into periodic aramid honeycomb plates with the three thicknesses of 300mm multiplied by 2mm, 300mm multiplied by 3mm and 300mm multiplied by 4mm, wherein the aperture of each periodic aramid honeycomb plate is 10mm, respectively covering a glass fiber reinforced resin matrix composite wave-transmitting skin and a carbon fiber reinforced resin matrix composite skin with the thicknesses of 0.5mm on the upper side and the lower side of each honeycomb plate by adopting a glue film bonding method, covering the resin matrix of the glass fiber reinforced resin matrix composite wave-transmitting skin covered on the upper surface of the filled honeycomb plate with cyanate resin, and finally obtaining the leaf-shaped nano Fe3O4A wave-absorbing composite material with a honeycomb sandwich structure filled with wave-absorbing materials.
National military standard GJB 2038A-2011 bow-shaped frame method for three thicknesses of leaf-shaped nano Fe3O4The reflectivity of 2-18GHz electromagnetic waves of the wave-absorbing composite material plate with the honeycomb sandwich structure filled with the wave-absorbing material is tested, and as a result, the effective absorption frequency bandwidth of 2.1GHz (13.1GHz-15.2GHz) with the reflection loss lower than-10 dB under the thickness of 3mm, and the maximum absorption intensity at the position of 13.8GHz reaches-25 dB.
Claims (1)
1. Leaf-shaped nano Fe3O4The preparation method of the filled wave-absorbing composite material with the honeycomb sandwich structure is characterized by comprising the following steps of: alpha-Fe with leaf shape is synthesized by hydrothermal method by taking potassium ferricyanide as raw material2O3(ii) a Adopting a high-temperature heat treatment method to remove alpha-Fe in the shape of leaves2O3Reducing into nanometer Fe with leaf shape3O4The prepared leaf-shaped nano Fe3O4Filling the mixture into honeycomb holes of a periodic aramid honeycomb plate, respectively covering glass fiber reinforced resin matrix composite skins and carbon fiber reinforced resin matrix composite skins on the upper side and the lower side of the honeycomb plate, and finally obtaining the leaf-shaped nano Fe3O4The filled wave-absorbing composite material with the honeycomb sandwich structure;
the preparation method comprises the following specific steps:
(1) dissolving potassium ferricyanide in deionized water; obtaining potassium ferricyanide solution, sealing, and carrying out high-temperature hydrothermal reaction to obtain leaf-shaped nano alpha-Fe2O3Centrifuging to collect precipitate, washing with deionized water and alcohol in sequence, and drying to obtain leaf-shaped nano alpha-Fe2O3A sample; the potassium ferricyanide is dissolved in deionized water, and the concentration is 0.1 mol/L; the high-temperature hydrothermal reaction is carried out at the reaction temperature of 100-150 ℃ for 12-48 h, and the centrifugation condition is 7000 and 9000rpm for 5-15 min; the drying temperature is not higher than 80 ℃;
(2) the dried leaf-shaped nano alpha-Fe obtained in the step (1)2O3Placing the sample in a tube furnace, and carrying out high-temperature heat treatment in a mixed gas environment of hydrogen and argon to obtain leaf-shaped nano Fe3O4A wave-absorbing material; the flow rates of the hydrogen and the argon are respectively 10mL/min and 120 mL/min; the heat treatment temperature is 300-500 ℃, and the time is 1-2 h;
(3) leaf-shaped nano Fe prepared in the step (2)3O4Filling wave-absorbing materials into the periodic aramid fiber honeycomb plate, respectively covering glass fiber reinforced resin matrix composite wave-transmitting skins and carbon fiber reinforced resin matrix composite skins with the thickness of 0.5mm on the upper and lower sides of the honeycomb plate by adopting a glue film bonding method, and finally obtaining leaf-shaped nano Fe3O4A wave-absorbing composite material with a honeycomb sandwich structure and filled with wave-absorbing materials; the specification of the periodic aramid fiber honeycomb plate is 300mm multiplied by 2mm, 300mm multiplied by 3mm or 300mm multiplied by 4mm, and the aperture is 2mm-10 mm; the resin matrix of the filled wave-transparent skin made of the glass fiber reinforced resin matrix composite material and covered on the upper surface of the honeycomb plate is epoxy resin orA cyanate ester resin.
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