CN110494030B - Preparation method of resin-reinforced ferrite solid waste based broadband electromagnetic wave absorber - Google Patents
Preparation method of resin-reinforced ferrite solid waste based broadband electromagnetic wave absorber Download PDFInfo
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Abstract
The invention discloses a preparation method of a resin reinforced ferrite solid waste based broadband electromagnetic wave absorber. According to the invention, from the angle of solid waste recycling, the resin is compounded and strengthened on the solid waste crystal boundary of the ferrite, and the interface dipole is introduced to enhance the dielectric loss, so that the performance difference caused by solid waste is balanced, the interface impedance matching and broadband electromagnetic wave absorption performance are improved, and the mechanical property and the thermodynamic stability of the electromagnetic wave absorber are enhanced.
Description
Technical Field
The invention relates to a preparation method of a broadband electromagnetic wave absorber, in particular to a preparation method of a resin-reinforced ferrite solid waste based broadband electromagnetic wave absorber, belonging to the technical field of electromagnetic functional materials.
Background
Electromagnetic shielding and electromagnetic absorption play a significant role in both the civil and military fields. The rapid development of electronic information technology and the explosive growth of intelligent internet of things products in the background of "industrial 4.0" are rapidly changing the daily life style of human beings, but also bring about serious problems of electromagnetic radiation and electromagnetic interference (EMI). Military radar countermeasure and electromagnetic stealth technologies in a complex international environment are also gradually becoming one of core technologies for improving national security and international status. The electromagnetic wave absorbing material and the absorber are considered to be key for solving the problems, have become the core of related research and products, and will occupy an important share in the frontier application fields of microwave darkrooms, wireless charging, smart homes, super roads and the like. However, for the current huge market demand, the electromagnetic wave absorbing materials represented by ferrite still have many problems of high density, weak thermal stability, poor mechanical properties, narrow absorption band, high production cost, dust pollution and the like, and the application and popularization of the electromagnetic wave absorber and related products are greatly limited.
In recent years, components such as soft magnetic ferrite cores have been widely used in industries such as electronics, computers, mobile communications, new energy, lighting, and the like, and continue to rapidly grow in emerging industries such as wireless charging, big data, electric vehicles, and 5G, and have become a cornerstone of the electronics industry. The yield of the soft magnetic ferrite in China accounts for 80% of the world, reaches 23.92 ten thousand tons in 2018, and continues to increase year by year. However, in the production process of ferrite materials and devices, a large amount of ferrite solid waste is inevitably generated in the grinding process, the solid waste amount can often reach 5-20% of the total amount of products, the recycling value is low, the treatment cost is high, and the environment is greatly polluted. The related technologies for ferrite solid waste recycling can be summarized into three categories: (1) directly crushing the raw materials to be used as raw materials; (2) adding new materials according to different proportions for mixing; (3) the compositional differences are neutralized by elemental doping. The former two still depend on the composition uniqueness of the solid waste, while the latter varies with the type of mixed solid waste. The method has the problems of grain size difference, impurities, component segregation and the like, poor mechanical property and unstable property caused by the factors, and the requirements of mainstream magnetic core products are difficult to meet, but the factors do not influence or even benefit the performance of solid wastes in the aspect of electromagnetic wave absorption. Therefore, the method for preparing the electromagnetic wave absorber with stable performance by recycling the solid waste of the soft magnetic ferrite greatly reduces the manufacturing cost and has great significance in environmental protection.
Disclosure of Invention
The present invention aims to provide a method for preparing a resin reinforced ferrite solid waste based broadband electromagnetic wave absorber. According to the invention, from the angle of solid waste recycling, the resin is modified and modified at the solid waste crystal boundary of the ferrite, the interface dipole is utilized to enhance the dielectric loss, balance the performance difference caused by solid waste, improve the interface impedance matching and the electromagnetic wave absorption performance, and enhance the mechanical property and the thermodynamic stability of the electromagnetic wave absorber.
The raw materials used by the invention are soft magnetic ferrite solid waste materials which are derived from grinding solid waste generated in the production process of soft magnetic materials and devices such as manganese zinc ferrite, nickel zinc ferrite and the like or crushing solid waste of blocks such as waste magnetic cores and the like, and the components of the soft magnetic ferrite solid waste materials can widely cover various solid waste such as power materials, high material guiding materials, wave absorbing materials, mixed materials and the like generated in the production of magnetic cores, magnetic shoes, patches and the like.
The invention provides a preparation method of a resin reinforced ferrite solid waste based broadband electromagnetic wave absorber, which comprises the steps of purifying soft magnetic ferrite solid waste through a series of steps of washing, dispersing, filtering, magnetic separation and the like, modifying and modifying a ferrite grain interface by using a coupling agent, and then carrying out composite molding and heat treatment on the ferrite grain interface and resin to obtain the electromagnetic wave absorber with excellent mechanical property and wave absorbing property. The method specifically comprises the following steps:
step 1: purification of soft magnetic ferrite solid waste
1a, fully mixing the solid waste of the soft magnetic ferrite with water, stirring and dispersing, sieving to filter out some larger impurity particles such as metal scraps, carborundum and the like, and applying a magnetic field to the obtained mixed liquid to separate magnetic soft magnetic ferrite particles from a non-magnetic impurity aqueous solution;
1b, repeating the step 1a for 1-6 times, and then drying and grinding to obtain purified soft magnetic ferrite powder;
step 2: homogenization of soft magnetic ferrite particles
Mixing the soft magnetic ferrite powder obtained in the step 1 with water and ball milling beads, putting the mixture into a ball milling tank, carrying out wet ball milling for 1-20h at a constant speed of 50-500r/min, taking out a sample, and drying to obtain the soft magnetic ferrite powder with a certain particle size and uniform particle size;
and step 3: modification of soft magnetic ferrite interface
Uniformly dissolving a coupling agent in a diluent, mixing the coupling agent with the soft magnetic ferrite powder obtained in the step 2, continuously stirring for 10-200min at 300-800 rpm/min, drying and sieving to obtain interface modified ferrite powder;
and 4, step 4: prepressing for shaping
Uniformly mixing and granulating the resin and the interface modified soft magnetic ferrite powder obtained in the step (3) according to the mass ratio of 1-200%, drying at 50-100 ℃ for 1-10h, taking out, putting the powder after grinding and sieving into a die, and putting the powder at the pressure of 0.5-10MPa/cm2Pressing and forming under pressure to obtain a pre-pressed green body;
and 5: thermal treatment
And (4) putting the green body obtained in the step (4) into a heat treatment furnace, raising the temperature to 800 ℃ at the heating rate of 1-10 ℃/min, preserving the heat for 0-10h, then cooling to room temperature at the cooling rate of 1-20 ℃/min to obtain a cooked blank, and processing to obtain wave absorbing bodies with different shapes.
In the step 2, the mass ratio of the soft magnetic ferrite powder obtained in the step 1 to the mixture of water and ball milling beads is 1:1-3: 0.5-2.
In the step 3, the coupling agent is one or more of KH-550, KH-560, KH-570, KH-792 and the like; the diluent is one or more of ethanol, isopropanol, toluene, acetone, xylene and the like.
In the step 4, the resin is one or more of phenolic resin, organic silicon resin, polyurethane, polypropylene and the like.
In the steps 4 and 5, different dies can be used for pre-pressing the green body and processing the cooked body according to different application environments, and different shapes including block bodies, patches, films, complex structures, flexible materials and the like can be customized.
The invention has the beneficial effects that:
1. the raw material of the invention is soft magnetic ferrite solid waste, thereby realizing the recycling of the waste, avoiding the pollution of the solid waste to the environment and having extremely high economic benefit and environmental protection significance.
2. The electromagnetic wave absorber prepared by the invention can be customized in shape according to the application environment, and can be industrially produced in batch, and compared with like products, the cost is lower under the condition of the same performance.
3. The invention uses interface dipole to enhance dielectric loss, balance the performance difference of mixed solid waste, improve interface impedance matching, improve electromagnetic wave absorption performance, enhance mechanical property and thermodynamic stability of the electromagnetic wave absorber, solve the common defects of cracks and brittle failure of ferrite solid waste matrix block body caused by grain size difference and temperature change, and can be used for preparing flexible electromagnetic wave absorber material.
4. The invention is suitable for electromagnetic shielding, electromagnetic interference resistance, electromagnetic radiation resistance and other purposes of various electronic, electrical and wireless communication equipment, has excellent low-frequency-band electromagnetic wave absorption performance, and can enhance the electromagnetic compatibility characteristic of the equipment. Meanwhile, the resin and ferrite solid waste composite structure widens the wave absorbing frequency band of the electromagnetic wave absorber, so that the resin and ferrite solid waste composite structure is suitable for wide frequency band application of high and low microwave frequency bands.
Drawings
FIG. 1 shows the Reflection Loss (RL) of the absorber of example 1 at 10MHz to 1GHz and a thickness of 2.09 mm. The RL value of the absorber exceeds-29 dB in a frequency band of 1GHz, exceeds-50 dB in a frequency band of 10-130MHz, and reaches the minimum value of-78.65 dB when f is 25.9 MHz.
FIG. 2 shows the Reflection Loss (RL) of the absorber of example 1 in the frequency range of 1 to 18GHz and the thickness range of 0 to 10 mm. RL reaches a minimum of-11.55 dB when d is 8mm and f is 16.7 GHz.
FIG. 3 is a scanning electron microscope image of a cross section of the absorber of example 1. As can be seen, the ferrite grains are arranged more densely and have a size distribution of 0.4-2 μm, and the rough surface image shows that the resin is more uniformly coated on the ferrite grain interface.
FIG. 4 shows the Reflection Loss (RL) of the absorber of example 2 at 10MHz to 1GHz and a thickness of 1.75 mm. The RL value of the absorber exceeds-30 dB in a frequency band of 1GHz, exceeds-50 dB in a frequency band of 10-140MHz, and reaches a minimum value of-77 dB when f is 25.9 MHz.
FIG. 5 shows the Reflection Loss (RL) of the absorber of example 2 in the frequency range of 1 to 18GHz and the thickness range of 0 to 10 mm. RL reaches a minimum of-4.18 dB when d is 8mm and f is 16.3 GHz.
FIG. 6 is a scanning electron microscope image of a cross section of the sample of example 2. As can be seen, the ferrite grains are arranged more densely and have a size distribution of 0.5-2 μm, and the rough surface image shows that the resin is more uniformly coated on the ferrite grain interface.
FIG. 7 is a graph showing the Reflection Loss (RL) of the absorber of example 3 at 10MHz to 1GHz and a thickness of 2.08 mm. The RL value of the absorber exceeds-28 dB in a frequency band of 1GHz, exceeds-50 dB in a frequency band of 10-125MHz, and reaches the minimum value of-83.7 dB when f is 25.9 MHz.
FIG. 8 shows the Reflection Loss (RL) of the absorber of example 3 in the frequency range of 1 to 18GHz and the thickness range of 0 to 10 mm. RL reaches a minimum of-9.15 dB when d is 8mm and f is 16.43 GHz.
FIG. 9 is a scanning electron microscope image of a cross section of the sample of example 3. As can be seen, the ferrite grains are arranged more densely and have a size distribution of 0.5-2.5 μm, and the rough surface image shows that the resin is more uniformly coated on the ferrite grain interface.
Detailed Description
Example 1:
in the embodiment, the broadband electromagnetic wave absorber with good mechanical property and wave-absorbing property is prepared by compounding the boron phenolic resin with the manganese-zinc ferrite solid waste, purifying and modifying the ferrite solid waste and compounding the ferrite solid waste with the resin. The preparation method comprises the following steps:
1. purification of soft magnetic ferrite solid waste
1a, fully mixing the solid waste of the soft magnetic ferrite with water, stirring and dispersing, sieving to filter out some larger impurity particles such as metal scraps, carborundum and the like, and applying a magnetic field to the obtained mixed liquid to separate magnetic soft magnetic ferrite particles from a non-magnetic impurity aqueous solution;
1b, repeating the step 1a for 5 times, and then drying and grinding the separated soft magnetic ferrite to obtain purified soft magnetic ferrite powder;
2. homogenization of soft magnetic ferrite particles
Mixing the ferrite powder purified in the step 1 with water and ball milling beads according to a mass ratio of 1:2:0.8 by a wet milling method, putting the mixture into a ball milling tank, carrying out wet milling for 6 hours at a constant speed of 300r/min, taking out a sample, and drying to obtain soft magnetic ferrite powder with a certain particle size and uniform particle size;
3. modification of soft magnetic ferrite interface
Uniformly dissolving KH-550 in absolute ethanol according to the mass ratio of 2.5%, mixing with the soft magnetic ferrite powder obtained in step 2, continuously stirring for 45min at the speed of 800r/min, drying, and sieving to obtain interface modified ferrite powder;
4. prepressing for shaping
Uniformly mixing boron phenolic resin with the interface modified soft magnetic ferrite powder obtained in the step (3) according to the mass ratio of 10%, granulating, drying at 60 ℃ for 3h, taking out, grinding and sieving, putting the powder into a die, and controlling the pressure to be 5MPa/cm2Pressing and forming under pressure to obtain a pre-pressed green body;
5. thermal treatment
And (4) putting the green body obtained in the step (4) into a heat treatment furnace, heating to 200 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, heating to 300 ℃ and preserving heat for 2h, heating to 400 ℃ and preserving heat for 1h, cooling to room temperature at a cooling rate of 3 ℃/min to obtain a cooked blank, and processing to obtain the wave absorbing body.
Example 2:
in the embodiment, the broadband electromagnetic wave absorber with good mechanical property and wave-absorbing property is prepared by compounding the aqueous polyurethane and the manganese-zinc ferrite solid waste, purifying and modifying the ferrite solid waste and compounding the ferrite solid waste with resin. The preparation method comprises the following steps:
1. purification of soft magnetic ferrite solid waste
1a, fully mixing the solid waste of the soft magnetic ferrite with water, stirring and dispersing, sieving to filter out some larger impurity particles such as metal scraps, carborundum and the like, and applying a magnetic field to the obtained mixed liquid to separate magnetic soft magnetic ferrite particles from a non-magnetic impurity aqueous solution;
1b, repeating the step 1a for 5 times, and then drying and grinding the separated soft magnetic ferrite to obtain purified soft magnetic ferrite powder;
2. homogenization of soft magnetic ferrite particles
Mixing the ferrite powder purified in the step 1 with water and ball milling beads according to the mass ratio of 1:3:1 by a wet milling method, putting the mixture into a ball milling tank, carrying out wet milling for 7 hours at a constant speed of 250r/min, taking out a sample, and drying to obtain soft magnetic ferrite powder with a certain particle size and uniform particle size;
3. modification of soft magnetic ferrite interface
Uniformly dissolving KH-560 in absolute ethanol according to the mass ratio of 5%, then mixing with the soft magnetic ferrite powder obtained in the step 2, continuously stirring for 45min at the speed of 600r/min, drying and sieving to obtain interface modified ferrite powder;
4. prepressing for shaping
Uniformly mixing the waterborne polyurethane and the interface modified soft magnetic ferrite powder obtained in the step 3 according to the proportion of 0.2ml/g, granulating, drying at 60 ℃ for 2h, taking out, putting the powder after grinding and sieving into a die, and putting the powder at the pressure of 6MPa/cm2Pressing and forming under pressure to obtain a pre-pressed green body;
5. thermal treatment
Putting the green body obtained in the step 4 into a heat treatment furnace, heating to 130 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 2h, heating to 150 ℃, keeping the temperature for 2h, heating to 180 ℃, and keeping the temperature for 2 h; and then cooling to room temperature at the cooling speed of 2 ℃/min to obtain a cooked embryo, and processing to obtain the wave absorbing body.
Example 3:
in the embodiment, the organic silicon resin is compounded with the manganese zinc ferrite solid waste, and the broadband electromagnetic wave absorber with good mechanical property and wave absorbing property is prepared by purifying and modifying the ferrite solid waste and compounding the ferrite solid waste with the resin. The preparation method comprises the following steps:
1. purification of soft magnetic ferrite solid waste
1a, fully mixing the solid waste of the soft magnetic ferrite with water, stirring and dispersing, sieving to filter out some larger impurity particles such as metal scraps, carborundum and the like, and applying a magnetic field to the obtained mixed liquid to separate magnetic soft magnetic ferrite particles from a non-magnetic impurity aqueous solution;
1b, repeating the step 1a for 5 times, and then drying and grinding the separated soft magnetic ferrite to obtain purified soft magnetic ferrite powder;
2. homogenization of soft magnetic ferrite particles
Mixing the ferrite powder purified in the step 1 with water and ball milling beads according to a mass ratio of 1:2:1 by a wet milling method, putting the mixture into a ball milling tank, carrying out wet milling for 8 hours at a constant speed of 200r/min, taking out a sample, and drying to obtain soft magnetic ferrite powder with a certain particle size and uniform particle size;
3. modification of soft magnetic ferrite interface
Uniformly dissolving KH-550 in absolute ethanol according to the mass ratio of 5%, mixing with the soft magnetic ferrite powder obtained in the step 2, continuously stirring for 45min at the speed of 600r/min, drying, and sieving to obtain interface modified ferrite powder;
4. prepressing for shaping
Uniformly mixing the organic silicon resin and the interface modified soft magnetic ferrite powder obtained in the step 3 according to the mass ratio of 10%, granulating, drying at 60 ℃ for 5 hours, taking out, putting the powder after grinding and sieving into a die, and putting the powder at the pressure of 5MPa/cm2Pressing and forming under pressure to obtain a pre-pressed green body;
5. thermal treatment
Putting the green body obtained in the step 4 into a heat treatment furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 1h, heating to 500 ℃, and keeping the temperature for 3 h; and then cooling to room temperature at the cooling speed of 2 ℃/min to obtain a cooked embryo, and processing to obtain the wave absorbing body.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (5)
1. A preparation method of a resin reinforced ferrite solid waste based broadband electromagnetic wave absorber is characterized by comprising the following steps:
firstly, purifying soft magnetic ferrite solid waste through a series of steps of washing, dispersing, filtering and magnetic separation, then modifying purified ferrite solid waste crystal grains, and then compounding the modified ferrite solid waste crystal grains with resin to prepare an electromagnetic wave absorber with excellent mechanical property and wave absorbing property; the method comprises the following steps:
step 1: purification of soft magnetic ferrite solid waste
1a, sufficiently mixing the soft magnetic ferrite solid waste with water, stirring and dispersing, sieving to remove impurity particles, and applying a magnetic field to the obtained mixed liquid to separate magnetic soft magnetic ferrite particles from a non-magnetic impurity water solution;
1b, repeating the step 1a for 1-6 times, and then drying and grinding to obtain purified soft magnetic ferrite powder;
step 2: homogenization of soft magnetic ferrite particles
Mixing the soft magnetic ferrite powder obtained in the step 1 with water and ball milling beads, putting the mixture into a ball milling tank, carrying out wet ball milling for 1-20h at a constant speed of 50-500r/min, taking out and drying to obtain soft magnetic ferrite powder with a certain particle size and uniform particle size;
and step 3: modification of soft magnetic ferrite interface
Uniformly dissolving a coupling agent in a diluent, mixing the coupling agent with the soft magnetic ferrite powder obtained in the step 2, continuously stirring for 10-200min at the rotating speed of 300-800r/min, drying and sieving to obtain interface modified ferrite powder;
and 4, step 4: prepressing for shaping
Uniformly mixing and granulating the resin and the interface modified soft magnetic ferrite powder obtained in the step (3) according to the mass ratio of 1-200%, drying at 50-100 ℃ for 1-10h, taking out, putting the powder after grinding and sieving into a die, and putting the powder at the pressure of 0.5-10MPa/cm2Pressing and forming under pressure to obtain a pre-pressed green body;
and 5: thermal treatment
Putting the green body obtained in the step 4 into a heat treatment furnace, raising the temperature to 800 ℃ at the heating rate of 1-10 ℃/min, preserving the heat for 0-10h, then cooling to room temperature at the cooling rate of 1-20 ℃/min to obtain a cooked blank, and processing to obtain wave absorbing bodies with different shapes;
in the step 3, the coupling agent is one or more of KH-550, KH-560, KH-570 and KH-792; the diluent is one or more of ethanol, isopropanol, toluene, acetone and xylene;
in the step 3, the coupling agent is poured into the diluent according to the mass ratio of 1-20%, and is uniformly stirred and dispersed at the rotating speed of 200-1000r/min, and the mass ratio of the obtained coupling agent dispersion liquid to the soft magnetic ferrite powder obtained in the step 2 is 80-160%.
2. The method of claim 1, wherein:
in the step 2, the mass ratio of the soft magnetic ferrite powder obtained in the step 1 to the mixture of water and ball milling beads is 1:1-3: 0.5-2.
3. The method of claim 1, wherein:
in the step 4, the resin is one or more of phenolic resin, organic silicon resin, polyurethane and polypropylene.
4. The method of claim 1, wherein:
in the step 4, the mass ratio of the resin to the modified soft magnetic ferrite powder obtained in the step 3 is 1-200%.
5. The method of claim 1, wherein:
in the steps 4 and 5, the pre-pressing of the green body and the processing of the cooked body can use different molds according to different application environments, and different shapes including block bodies, patches, films and flexible materials are customized.
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