CN110712400B - Method for preparing layered carbon fiber electromagnetic shielding composite material by using three-dimensional carbon/ferroferric oxide Koch layered layer - Google Patents
Method for preparing layered carbon fiber electromagnetic shielding composite material by using three-dimensional carbon/ferroferric oxide Koch layered layer Download PDFInfo
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Abstract
The invention relates to a method for preparing a layered carbon fiber electromagnetic shielding composite material by using a three-dimensional carbon/ferroferric oxide Koch fractal layer, which comprises the following steps of preparing a Koch fractal pattern in a linear cutting mode, obtaining a mold of a fractal region and a non-fractal region, and then: 1) preparing three-dimensional carbon; 2) preparing three-dimensional carbon epoxy resin mixed filler; 3) preparing ferroferric oxide epoxy resin mixed filler; 4) preparing a Koch-shaped layer of the absorption layer; 5) and (4) preparing an integral composite material.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a method for preparing a layered carbon fiber electromagnetic shielding composite material.
Background
In modern society, electronic pollution such as electronic noise, electromagnetic interference (EMI) and Radio Frequency Interference (RFI) rapidly rises with the rapid spread and increase in use of electronic equipment, resulting in malfunction of the electronic equipment. Metals and their alloys can be the best emi shielding materials, but their weight, cost, and corrosion resistance are high, limiting their application in emi shielding. The emergence of carbon fiber polymer composite materials is gradually replacing metal and metal alloy-based electromagnetic interference shielding materials, which have the characteristics of light weight, good corrosion resistance, good electrical, dielectric, thermal and mechanical properties and the like, and are very effective in inhibiting electromagnetic noise. Wherein the carbon filler is as follows: carbon nanofillers in various forms such as carbon black, carbon nanotubes, graphite, graphene oxide, graphene nanoplatelets, graphene nanoribbons, graphene nanoplatelets, and the like have been widely studied as fillers replacing metal bases. However, the carbon material is difficult to mass-produce when made into a composite material sample due to the limitations of size, process, cost, and the like. Carbon materials should therefore be used as one of the fillers in composite materials. Meanwhile, the advantages of the metal matrix as the traditional electromagnetic interference shielding material should not be ignored, and the composite material prepared by combining the advanced carbon material and the traditional metal material in a novel mode can not only exert the advantages of different types of fillers, but also obtain excellent electromagnetic interference shielding effect.
The development direction of the electromagnetic shielding composite material at present can be summarized into the following three aspects:
the first is the design of multilayer structure, can design combined material's impedance matching layer, absorbed layer, reflection stratum. The impedance matching layer can enable electromagnetic waves to better enter the wave absorbing layer; the electromagnetic wave is absorbed in the wave-absorbing layer; meanwhile, the strong reflection layer is reflected to carry out multiple absorption on electromagnetic waves, but in this aspect, the electromagnetic waves are simply stacked in a layered mode, and the problem of lack of interlayer design exists.
And secondly, the application of various loss mechanisms, namely the composition of various loss mechanisms, such as the composition of metal micro powder, carbon materials, conductive polymers and the like, can be carried out on the filler of the absorption layer. However, the problem with this aspect is that the filler is difficult to apply to the actual composite after its preparation.
Thirdly, patterning design of the electromagnetic protection material is carried out, so that the material has super-strong absorption effect in a certain frequency band; the problems of single action frequency band, incapability of meeting the multi-frequency-band absorption effect, high cost and complex process exist.
The literature indicates that people mainly focus on means for improving the electromagnetic shielding performance of the carbon fiber composite material: mixing the conductive or magnetic conductive material with the carbon fiber and modifying the surface of the carbon fiber. The method for mixing the conductive or magnetic conductive material with the carbon fiber is mainly characterized in that a single type of carbon nano filler or ferroferric oxide and other magnetic conductive materials are added on the surface of the carbon fiber composite material, so that the electromagnetic waves are lost through the conductive material or the magnetic conductive material in the transmission process. The surface modification method of the carbon fiber generally comprises the step of growing carbon nanotubes on the surface of the carbon fiber or chemically plating a metal magnetic conductive material to improve the electromagnetic shielding performance of the carbon fiber composite material. There are also some methods to creatively mix the conductive and magnetic conductive materials by fractal theory to achieve special electromagnetic shielding effect.
Among numerous fractal theories, the Koch fractal theory can theoretically infinitely increase the perimeter with the continuous increase of fractal times due to the unique size effect under the condition of not exceeding the area of a triangle circumcircle, and a large number of regularly distributed multi-element scale spaces which change according to a certain rule are formed in the fractal process, so that the characteristic can generate a special electromagnetic shielding effect due to the special size effect of electromagnetic waves. Therefore, the filler which utilizes two loss mechanisms of three-dimensional carbon and ferroferric oxide distributed in a Koch fractal theory form is designed to be used as an absorption layer applied to the carbon fiber electromagnetic protection composite material, and a good electromagnetic shielding effect can be generated. In the invention, a Koch fractal pattern is prepared by utilizing a linear cutting mode to obtain a mould of a fractal region and an undistributed region.
Disclosure of Invention
The invention provides a method for preparing a layered carbon fiber electromagnetic shielding composite material, which aims to solve the problem of combining an electric loss type electromagnetic shielding filler with a magnetic loss type electromagnetic shielding filler on a macroscopic scale and achieve the aim of achieving a good shielding effect at high frequency and low frequency simultaneously. The invention takes surface layer glass fiber as a wave-transmitting layer, three-dimensional carbon epoxy resin mixed filler and ferroferric oxide epoxy resin mixed filler are distributed in the middle as an absorption layer in a Koch fractal form, and carbon fiber is taken as a reflection layer at the bottom layer to form the carbon fiber electromagnetic shielding composite material with a layered design, thereby obviously improving the electromagnetic shielding performance at 6-12 GHz. The technical scheme of the invention is as follows:
a method for preparing a layered carbon fiber electromagnetic shielding composite material by using a three-dimensional carbon/ferroferric oxide Koch fractal layer is implemented by preparing a Koch fractal pattern in a wire cutting mode, obtaining a mold of a fractal region and a mold of an undistributed region and then performing the following steps:
1) preparing three-dimensional carbon;
2) preparing three-dimensional carbon epoxy resin mixed filler: three-dimensional carbon and epoxy resin are mixed according to the following ratio of (2.5-3.5): preparing a filler according to the mass ratio of 100, then mixing and stirring, and adding a silane coupling agent with the mass fraction of 1% as an auxiliary dispersing agent;
3) preparing a ferroferric oxide epoxy resin mixed filler: mixing ferroferric oxide and epoxy resin according to the weight ratio of (25-35): 100 mass percent of the filler is prepared, then mixing and stirring are carried out, and 1 mass percent of silane coupling agent is added as a dispersion aid.
4) Preparation of the Koch-shaped layer of the absorption layer: firstly, a layer of carbon fiber prepreg is laid below a mold, then the mold of a fractal region is placed at a specified position according to the fractal size of the fractal mold, and then the ferroferric oxide epoxy resin mixed filler is mixed according to the mass ratio of 10: 1, adding a triethylenetetramine curing agent in the proportion of 1, uniformly stirring, uniformly distributing the mixture in an undistributed area, then placing a sample in a vacuum oven at 60 ℃, preserving the temperature for a period of time, semi-curing ferroferric oxide epoxy resin mixed filler in the undistributed area, taking out a fractal die, and mixing the three-dimensional carbon epoxy resin mixed filler according to the mass ratio of 10: 1, adding a triethylenetetramine curing agent in the proportion, uniformly stirring, and uniformly distributing the mixture in a fractal region; finally, preserving the heat for a period of time in a vacuum oven at 60 ℃ to completely solidify the sample and finish the preparation of the laminated layer;
5) preparing an integral composite material: and spreading two layers of glass fiber prepregs on the upper layer and three layers of carbon fiber prepregs on the lower layer of the cured parting layer, fixing the layers in a mold, and curing for a period of time at 120 ℃ in a forced air drying oven to obtain the electromagnetic shielding test sample.
In conclusion, the core of the invention is that three-dimensional carbon and ferroferric oxide are distributed in a Koch fractal mode, three-dimensional carbon epoxy resin mixed filler is put in a fractal region, ferroferric oxide epoxy resin mixed filler is put in an undistributed region, and the electromagnetic shielding performance of the composite material is continuously increased along with the increase of the Koch fractal frequency. Compared with the prior art, the invention has the advantages that:
(1) the invention has low cost, the used three-dimensional carbon and ferroferric oxide can be simply prepared, and the raw materials are easy to obtain and have low price; compared with other types of electromagnetic protection packing, the cost is greatly reduced.
(2) The invention utilizes the fractal theory of layered structure design and patterning to compound the traditional electromagnetic protection material and the novel nano carbon filler in the corresponding fractal region and the non-fractal region, so that the materials can play roles in different frequency bands. The shielding effect of the composite material at high frequency and low frequency is greatly improved; and the method has strong designable type, and can carry out optimization design according to environment and performance requirements.
(3) The method has the advantages of simple equipment, simple process, high reliability, good repeatability, good application prospect and environmental protection.
Drawings
FIG. 1 is a scanned photograph of a sample charge
FIG. 2 is a flow chart of preparation of a secondary fractal sample
FIG. 3 is a graph showing the shielding performance of the sample at 1-18 GHz
Detailed Description
The three-dimensional carbon related to the invention adopts the following preparation method:
preparation of three-dimensional carbon: mixing sodium chloride and glucose according to the weight ratio of 30: 100 parts were prepared as aqueous solutions. And then carrying out spray drying in a spray dryer according to the parameters of 180 ℃ of air inlet temperature, 90 ℃ of air outlet temperature, 25r/min of air outlet speed, 20 times/min of needle passing frequency and 15ml/min of peristaltic speed to obtain the composite powder of glucose and sodium chloride. The composite powder was then calcined in a tube furnace at 760 ℃ for two hours under an argon (200-. And finally, carrying out suction filtration on the obtained black powder in a suction filtration system, and drying the sample to obtain a three-dimensional carbon sample.
Example 1
(1) And (3) mixing the following components in percentage by mass: adding 1% of silane coupling agent by mass into 100 three-dimensional carbon and epoxy resin mixed filler, stirring for 10min, performing ultrasonic treatment in an ultrasonic oscillation machine for 30min, and standing for 60 min. Obtaining the three-dimensional carbon epoxy resin mixed filler.
(2) Adding 1% of silane coupling agent by mass into 30: 100 ferroferric oxide and epoxy resin mixed filler. Stirring for 10min, performing ultrasonic treatment in an ultrasonic shaker for 30min, and standing for 60 min. Obtaining the ferroferric oxide epoxy resin mixed filler.
(3) In the forming process, firstly, 10 percent of triethylene tetramine curing agent by mass is added into the ferroferric oxide epoxy resin mixed filler, and the mixture is uniformly stirred. Adding ferroferric oxide mixed filler into an undistributed area around the secondary fractal mould, and semi-curing at 60 ℃ for half an hour in a vacuum oven as shown in figure 2 (a).
(4) After the fractal region die is taken out, the effect is shown in fig. 2(b), the three-dimensional carbon mixed filler is added, then the sample is placed into a vacuum oven at 60 ℃ and is completely cured for 240min, and a fractal layer is obtained, as shown in fig. 2(c) and (d).
(5) Spreading two layers of glass fibers on the upper surface of the fractal layer, spreading three layers of carbon fibers on the lower layer, putting the fractal layer into a forming die, and completely curing at 120 ℃ for 2 hours to obtain a composite material with the thickness of 2mm, as shown in (e) and (f) in the figure.
The preparation process of the fractal sample and the fractal sample for the first time is the same as that of the fractal sample for the second time, but the amounts of the added ferroferric oxide epoxy resin mixed filler and the added three-dimensional carbon epoxy resin mixed filler are different because the areas of the fractal region and the fractal region are different, and the description is not necessarily carried out here.
Example 2
(1) And (2) mixing the following components in percentage by mass: adding 1% of silane coupling agent by mass into 100 three-dimensional carbon and epoxy resin mixed filler, stirring for 10min, performing ultrasonic treatment in an ultrasonic oscillation machine for 30min, and standing for 60 min. Obtaining the three-dimensional carbon epoxy resin mixed filler.
(2) Adding 1% of silane coupling agent by mass into the mixed filler of ferroferric oxide and epoxy resin with the mass ratio of 20: 100. Stirring for 10min, performing ultrasonic treatment in an ultrasonic shaker for 30min, and standing for 60 min. Obtaining the ferroferric oxide epoxy resin mixed filler.
(3) In the forming process, firstly, 10 percent of triethylene tetramine curing agent by mass is added into the ferroferric oxide epoxy resin mixed filler, and the mixture is uniformly stirred. Adding ferroferric oxide mixed filler into an undistributed area around the secondary fractal mould, and semi-curing at 60 ℃ for half an hour in a vacuum oven as shown in figure 2 (a).
(4) After the fractal region die is taken out, the effect is shown in fig. 2(b), the three-dimensional carbon mixed filler is added, then the sample is placed into a vacuum oven at 60 ℃ and is completely cured for 240min, and a fractal layer is obtained, as shown in fig. 2(c) and (d).
(5) Spreading two layers of glass fibers on the upper surface of the fractal layer, spreading three layers of carbon fibers on the lower layer, putting the fractal layer into a forming die, and completely curing at 120 ℃ for 2 hours to obtain a composite material with the thickness of 2mm, as shown in (e) and (f) in the figure.
The preparation process of the fractal sample and the fractal sample for the first time is the same as that of the fractal sample for the second time, but the amounts of the added ferroferric oxide epoxy resin mixed filler and the added three-dimensional carbon epoxy resin mixed filler are different because the areas of the fractal region and the fractal region are different, and the description is not necessarily carried out here.
Example 3
(1) Mixing the components in a mass ratio of 1: adding 0.5 mass percent of silane coupling agent into 100 parts of three-dimensional carbon and epoxy resin mixed filler, stirring for 10min, carrying out ultrasonic treatment in an ultrasonic oscillation machine for 30min, and standing for 60 min. Obtaining the three-dimensional carbon epoxy resin mixed filler.
(2) Adding 0.5 mass percent of silane coupling agent into the mixed filler of ferroferric oxide and epoxy resin with the mass ratio of 10 to 100. Stirring for 10min, performing ultrasonic treatment in an ultrasonic shaker for 30min, and standing for 60 min. Obtaining the ferroferric oxide epoxy resin mixed filler.
(3) In the forming process, firstly, 10 percent of triethylene tetramine curing agent by mass is added into the ferroferric oxide epoxy resin mixed filler, and the mixture is uniformly stirred. Adding ferroferric oxide mixed filler into an undistributed area around the secondary fractal mould, and semi-curing at 60 ℃ for half an hour in a vacuum oven as shown in figure 2 (a).
(4) After the fractal region die is taken out, the effect is shown in fig. 2(b), the three-dimensional carbon mixed filler is added, then the sample is placed into a vacuum oven at 60 ℃ and is completely cured for 240min, and a fractal layer is obtained, as shown in fig. 2(c) and (d).
(5) Spreading two layers of glass fibers on the upper surface of the fractal layer, spreading three layers of carbon fibers on the lower layer, putting the fractal layer into a forming die, and completely curing at 120 ℃ for 2 hours to obtain a composite material with the thickness of 2mm, as shown in (e) and (f) in the figure.
The preparation process of the fractal sample and the fractal sample for the first time is the same as that of the fractal sample for the second time, but the amounts of the added ferroferric oxide epoxy resin mixed filler and the added three-dimensional carbon epoxy resin mixed filler are different because the areas of the fractal region and the fractal region are different, and the description is not necessarily carried out here.
Example 4
(1) And (2) mixing the components in a mass ratio of 4: adding 1.5 mass percent of silane coupling agent into 100 three-dimensional carbon and epoxy resin mixed filler, stirring for 10min, carrying out ultrasonic treatment in an ultrasonic oscillation machine for 30min, and standing for 60 min. Obtaining the three-dimensional carbon epoxy resin mixed filler.
(2) Adding 1.5 mass percent of silane coupling agent into the mixed filler of ferroferric oxide and epoxy resin with the mass ratio of 40 to 100. Stirring for 10min, performing ultrasonic treatment in an ultrasonic shaker for 30min, and standing for 60 min. Obtaining the ferroferric oxide epoxy resin mixed filler.
(3) In the forming process, firstly, 10 percent of triethylene tetramine curing agent by mass is added into the ferroferric oxide epoxy resin mixed filler, and the mixture is uniformly stirred. Adding ferroferric oxide mixed filler into an undistributed area around the secondary fractal mould, and semi-curing at 60 ℃ for half an hour in a vacuum oven as shown in figure 2 (a).
(4) After the fractal region die is taken out, the effect is shown in fig. 2(b), the three-dimensional carbon mixed filler is added, then the sample is placed into a vacuum oven at 60 ℃ and is completely cured for 240min, and a fractal layer is obtained, as shown in fig. 2(c) and (d).
(5) Spreading two layers of glass fibers on the upper surface of the fractal layer, spreading three layers of carbon fibers on the lower layer, putting the fractal layer into a forming die, and completely curing at 120 ℃ for 2 hours to obtain a composite material with the thickness of 2mm, as shown in (e) and (f) in the figure.
The preparation process of the fractal sample and the fractal sample for the first time is the same as that of the fractal sample for the second time, but the amounts of the added ferroferric oxide epoxy resin mixed filler and the added three-dimensional carbon epoxy resin mixed filler are different because the areas of the fractal region and the fractal region are different, and the description is not necessarily carried out here.
Control sample
Adding pure epoxy resin with corresponding mass into the original parting zone, spreading two layers of glass fiber on the upper layer and three layers of carbon fiber on the lower layer after curing, and taking the composite material obtained after curing as a control sample.
Claims (1)
1. A method for preparing a layered carbon fiber electromagnetic shielding composite material by using a three-dimensional carbon/ferroferric oxide Koch fractal layer is implemented by preparing a Koch fractal pattern in a wire cutting mode, obtaining a mold of a fractal region and a mold of an undistributed region and then performing the following steps:
1) preparing three-dimensional carbon;
2) preparing three-dimensional carbon epoxy resin mixed filler: three-dimensional carbon and epoxy resin are mixed according to the following ratio of (2.5-3.5): preparing a filler according to the mass ratio of 100, then mixing and stirring, and adding a silane coupling agent with the mass fraction of 1% as an auxiliary dispersing agent;
3) preparing a ferroferric oxide epoxy resin mixed filler: mixing ferroferric oxide and epoxy resin according to the weight ratio of (25-35): preparing a filler according to the mass ratio of 100, then mixing and stirring, and adding a silane coupling agent with the mass fraction of 1% as an auxiliary dispersing agent;
4) preparation of the Koch-shaped layer of the absorption layer: firstly, a layer of carbon fiber prepreg is laid below a mold, then the mold of a fractal region is placed at a specified position according to the fractal size of the fractal mold, and then the ferroferric oxide epoxy resin mixed filler is mixed according to the mass ratio of 10: 1, adding a triethylenetetramine curing agent in the proportion of 1, uniformly stirring, uniformly distributing the mixture in an undistributed area, then placing a sample in a vacuum oven at 60 ℃, preserving the temperature for a period of time, semi-curing ferroferric oxide epoxy resin mixed filler in the undistributed area, taking out a fractal die, and mixing the three-dimensional carbon epoxy resin mixed filler according to the mass ratio of 10: 1, adding a triethylenetetramine curing agent in the proportion, uniformly stirring, and uniformly distributing the mixture in a fractal region; finally, preserving the heat for a period of time in a vacuum oven at 60 ℃ to completely solidify the sample and finish the preparation of the laminated layer;
5) preparing an integral composite material: and spreading two layers of glass fiber prepregs on the upper layer and three layers of carbon fiber prepregs on the lower layer of the cured parting layer, fixing the layers in a mold, and curing for a period of time at 120 ℃ in a forced air drying oven to obtain the electromagnetic shielding test sample.
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